# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_POD_Cl
_database_code_depnum_ccdc_archive 'CCDC 2268769'
loop_
_audit_author_name
_audit_author_address
'Sandeep Kumar Dey'
;CSIR Northeast Institute of Science and Technology Jorhat
India
;
_audit_update_record             
;
2023-06-09 deposited with the CCDC.	2023-09-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        1,3,5-tris(4-chloro-phenoxymethyl)mesitylene
_chemical_name_common            ?
_chemical_melting_point          543
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H27 Cl3 O3'
_chemical_formula_weight         541.87

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'
Cl Cl 0.1484 0.1585 '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'

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

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

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

_cell_length_a                   9.4393(10)
_cell_length_b                   11.7938(12)
_cell_length_c                   12.8424(12)
_cell_angle_alpha                75.714(3)
_cell_angle_beta                 89.665(3)
_cell_angle_gamma                77.614(3)
_cell_volume                     1351.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9950
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      25.79

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_F_000             564
_exptl_transmission_factor_min   0.7027
_exptl_transmission_factor_max   0.7457
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_absorpt_coefficient_mu    0.369
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56924
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.540
_diffrn_reflns_theta_max         28.316
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6718
_reflns_number_gt                4863
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0601P)²+1.2764P] 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_number_reflns         6718
_refine_ls_number_parameters     328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0731
_refine_ls_wR_factor_ref         0.1749
_refine_ls_wR_factor_gt          0.1590
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_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
Cl1 Cl 0.57973(11) -0.05793(8) 1.22356(7) 0.0649(3) Uani 1 1 d . . . . .
Cl2 Cl 1.14257(10) 0.97054(9) 0.65707(10) 0.0763(3) Uani 1 1 d . . . . .
Cl3 Cl 0.01403(13) 0.70831(14) -0.09245(8) 0.1000(5) Uani 1 1 d . . . . .
O1 O 0.4538(2) 0.34915(19) 0.84356(16) 0.0510(5) Uani 1 1 d . . . . .
O2 O 0.6705(2) 0.72958(18) 0.6165(2) 0.0540(6) Uani 1 1 d . . . . .
O3 O 0.1634(2) 0.65714(19) 0.36253(16) 0.0471(5) Uani 1 1 d . . . . .
C1 C 0.5381(4) 0.0657(3) 1.1117(2) 0.0450(7) Uani 1 1 d . . . . .
C8 C 0.3325(3) 0.5207(2) 0.7168(2) 0.0354(6) Uani 1 1 d . . . . .
C9 C 0.4079(3) 0.6094(2) 0.7211(2) 0.0363(6) Uani 1 1 d . . . . .
C10 C 0.4580(4) 0.6208(3) 0.8298(3) 0.0608(9) Uani 1 1 d . . . . .
H10A H 0.544426 0.652125 0.822032 0.091 Uiso 1 1 calc R U . . .
H10B H 0.478152 0.543358 0.879909 0.091 Uiso 1 1 calc R U . . .
H10C H 0.383042 0.674230 0.856058 0.091 Uiso 1 1 calc R U . . .
C11 C 0.4374(3) 0.6857(2) 0.6258(2) 0.0362(6) Uani 1 1 d . . . . .
C12 C 0.5210(3) 0.7815(2) 0.6286(3) 0.0442(7) Uani 1 1 d . . . . .
H12A H 0.486085 0.852329 0.570532 0.053 Uiso 1 1 calc R U . . .
H12B H 0.509719 0.803946 0.696450 0.053 Uiso 1 1 calc R U . . .
C13 C 0.7729(3) 0.7943(2) 0.6235(2) 0.0398(6) Uani 1 1 d . . . . .
C14 C 0.9147(3) 0.7368(3) 0.6148(3) 0.0588(9) Uani 1 1 d . . . . .
H14 H 0.933996 0.660455 0.602836 0.071 Uiso 1 1 calc R U . . .
C15 C 1.0276(3) 0.7913(3) 0.6237(3) 0.0557(8) Uani 1 1 d . . . . .
H15 H 1.122829 0.751926 0.618325 0.067 Uiso 1 1 calc R U . . .
C16 C 0.9987(3) 0.9039(3) 0.6406(3) 0.0461(7) Uani 1 1 d . . . . .
C17 C 0.8590(3) 0.9623(3) 0.6485(3) 0.0554(8) Uani 1 1 d . . . . .
H17 H 0.840543 1.038722 0.660184 0.066 Uiso 1 1 calc R U . . .
C18 C 0.7445(3) 0.9080(2) 0.6393(3) 0.0457(7) Uani 1 1 d . . . . .
H18 H 0.649363 0.948261 0.643795 0.055 Uiso 1 1 calc R U . . .
C19 C 0.3967(3) 0.6710(2) 0.5255(2) 0.0346(6) Uani 1 1 d . . . . .
C20 C 0.4350(3) 0.7487(3) 0.4219(3) 0.0513(8) Uani 1 1 d . . . . .
H20A H 0.349698 0.806670 0.388628 0.077 Uiso 1 1 calc R U . . .
H20B H 0.472326 0.699488 0.374190 0.077 Uiso 1 1 calc R U . . .
H20C H 0.507298 0.789418 0.436910 0.077 Uiso 1 1 calc R U . . .
C21 C 0.3198(3) 0.5820(2) 0.5226(2) 0.0336(5) Uani 1 1 d . . . . .
C22 C 0.2836(3) 0.5629(2) 0.4148(2) 0.0404(6) Uani 1 1 d . . . . .
H22A H 0.367210 0.563752 0.370616 0.048 Uiso 1 1 calc R U . . .
H22B H 0.258115 0.485663 0.424573 0.048 Uiso 1 1 calc R U . . .
C23 C 0.1306(3) 0.6622(3) 0.2579(2) 0.0412(6) Uani 1 1 d . . . . .
C24 C 0.0385(3) 0.7666(3) 0.1997(3) 0.0524(8) Uani 1 1 d . . . . .
H24 H 0.001513 0.827846 0.232737 0.063 Uiso 1 1 calc R U . . .
C25 C 0.0016(4) 0.7798(3) 0.0926(3) 0.0606(9) Uani 1 1 d . . . . .
H25 H -0.059718 0.850079 0.053646 0.073 Uiso 1 1 calc R U . . .
C26 C 0.0551(4) 0.6898(4) 0.0442(3) 0.0595(9) Uani 1 1 d . . . . .
C27 C 0.1427(4) 0.5851(4) 0.1014(3) 0.0610(9) Uani 1 1 d . . . . .
H27 H 0.176721 0.523358 0.068230 0.073 Uiso 1 1 calc R U . . .
C28 C 0.1809(3) 0.5708(3) 0.2088(2) 0.0507(7) Uani 1 1 d . . . . .
H28 H 0.240391 0.499466 0.247686 0.061 Uiso 1 1 calc R U . . .
C29 C 0.2833(3) 0.5089(2) 0.6176(2) 0.0342(5) Uani 1 1 d . . . . .
C30 C 0.1916(4) 0.4193(3) 0.6139(3) 0.0539(8) Uani 1 1 d . . . . .
H30A H 0.133037 0.445333 0.547981 0.081 Uiso 1 1 calc R U . . .
H30B H 0.129898 0.413264 0.673804 0.081 Uiso 1 1 calc R U . . .
H30C H 0.253768 0.342245 0.617618 0.081 Uiso 1 1 calc R U . . .
C2 C 0.6476(4) 0.0963(3) 1.0469(3) 0.0542(8) Uani 1 1 d . . . . .
H2 H 0.742688 0.052702 1.063091 0.065 Uiso 1 1 calc R U . . .
C3 C 0.6150(3) 0.1914(3) 0.9584(3) 0.0514(8) Uani 1 1 d . . . . .
H3 H 0.688386 0.211775 0.913739 0.062 Uiso 1 1 calc R U . . .
C4 C 0.4742(3) 0.2576(3) 0.9347(2) 0.0405(6) Uani 1 1 d . . . . .
C5 C 0.3645(3) 0.2281(3) 1.0013(2) 0.0458(7) Uani 1 1 d . . . . .
H5 H 0.269823 0.273086 0.986899 0.055 Uiso 1 1 calc R U . . .
C6 C 0.3987(4) 0.1299(3) 1.0903(2) 0.0509(8) Uani 1 1 d . . . . .
H6 H 0.326065 0.108183 1.135126 0.061 Uiso 1 1 calc R U . . .
C7 C 0.3150(3) 0.4309(3) 0.8197(2) 0.0442(7) Uani 1 1 d . . . . .
H7A H 0.289419 0.470285 0.877234 0.053 Uiso 1 1 calc R U . . .
H7B H 0.240060 0.389058 0.809850 0.053 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
Cl1 C1 1.752(3) . ?
Cl2 C16 1.746(3) . ?
Cl3 C26 1.749(3) . ?
O1 C4 1.365(3) . ?
O1 C7 1.434(3) . ?
O2 C13 1.370(3) . ?
O2 C12 1.437(3) . ?
O3 C23 1.365(3) . ?
O3 C22 1.439(3) . ?
C1 C6 1.362(4) . ?
C1 C2 1.376(4) . ?
C8 C9 1.397(4) . ?
C8 C29 1.407(4) . ?
C8 C7 1.509(4) . ?
C9 C11 1.395(4) . ?
C9 C10 1.523(4) . ?
C11 C19 1.409(4) . ?
C11 C12 1.517(4) . ?
C13 C18 1.375(4) . ?
C13 C14 1.382(4) . ?
C14 C15 1.377(4) . ?
C15 C16 1.367(4) . ?
C16 C17 1.366(4) . ?
C17 C18 1.388(4) . ?
C19 C21 1.406(4) . ?
C19 C20 1.508(4) . ?
C21 C29 1.399(4) . ?
C21 C22 1.508(4) . ?
C23 C28 1.378(4) . ?
C23 C24 1.387(4) . ?
C24 C25 1.383(5) . ?
C25 C26 1.365(5) . ?
C26 C27 1.367(5) . ?
C27 C28 1.389(4) . ?
C29 C30 1.511(4) . ?
C2 C3 1.368(4) . ?
C3 C4 1.382(4) . ?
C4 C5 1.386(4) . ?
C5 C6 1.393(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 O1 C7 119.3(2) . . ?
C13 O2 C12 118.7(2) . . ?
C23 O3 C22 116.1(2) . . ?
C6 C1 C2 121.1(3) . . ?
C6 C1 Cl1 119.8(2) . . ?
C2 C1 Cl1 119.1(3) . . ?
C9 C8 C29 120.9(2) . . ?
C9 C8 C7 118.9(2) . . ?
C29 C8 C7 120.0(2) . . ?
C11 C9 C8 119.6(2) . . ?
C11 C9 C10 120.8(3) . . ?
C8 C9 C10 119.6(3) . . ?
C9 C11 C19 120.5(2) . . ?
C9 C11 C12 120.5(3) . . ?
C19 C11 C12 118.9(2) . . ?
O2 C12 C11 106.1(2) . . ?
O2 C13 C18 125.2(2) . . ?
O2 C13 C14 115.3(2) . . ?
C18 C13 C14 119.5(3) . . ?
C15 C14 C13 120.7(3) . . ?
C16 C15 C14 119.5(3) . . ?
C17 C16 C15 120.5(3) . . ?
C17 C16 Cl2 120.1(2) . . ?
C15 C16 Cl2 119.4(2) . . ?
C16 C17 C18 120.4(3) . . ?
C13 C18 C17 119.4(3) . . ?
C21 C19 C11 119.1(2) . . ?
C21 C19 C20 119.9(3) . . ?
C11 C19 C20 121.0(2) . . ?
C29 C21 C19 120.9(2) . . ?
C29 C21 C22 120.5(2) . . ?
C19 C21 C22 118.6(2) . . ?
O3 C22 C21 109.1(2) . . ?
O3 C23 C28 124.2(3) . . ?
O3 C23 C24 116.4(3) . . ?
C28 C23 C24 119.3(3) . . ?
C25 C24 C23 120.1(3) . . ?
C26 C25 C24 120.0(3) . . ?
C25 C26 C27 120.5(3) . . ?
C25 C26 Cl3 120.1(3) . . ?
C27 C26 Cl3 119.4(3) . . ?
C26 C27 C28 120.1(3) . . ?
C23 C28 C27 119.9(3) . . ?
C21 C29 C8 118.9(2) . . ?
C21 C29 C30 120.6(2) . . ?
C8 C29 C30 120.6(2) . . ?
C3 C2 C1 119.3(3) . . ?
C2 C3 C4 120.7(3) . . ?
O1 C4 C3 115.7(2) . . ?
O1 C4 C5 124.4(3) . . ?
C3 C4 C5 119.9(3) . . ?
C4 C5 C6 118.9(3) . . ?
C1 C6 C5 120.2(3) . . ?
O1 C7 C8 105.1(2) . . ?

_refine_diff_density_max         0.448
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.055

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetone ethanol'
####################################################################### 
# 
# 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_POD_I
_database_code_depnum_ccdc_archive 'CCDC 2268771'
loop_
_audit_author_name
_audit_author_address
'Sandeep Kumar Dey'
;CSIR Northeast Institute of Science and Technology Jorhat
India
;
_audit_update_record             
;
2023-06-09 deposited with the CCDC.	2023-09-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/2
_shelx_SHELXL_version_number     2019/2
_chemical_name_systematic        1,3,5-tris(4-iodo-phenoxymethyl)mesitylene
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H27 I3 O3'
_chemical_formula_weight         816.21

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'
I I -0.4742 1.8119 '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'

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

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

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

_cell_length_a                   9.645(3)
_cell_length_b                   12.616(4)
_cell_length_c                   14.168(5)
_cell_angle_alpha                106.195(10)
_cell_angle_beta                 93.337(10)
_cell_angle_gamma                93.160(9)
_cell_volume                     1648.2(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    8917
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      23.01

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_F_000             780
_exptl_transmission_factor_min   0.5417
_exptl_transmission_factor_max   0.7457
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.870
_shelx_estimated_absorpt_T_min   0.451
_shelx_estimated_absorpt_T_max   0.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-III photon detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11722
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.121
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5791
_reflns_number_gt                3938
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0693P)²+7.3666P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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_number_reflns         5791
_refine_ls_number_parameters     353
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0798
_refine_ls_wR_factor_ref         0.2059
_refine_ls_wR_factor_gt          0.1896
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.003
_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 0.7810(7) 0.3713(5) 0.3748(5) 0.0763(19) Uani 1 1 d . . . . .
O2 O 0.2483(6) 0.5998(6) 0.3076(5) 0.0741(18) Uani 1 1 d . . . . .
O3 O 0.6000(8) 0.8479(6) 0.6265(6) 0.094(2) Uani 1 1 d . . . . .
C1 C 0.4821(11) 0.4151(9) 0.2852(8) 0.083(3) Uani 1 1 d . . . . .
H1A H 0.524564 0.354773 0.301581 0.125 Uiso 1 1 calc R U . . .
H1B H 0.383465 0.407759 0.290505 0.125 Uiso 1 1 calc R U . . .
H1C H 0.499741 0.413890 0.218964 0.125 Uiso 1 1 calc R U . . .
C2 C 0.5411(8) 0.5204(7) 0.3536(7) 0.055(2) Uani 1 1 d . . . . .
C3 C 0.4926(8) 0.6192(8) 0.3422(7) 0.060(2) Uani 1 1 d . . . . .
C4 C 0.5440(9) 0.7211(7) 0.4076(7) 0.060(2) Uani 1 1 d . . . . .
C5 C 0.4844(12) 0.8297(8) 0.3996(9) 0.084(3) Uani 1 1 d . . . . .
H5A H 0.530939 0.891066 0.449609 0.126 Uiso 1 1 calc R U . . .
H5B H 0.498713 0.838858 0.335782 0.126 Uiso 1 1 calc R U . . .
H5C H 0.386505 0.826603 0.408524 0.126 Uiso 1 1 calc R U . . .
C6 C 0.6505(9) 0.7248(8) 0.4808(7) 0.066(2) Uani 1 1 d . . . . .
C7 C 0.7020(8) 0.6248(8) 0.4887(7) 0.059(2) Uani 1 1 d . . . . .
C8 C 0.8234(11) 0.6290(10) 0.5634(8) 0.088(3) Uani 1 1 d . . . . .
H8A H 0.850924 0.704663 0.598587 0.132 Uiso 1 1 calc R U . . .
H8B H 0.795450 0.589669 0.609108 0.132 Uiso 1 1 calc R U . . .
H8C H 0.900303 0.595247 0.529835 0.132 Uiso 1 1 calc R U . . .
C9 C 0.6446(9) 0.5247(7) 0.4294(7) 0.058(2) Uani 1 1 d . . . . .
C10 C 0.6873(9) 0.4186(8) 0.4468(8) 0.067(2) Uani 1 1 d . . . . .
H10A H 0.732594 0.433101 0.512543 0.081 Uiso 1 1 calc R U . . .
H10B H 0.605991 0.367783 0.441055 0.081 Uiso 1 1 calc R U . . .
C11 C 0.8079(9) 0.2638(8) 0.3679(8) 0.067(2) Uani 1 1 d . . . . .
C12 C 0.7919(12) 0.2143(9) 0.4426(9) 0.086(3) Uani 1 1 d . . . . .
H12 H 0.759183 0.254589 0.501499 0.104 Uiso 1 1 calc R U . . .
C13 C 0.8239(12) 0.1048(9) 0.4315(10) 0.093(3) Uani 1 1 d . . . . .
H13 H 0.814842 0.072806 0.482772 0.112 Uiso 1 1 calc R U . . .
C14 C 0.8677(11) 0.0471(9) 0.3454(11) 0.087(3) Uani 1 1 d . . . . .
C15 C 0.8893(12) 0.0946(10) 0.2708(10) 0.095(4) Uani 1 1 d . . . . .
H15 H 0.922154 0.053985 0.212194 0.114 Uiso 1 1 calc R U . . .
C16 C 0.8614(12) 0.2031(11) 0.2844(9) 0.093(3) Uani 1 1 d . . . . .
H16 H 0.879652 0.236372 0.235025 0.112 Uiso 1 1 calc R U . . .
C17 C 0.3757(8) 0.6154(9) 0.2638(7) 0.070(3) Uani 1 1 d . . . . .
H17A H 0.378405 0.684035 0.245523 0.084 Uiso 1 1 calc R U . . .
H17B H 0.384107 0.554685 0.205353 0.084 Uiso 1 1 calc R U . . .
C18 C 0.1257(8) 0.5971(8) 0.2515(7) 0.062(2) Uani 1 1 d . . . . .
C19 C 0.0046(9) 0.5810(9) 0.2957(8) 0.077(3) Uani 1 1 d . . . . .
H19 H 0.009493 0.572057 0.358753 0.092 Uiso 1 1 calc R U . . .
C20 C -0.1224(11) 0.5784(10) 0.2457(10) 0.088(3) Uani 1 1 d . . . . .
H20 H -0.203400 0.567979 0.275567 0.105 Uiso 1 1 calc R U . . .
C21 C -0.1318(9) 0.5906(8) 0.1549(8) 0.068(3) Uani 1 1 d . . . . .
C22 C -0.0124(10) 0.6061(9) 0.1105(7) 0.079(3) Uani 1 1 d . . . . .
H22 H -0.018016 0.615559 0.047636 0.095 Uiso 1 1 calc R U . . .
C23 C 0.1156(9) 0.6074(8) 0.1595(7) 0.069(3) Uani 1 1 d . . . . .
H23 H 0.196198 0.615541 0.128393 0.083 Uiso 1 1 calc R U . . .
C24 C 0.6989(11) 0.8314(8) 0.5550(8) 0.077(3) Uani 1 1 d . . . . .
H24A H 0.790879 0.827011 0.584601 0.092 Uiso 1 1 calc R U . . .
H24B H 0.702327 0.891477 0.524721 0.092 Uiso 1 1 calc R U . . .
C25 C 0.6170(11) 0.9369(10) 0.7046(9) 0.085(3) Uani 1 1 d . . . . .
C26 C 0.7282(11) 1.0134(8) 0.7302(9) 0.083(3) Uani 1 1 d . . . . .
H26 H 0.801190 1.006851 0.689329 0.099 Uiso 1 1 calc R U . . .
C27 C 0.7349(15) 1.0966(10) 0.8115(11) 0.107(4) Uani 1 1 d . . . . .
H27 H 0.814610 1.144904 0.827224 0.128 Uiso 1 1 calc R U . . .
C28 C 0.6319(15) 1.1146(12) 0.8725(10) 0.109(4) Uani 1 1 d . . . . .
C29 C 0.5163(17) 1.0464(15) 0.8485(13) 0.141(6) Uani 1 1 d . . . . .
H29 H 0.442069 1.059485 0.888199 0.169 Uiso 1 1 calc R U . . .
C30 C 0.5058(14) 0.9565(13) 0.7653(12) 0.127(5) Uani 1 1 d . . . . .
H30 H 0.425193 0.909123 0.749707 0.152 Uiso 1 1 calc R U . . .
I1B I 0.9034(5) -0.1171(4) 0.3177(5) 0.187(3) Uani 0.650(19) 1 d . U P A 2
I1A I 0.9005(4) -0.1245(3) 0.3273(3) 0.071(2) Uani 0.350(19) 1 d . . P A 1
I2A I -0.3271(7) 0.5871(8) 0.0850(4) 0.111(3) Uani 0.350(19) 1 d . . P A 1
I2B I -0.3270(4) 0.5995(4) 0.0808(3) 0.1140(15) Uani 0.650(19) 1 d . U P A 2
I3B I 0.6516(7) 1.2378(5) 1.0078(4) 0.221(4) Uani 0.650(19) 1 d . U P A 2
I3A I 0.6433(4) 1.2477(3) 1.0023(2) 0.075(2) Uani 0.350(19) 1 d . . 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
O1 C11 1.371(11) . ?
O1 C10 1.429(10) . ?
O2 C18 1.379(11) . ?
O2 C17 1.436(10) . ?
O3 C25 1.333(13) . ?
O3 C24 1.413(12) . ?
C1 C2 1.471(13) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.402(12) . ?
C2 C9 1.411(12) . ?
C3 C4 1.403(12) . ?
C3 C17 1.525(12) . ?
C4 C6 1.406(13) . ?
C4 C5 1.545(12) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.411(13) . ?
C6 C24 1.488(13) . ?
C7 C9 1.373(12) . ?
C7 C8 1.521(13) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.501(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C16 1.365(14) . ?
C11 C12 1.384(14) . ?
C12 C13 1.400(15) . ?
C12 H12 0.9300 . ?
C13 C14 1.340(15) . ?
C13 H13 0.9300 . ?
C14 C15 1.373(17) . ?
C14 I1B 2.051(11) . ?
C14 I1A 2.152(11) . ?
C15 C16 1.372(16) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C23 1.345(13) . ?
C18 C19 1.388(12) . ?
C19 C20 1.373(14) . ?
C19 H19 0.9300 . ?
C20 C21 1.336(14) . ?
C20 H20 0.9300 . ?
C21 C22 1.374(13) . ?
C21 I2A 2.069(10) . ?
C21 I2B 2.125(9) . ?
C22 C23 1.378(13) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.364(14) . ?
C25 C30 1.404(17) . ?
C26 C27 1.320(16) . ?
C26 H26 0.9300 . ?
C27 C28 1.342(18) . ?
C27 H27 0.9300 . ?
C28 C29 1.337(19) . ?
C28 I3B 2.096(14) . ?
C28 I3A 2.108(13) . ?
C29 C30 1.383(19) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 O1 C10 115.4(7) . . ?
C18 O2 C17 117.0(7) . . ?
C25 O3 C24 119.4(8) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C9 119.5(8) . . ?
C3 C2 C1 118.5(8) . . ?
C9 C2 C1 122.0(8) . . ?
C2 C3 C4 120.0(8) . . ?
C2 C3 C17 119.9(8) . . ?
C4 C3 C17 119.9(8) . . ?
C3 C4 C6 120.1(8) . . ?
C3 C4 C5 120.4(9) . . ?
C6 C4 C5 119.6(9) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 C7 119.0(8) . . ?
C4 C6 C24 120.5(9) . . ?
C7 C6 C24 120.2(9) . . ?
C9 C7 C6 120.9(8) . . ?
C9 C7 C8 120.0(9) . . ?
C6 C7 C8 119.2(9) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 C2 120.3(8) . . ?
C7 C9 C10 120.5(9) . . ?
C2 C9 C10 119.2(8) . . ?
O1 C10 C9 108.3(7) . . ?
O1 C10 H10A 110.0 . . ?
C9 C10 H10A 110.0 . . ?
O1 C10 H10B 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
C16 C11 O1 118.4(10) . . ?
C16 C11 C12 117.3(10) . . ?
O1 C11 C12 124.2(9) . . ?
C11 C12 C13 121.4(11) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C14 C13 C12 118.6(12) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
C13 C14 C15 121.6(11) . . ?
C13 C14 I1B 121.7(10) . . ?
C15 C14 I1B 116.6(9) . . ?
C13 C14 I1A 117.4(10) . . ?
C15 C14 I1A 120.9(9) . . ?
C16 C15 C14 118.8(11) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
C11 C16 C15 122.1(12) . . ?
C11 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
O2 C17 C3 105.9(7) . . ?
O2 C17 H17A 110.6 . . ?
C3 C17 H17A 110.6 . . ?
O2 C17 H17B 110.6 . . ?
C3 C17 H17B 110.6 . . ?
H17A C17 H17B 108.7 . . ?
C23 C18 O2 125.6(8) . . ?
C23 C18 C19 118.9(8) . . ?
O2 C18 C19 115.5(8) . . ?
C20 C19 C18 119.6(10) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C21 C20 C19 121.2(9) . . ?
C21 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
C20 C21 C22 119.6(9) . . ?
C20 C21 I2A 118.8(8) . . ?
C22 C21 I2A 121.6(8) . . ?
C20 C21 I2B 121.7(8) . . ?
C22 C21 I2B 118.6(8) . . ?
C21 C22 C23 119.7(9) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C18 C23 C22 121.0(9) . . ?
C18 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
O3 C24 C6 105.3(7) . . ?
O3 C24 H24A 110.7 . . ?
C6 C24 H24A 110.7 . . ?
O3 C24 H24B 110.7 . . ?
C6 C24 H24B 110.7 . . ?
H24A C24 H24B 108.8 . . ?
O3 C25 C26 127.3(11) . . ?
O3 C25 C30 116.4(10) . . ?
C26 C25 C30 116.2(12) . . ?
C27 C26 C25 121.7(12) . . ?
C27 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C26 C27 C28 123.0(12) . . ?
C26 C27 H27 118.5 . . ?
C28 C27 H27 118.5 . . ?
C29 C28 C27 118.3(13) . . ?
C29 C28 I3B 119.1(12) . . ?
C27 C28 I3B 122.5(10) . . ?
C29 C28 I3A 118.9(12) . . ?
C27 C28 I3A 122.8(10) . . ?
C28 C29 C30 120.8(14) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C29 C30 C25 119.8(13) . . ?
C29 C30 H30 120.1 . . ?
C25 C30 H30 120.1 . . ?

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
C9 C2 C3 C4 -1.8(12) . . . . ?
C1 C2 C3 C4 178.4(8) . . . . ?
C9 C2 C3 C17 -176.9(7) . . . . ?
C1 C2 C3 C17 3.3(12) . . . . ?
C2 C3 C4 C6 4.1(13) . . . . ?
C17 C3 C4 C6 179.1(8) . . . . ?
C2 C3 C4 C5 -176.1(8) . . . . ?
C17 C3 C4 C5 -1.0(13) . . . . ?
C3 C4 C6 C7 -1.5(13) . . . . ?
C5 C4 C6 C7 178.6(8) . . . . ?
C3 C4 C6 C24 -175.6(8) . . . . ?
C5 C4 C6 C24 4.5(13) . . . . ?
C4 C6 C7 C9 -3.4(13) . . . . ?
C24 C6 C7 C9 170.8(8) . . . . ?
C4 C6 C7 C8 176.2(9) . . . . ?
C24 C6 C7 C8 -9.7(13) . . . . ?
C6 C7 C9 C2 5.6(12) . . . . ?
C8 C7 C9 C2 -173.9(8) . . . . ?
C6 C7 C9 C10 -172.2(8) . . . . ?
C8 C7 C9 C10 8.3(12) . . . . ?
C3 C2 C9 C7 -3.0(12) . . . . ?
C1 C2 C9 C7 176.8(8) . . . . ?
C3 C2 C9 C10 174.8(7) . . . . ?
C1 C2 C9 C10 -5.4(12) . . . . ?
C11 O1 C10 C9 -167.5(8) . . . . ?
C7 C9 C10 O1 -102.8(10) . . . . ?
C2 C9 C10 O1 79.4(9) . . . . ?
C10 O1 C11 C16 161.2(9) . . . . ?
C10 O1 C11 C12 -22.7(13) . . . . ?
C16 C11 C12 C13 -2.6(16) . . . . ?
O1 C11 C12 C13 -178.7(10) . . . . ?
C11 C12 C13 C14 -1.5(18) . . . . ?
C12 C13 C14 C15 3.7(18) . . . . ?
C12 C13 C14 I1B -175.4(9) . . . . ?
C12 C13 C14 I1A -175.3(9) . . . . ?
C13 C14 C15 C16 -1.7(19) . . . . ?
I1B C14 C15 C16 177.4(9) . . . . ?
I1A C14 C15 C16 177.3(9) . . . . ?
O1 C11 C16 C15 -179.0(10) . . . . ?
C12 C11 C16 C15 4.7(17) . . . . ?
C14 C15 C16 C11 -2.7(18) . . . . ?
C18 O2 C17 C3 178.0(8) . . . . ?
C2 C3 C17 O2 83.6(10) . . . . ?
C4 C3 C17 O2 -91.5(10) . . . . ?
C17 O2 C18 C23 0.3(14) . . . . ?
C17 O2 C18 C19 179.5(9) . . . . ?
C23 C18 C19 C20 -1.5(16) . . . . ?
O2 C18 C19 C20 179.3(10) . . . . ?
C18 C19 C20 C21 0.3(18) . . . . ?
C19 C20 C21 C22 0.0(17) . . . . ?
C19 C20 C21 I2A -179.5(9) . . . . ?
C19 C20 C21 I2B -175.1(9) . . . . ?
C20 C21 C22 C23 0.8(16) . . . . ?
I2A C21 C22 C23 -179.7(8) . . . . ?
I2B C21 C22 C23 176.1(8) . . . . ?
O2 C18 C23 C22 -178.5(10) . . . . ?
C19 C18 C23 C22 2.3(15) . . . . ?
C21 C22 C23 C18 -2.0(16) . . . . ?
C25 O3 C24 C6 178.7(9) . . . . ?
C4 C6 C24 O3 80.5(11) . . . . ?
C7 C6 C24 O3 -93.6(10) . . . . ?
C24 O3 C25 C26 -6.0(18) . . . . ?
C24 O3 C25 C30 171.4(12) . . . . ?
O3 C25 C26 C27 -177.8(12) . . . . ?
C30 C25 C26 C27 4.8(19) . . . . ?
C25 C26 C27 C28 -3(2) . . . . ?
C26 C27 C28 C29 -1(2) . . . . ?
C26 C27 C28 I3B 174.1(11) . . . . ?
C26 C27 C28 I3A 180.0(10) . . . . ?
C27 C28 C29 C30 3(3) . . . . ?
I3B C28 C29 C30 -172.7(14) . . . . ?
I3A C28 C29 C30 -178.4(14) . . . . ?
C28 C29 C30 C25 -1(3) . . . . ?
O3 C25 C30 C29 179.1(15) . . . . ?
C26 C25 C30 C29 -3(2) . . . . ?

_refine_diff_density_max         0.781
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.104



# start Validation Reply Form
_vrf_PLAT412_POD_I_sq            
;
PROBLEM: Short Intra XH3 .. XHn     H8A      ..H24A     .       1.74 Ang.  
RESPONSE: This is due to the close proximity between the hydrogen atom of 
methylene group and the hydrogen atom of methyl group in the ligand. At the
same time, as we collected the data at 298 K, all the atoms have slightly 
higher thermal vibration.
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetone dmf'
####################################################################### 
# 
# 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_POD_CN
_database_code_depnum_ccdc_archive 'CCDC 2268772'
loop_
_audit_author_name
_audit_author_address
'Sandeep Kumar Dey'
;CSIR Northeast Institute of Science and Technology Jorhat
India
;
_audit_update_record             
;
2023-06-09 deposited with the CCDC.	2023-09-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/2
_shelx_SHELXL_version_number     2019/2
_chemical_name_systematic        1,3,5-tris(4-cyano-phenoxymethyl)mesitylene
_chemical_name_common            ?
_chemical_melting_point          573
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H27 N3 O3'
_chemical_formula_weight         513.57

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   30.916(10)
_cell_length_b                   8.682(3)
_cell_length_c                   25.527(8)
_cell_angle_alpha                90
_cell_angle_beta                 119.415(11)
_cell_angle_gamma                90
_cell_volume                     5968(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4985
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      23.15

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_F_000             2160
_exptl_transmission_factor_min   0.6011
_exptl_transmission_factor_max   0.7453
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    0.074
_shelx_estimated_absorpt_T_min   0.982
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-III detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24223
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.465
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5245
_reflns_number_gt                3224
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0899P)²+11.2321P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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_number_reflns         5245
_refine_ls_number_parameters     364
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1527
_refine_ls_R_factor_gt           0.0999
_refine_ls_wR_factor_ref         0.2567
_refine_ls_wR_factor_gt          0.2278
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_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 0.23608(11) 0.4034(3) 0.61817(13) 0.0712(9) Uani 1 1 d . . . . .
O2 O 0.16087(11) 0.5124(3) 0.35104(13) 0.0718(9) Uani 1 1 d . . . . .
O3 O 0.37690(11) 0.4474(3) 0.49628(16) 0.0822(10) Uani 1 1 d . . . . .
N1A N 0.1462(4) -0.0067(15) 0.7639(5) 0.1101(15) Uani 0.5 1 d . . P A 1
N2A N -0.0534(5) 0.6041(16) 0.0939(6) 0.1101(15) Uani 0.5 1 d . . P B 1
N3A N 0.6232(4) 0.2710(14) 0.6154(5) 0.1101(15) Uani 0.5 1 d . . P C 1
C1A C 0.1643(4) 0.0675(17) 0.7413(6) 0.0883(14) Uani 0.5 1 d . . P A 1
C2 C 0.1774(2) 0.1530(6) 0.7056(2) 0.0958(17) Uani 1 1 d . . . . .
C3 C 0.1646(2) 0.3057(7) 0.6896(3) 0.1032(19) Uani 1 1 d . . . . .
H3 H 0.141726 0.353378 0.697943 0.124 Uiso 1 1 calc R U . . .
C4 C 0.1854(2) 0.3864(6) 0.6617(2) 0.0858(15) Uani 1 1 d . . . . .
H4 H 0.176758 0.489103 0.651479 0.103 Uiso 1 1 calc R U . . .
C5 C 0.21898(17) 0.3172(5) 0.64850(19) 0.0650(11) Uani 1 1 d . . . . .
C6 C 0.2327(2) 0.1648(5) 0.6659(2) 0.0860(15) Uani 1 1 d . . . . .
H6 H 0.256209 0.117190 0.658660 0.103 Uiso 1 1 calc R U . . .
C7 C 0.2113(2) 0.0857(6) 0.6937(3) 0.1047(19) Uani 1 1 d . . . . .
H7 H 0.220161 -0.016436 0.704688 0.126 Uiso 1 1 calc R U . . .
C8 C 0.25739(17) 0.3220(5) 0.5871(2) 0.0693(12) Uani 1 1 d . . . . .
H8A H 0.236598 0.234681 0.565723 0.083 Uiso 1 1 calc R U . . .
H8B H 0.289992 0.283464 0.615934 0.083 Uiso 1 1 calc R U . . .
C9 C 0.26170(15) 0.4275(4) 0.54353(18) 0.0553(10) Uani 1 1 d . . . . .
C10 C 0.21816(15) 0.4814(4) 0.49318(19) 0.0575(10) Uani 1 1 d . . . . .
C11 C 0.16804(15) 0.4386(5) 0.4855(2) 0.0746(13) Uani 1 1 d . . . . .
H11A H 0.170263 0.340382 0.503958 0.112 Uiso 1 1 calc R U . . .
H11B H 0.144192 0.432817 0.443431 0.112 Uiso 1 1 calc R U . . .
H11C H 0.157789 0.515301 0.504233 0.112 Uiso 1 1 calc R U . . .
C12 C 0.22252(15) 0.5720(4) 0.45054(18) 0.0554(10) Uani 1 1 d . . . . .
C13 C 0.26887(15) 0.6060(4) 0.45618(18) 0.0560(10) Uani 1 1 d . . . . .
C14 C 0.2725(2) 0.6936(5) 0.4071(2) 0.0820(14) Uani 1 1 d . . . . .
H14A H 0.244389 0.668923 0.368809 0.123 Uiso 1 1 calc R U . . .
H14B H 0.302478 0.665011 0.407130 0.123 Uiso 1 1 calc R U . . .
H14C H 0.272824 0.802217 0.414296 0.123 Uiso 1 1 calc R U . . .
C15 C 0.31160(15) 0.5536(4) 0.50696(19) 0.0567(10) Uani 1 1 d . . . . .
C16 C 0.30830(14) 0.4668(4) 0.55121(18) 0.0555(10) Uani 1 1 d . . . . .
C17 C 0.35508(17) 0.4119(6) 0.6069(2) 0.0819(14) Uani 1 1 d . . . . .
H17A H 0.353113 0.438006 0.642179 0.123 Uiso 1 1 calc R U . . .
H17B H 0.383570 0.460957 0.608544 0.123 Uiso 1 1 calc R U . . .
H17C H 0.358041 0.302287 0.604937 0.123 Uiso 1 1 calc R U . . .
C18 C 0.17631(16) 0.6302(5) 0.39710(19) 0.0667(12) Uani 1 1 d . . . . .
H18A H 0.150517 0.648045 0.407585 0.080 Uiso 1 1 calc R U . . .
H18B H 0.182934 0.726172 0.382894 0.080 Uiso 1 1 calc R U . . .
C19 C 0.11870(16) 0.5355(5) 0.29812(18) 0.0616(11) Uani 1 1 d . . . . .
C20 C 0.08928(18) 0.6669(5) 0.2841(2) 0.0774(13) Uani 1 1 d . . . . .
H20 H 0.097981 0.745835 0.312140 0.093 Uiso 1 1 calc R U . . .
C21 C 0.04767(19) 0.6797(6) 0.2292(2) 0.0848(14) Uani 1 1 d . . . . .
H21 H 0.028697 0.769032 0.219934 0.102 Uiso 1 1 calc R U . . .
C22 C 0.03323(18) 0.5643(6) 0.1876(2) 0.0827(14) Uani 1 1 d . . . . .
C23 C 0.0630(2) 0.4326(6) 0.2015(2) 0.0920(16) Uani 1 1 d . . . . .
H23 H 0.054240 0.354025 0.173275 0.110 Uiso 1 1 calc R U . . .
C24 C 0.10482(19) 0.4189(5) 0.2562(2) 0.0806(14) Uani 1 1 d . . . . .
H24 H 0.124110 0.330309 0.265275 0.097 Uiso 1 1 calc R U . . .
C25A C -0.0168(6) 0.5843(18) 0.1366(7) 0.0883(14) Uani 0.5 1 d . . P B 1
C26 C 0.36221(16) 0.5862(5) 0.5147(2) 0.0718(12) Uani 1 1 d . . . . .
H26A H 0.360829 0.672533 0.489752 0.086 Uiso 1 1 calc R U . . .
H26B H 0.385602 0.610279 0.556288 0.086 Uiso 1 1 calc R U . . .
C27 C 0.42615(18) 0.4148(6) 0.5188(2) 0.0781(14) Uani 1 1 d . . . . .
C32A C 0.4427(7) 0.270(2) 0.5145(7) 0.080(5) Uani 0.5 1 d . . P C 1
H32A H 0.419992 0.190331 0.496060 0.097 Uiso 0.5 1 calc R U P C 1
C31A C 0.4928(7) 0.242(2) 0.5374(6) 0.090(5) Uani 0.5 1 d . . P C 1
H31A H 0.504020 0.146753 0.532467 0.108 Uiso 0.5 1 calc R U P C 1
C30A C 0.5223(13) 0.347(4) 0.5646(18) 0.097(4) Uani 0.5 1 d . . P C 1
C29 C 0.5139(2) 0.4651(9) 0.5769(3) 0.1052(19) Uani 1 1 d . . . . .
H29 H 0.539719 0.531278 0.601059 0.126 Uiso 1 1 calc R U . C 1
C28 C 0.46441(19) 0.5107(7) 0.5556(2) 0.0896(15) Uani 1 1 d . . . . .
H28 H 0.457588 0.605995 0.566547 0.108 Uiso 1 1 calc R U . . .
C33A C 0.5802(5) 0.3067(15) 0.5954(5) 0.0883(14) Uani 0.5 1 d . . P C 1
C31B C 0.4775(7) 0.228(2) 0.5075(8) 0.097(4) Uani 0.5 1 d . . P C 2
H31B H 0.481619 0.137465 0.490840 0.116 Uiso 0.5 1 calc R U P C 2
N2B N -0.0402(5) 0.5918(16) 0.0799(6) 0.1101(15) Uani 0.5 1 d . . P B 2
C25B C -0.0056(6) 0.5753(18) 0.1259(7) 0.0883(14) Uani 0.5 1 d . . P B 2
N3B N 0.6060(4) 0.2112(14) 0.5852(5) 0.1101(15) Uani 0.5 1 d . . P C 2
C33B C 0.5648(5) 0.2536(15) 0.5674(5) 0.0883(14) Uani 0.5 1 d . . P C 2
C30B C 0.5266(11) 0.313(4) 0.5591(16) 0.101(9) Uani 0.5 1 d . . P C 2
C32B C 0.4292(9) 0.282(3) 0.4865(9) 0.097(4) Uani 0.5 1 d . . P C 2
H32B H 0.401438 0.237460 0.454557 0.116 Uiso 0.5 1 calc R U P C 2
N1B N 0.1195(4) -0.0095(15) 0.7375(5) 0.1101(15) Uani 0.5 1 d . . P A 2
C1B C 0.1417(4) 0.0625(17) 0.7211(6) 0.0883(14) Uani 0.5 1 d . . 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 C5 1.357(5) . ?
O1 C8 1.441(4) . ?
O2 C19 1.355(5) . ?
O2 C18 1.451(5) . ?
O3 C27 1.367(5) . ?
O3 C26 1.445(5) . ?
N1A C1A 1.175(16) . ?
N2A C25A 1.133(19) . ?
N3A C33A 1.208(15) . ?
C1A C2 1.380(14) . ?
C2 C7 1.358(7) . ?
C2 C3 1.386(7) . ?
C2 C1B 1.555(15) . ?
C3 C4 1.364(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.378(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(6) . ?
C6 C7 1.369(7) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.496(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C16 1.398(5) . ?
C9 C10 1.408(6) . ?
C10 C12 1.402(6) . ?
C10 C11 1.510(6) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.400(5) . ?
C12 C18 1.498(6) . ?
C13 C15 1.397(6) . ?
C13 C14 1.515(6) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.403(6) . ?
C15 C26 1.505(5) . ?
C16 C17 1.523(6) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C24 1.380(6) . ?
C19 C20 1.392(6) . ?
C20 C21 1.364(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.367(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.400(7) . ?
C22 C25B 1.440(17) . ?
C22 C25A 1.463(17) . ?
C23 C24 1.365(7) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.373(7) . ?
C27 C32A 1.384(18) . ?
C27 C32B 1.44(2) . ?
C32A C31A 1.381(19) . ?
C32A H32A 0.9300 . ?
C31A C30A 1.23(5) . ?
C31A H31A 0.9300 . ?
C30A C29 1.14(3) . ?
C30A C33A 1.60(3) . ?
C29 C28 1.405(7) . ?
C29 C30B 1.51(3) . ?
C29 H29 0.9300 . ?
C28 H28 0.9300 . ?
C31B C32B 1.40(2) . ?
C31B C30B 1.62(4) . ?
C31B H31B 0.9300 . ?
N2B C25B 1.144(19) . ?
N3B C33B 1.181(15) . ?
C33B C30B 1.21(2) . ?
C32B H32B 0.9300 . ?
N1B C1B 1.148(16) . ?

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
C5 O1 C8 117.1(3) . . ?
C19 O2 C18 118.4(3) . . ?
C27 O3 C26 119.9(4) . . ?
N1A C1A C2 169.8(12) . . ?
C7 C2 C1A 115.1(7) . . ?
C7 C2 C3 119.0(5) . . ?
C1A C2 C3 125.1(7) . . ?
C7 C2 C1B 124.1(7) . . ?
C3 C2 C1B 115.1(7) . . ?
C4 C3 C2 120.4(5) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.5(5) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
O1 C5 C4 116.8(4) . . ?
O1 C5 C6 124.2(4) . . ?
C4 C5 C6 119.0(4) . . ?
C7 C6 C5 119.5(4) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C2 C7 C6 121.5(5) . . ?
C2 C7 H7 119.2 . . ?
C6 C7 H7 119.2 . . ?
O1 C8 C9 109.9(3) . . ?
O1 C8 H8A 109.7 . . ?
C9 C8 H8A 109.7 . . ?
O1 C8 H8B 109.7 . . ?
C9 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
C16 C9 C10 120.3(4) . . ?
C16 C9 C8 120.5(4) . . ?
C10 C9 C8 119.2(4) . . ?
C12 C10 C9 118.8(4) . . ?
C12 C10 C11 121.4(4) . . ?
C9 C10 C11 119.8(4) . . ?
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 . . ?
C13 C12 C10 121.5(4) . . ?
C13 C12 C18 119.5(4) . . ?
C10 C12 C18 118.9(4) . . ?
C15 C13 C12 118.7(4) . . ?
C15 C13 C14 120.7(4) . . ?
C12 C13 C14 120.5(4) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 C16 120.8(4) . . ?
C13 C15 C26 120.6(4) . . ?
C16 C15 C26 118.6(4) . . ?
C9 C16 C15 119.7(4) . . ?
C9 C16 C17 119.7(4) . . ?
C15 C16 C17 120.5(4) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O2 C18 C12 106.7(3) . . ?
O2 C18 H18A 110.4 . . ?
C12 C18 H18A 110.4 . . ?
O2 C18 H18B 110.4 . . ?
C12 C18 H18B 110.4 . . ?
H18A C18 H18B 108.6 . . ?
O2 C19 C24 116.4(4) . . ?
O2 C19 C20 124.4(4) . . ?
C24 C19 C20 119.2(4) . . ?
C21 C20 C19 119.9(4) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 121.5(5) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
C21 C22 C23 118.6(5) . . ?
C21 C22 C25B 125.5(8) . . ?
C23 C22 C25B 115.0(8) . . ?
C21 C22 C25A 113.8(7) . . ?
C23 C22 C25A 126.8(8) . . ?
C24 C23 C22 120.3(5) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C19 120.5(5) . . ?
C23 C24 H24 119.8 . . ?
C19 C24 H24 119.8 . . ?
N2A C25A C22 173.2(12) . . ?
O3 C26 C15 105.8(3) . . ?
O3 C26 H26A 110.6 . . ?
C15 C26 H26A 110.6 . . ?
O3 C26 H26B 110.6 . . ?
C15 C26 H26B 110.6 . . ?
H26A C26 H26B 108.7 . . ?
O3 C27 C28 124.7(4) . . ?
O3 C27 C32A 122.3(9) . . ?
C28 C27 C32A 112.2(9) . . ?
O3 C27 C32B 107.2(10) . . ?
C28 C27 C32B 126.8(10) . . ?
C31A C32A C27 120.4(13) . . ?
C31A C32A H32A 119.8 . . ?
C27 C32A H32A 119.8 . . ?
C30A C31A C32A 118.5(19) . . ?
C30A C31A H31A 120.8 . . ?
C32A C31A H31A 120.8 . . ?
C29 C30A C31A 128(3) . . ?
C29 C30A C33A 114(3) . . ?
C31A C30A C33A 117(2) . . ?
C30A C29 C28 120(2) . . ?
C28 C29 C30B 121.7(14) . . ?
C30A C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C27 C28 C29 120.1(6) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
N3A C33A C30A 175.8(18) . . ?
C32B C31B C30B 123.7(16) . . ?
C32B C31B H31B 118.1 . . ?
C30B C31B H31B 118.1 . . ?
N2B C25B C22 170.9(12) . . ?
N3B C33B C30B 168(2) . . ?
C33B C30B C29 134(3) . . ?
C33B C30B C31B 113(2) . . ?
C29 C30B C31B 111.4(16) . . ?
C31B C32B C27 114.0(17) . . ?
C31B C32B H32B 123.0 . . ?
C27 C32B H32B 123.0 . . ?
N1B C1B C2 173.2(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1A C1A C2 C7 -113(8) . . . . ?
N1A C1A C2 C3 77(8) . . . . ?
C7 C2 C3 C4 0.8(10) . . . . ?
C1A C2 C3 C4 170.2(8) . . . . ?
C1B C2 C3 C4 -164.5(7) . . . . ?
C2 C3 C4 C5 0.6(9) . . . . ?
C8 O1 C5 C4 -160.0(4) . . . . ?
C8 O1 C5 C6 19.0(6) . . . . ?
C3 C4 C5 O1 177.0(5) . . . . ?
C3 C4 C5 C6 -2.1(8) . . . . ?
O1 C5 C6 C7 -176.7(5) . . . . ?
C4 C5 C6 C7 2.3(8) . . . . ?
C1A C2 C7 C6 -171.0(8) . . . . ?
C3 C2 C7 C6 -0.6(10) . . . . ?
C1B C2 C7 C6 163.3(7) . . . . ?
C5 C6 C7 C2 -0.9(9) . . . . ?
C5 O1 C8 C9 165.0(4) . . . . ?
O1 C8 C9 C16 115.5(4) . . . . ?
O1 C8 C9 C10 -67.3(5) . . . . ?
C16 C9 C10 C12 1.4(5) . . . . ?
C8 C9 C10 C12 -175.9(3) . . . . ?
C16 C9 C10 C11 -179.8(4) . . . . ?
C8 C9 C10 C11 3.0(5) . . . . ?
C9 C10 C12 C13 1.7(5) . . . . ?
C11 C10 C12 C13 -177.1(4) . . . . ?
C9 C10 C12 C18 -179.7(3) . . . . ?
C11 C10 C12 C18 1.5(5) . . . . ?
C10 C12 C13 C15 -2.8(5) . . . . ?
C18 C12 C13 C15 178.6(3) . . . . ?
C10 C12 C13 C14 175.2(4) . . . . ?
C18 C12 C13 C14 -3.4(5) . . . . ?
C12 C13 C15 C16 0.8(5) . . . . ?
C14 C13 C15 C16 -177.2(4) . . . . ?
C12 C13 C15 C26 179.4(3) . . . . ?
C14 C13 C15 C26 1.4(5) . . . . ?
C10 C9 C16 C15 -3.3(5) . . . . ?
C8 C9 C16 C15 173.9(3) . . . . ?
C10 C9 C16 C17 178.1(3) . . . . ?
C8 C9 C16 C17 -4.7(5) . . . . ?
C13 C15 C16 C9 2.3(5) . . . . ?
C26 C15 C16 C9 -176.4(3) . . . . ?
C13 C15 C16 C17 -179.2(3) . . . . ?
C26 C15 C16 C17 2.2(5) . . . . ?
C19 O2 C18 C12 178.2(4) . . . . ?
C13 C12 C18 O2 90.2(4) . . . . ?
C10 C12 C18 O2 -88.4(4) . . . . ?
C18 O2 C19 C24 -178.5(4) . . . . ?
C18 O2 C19 C20 1.3(6) . . . . ?
O2 C19 C20 C21 179.4(4) . . . . ?
C24 C19 C20 C21 -0.8(7) . . . . ?
C19 C20 C21 C22 1.6(8) . . . . ?
C20 C21 C22 C23 -2.0(8) . . . . ?
C20 C21 C22 C25B -170.5(7) . . . . ?
C20 C21 C22 C25A 168.6(7) . . . . ?
C21 C22 C23 C24 1.7(8) . . . . ?
C25B C22 C23 C24 171.4(7) . . . . ?
C25A C22 C23 C24 -167.5(7) . . . . ?
C22 C23 C24 C19 -1.0(8) . . . . ?
O2 C19 C24 C23 -179.6(5) . . . . ?
C20 C19 C24 C23 0.5(7) . . . . ?
C27 O3 C26 C15 -154.3(4) . . . . ?
C13 C15 C26 O3 -99.5(4) . . . . ?
C16 C15 C26 O3 79.2(5) . . . . ?
C26 O3 C27 C28 -4.7(7) . . . . ?
C26 O3 C27 C32A 164.4(8) . . . . ?
C26 O3 C27 C32B -172.3(8) . . . . ?
O3 C27 C32A C31A 179.4(10) . . . . ?
C28 C27 C32A C31A -10.2(15) . . . . ?
C27 C32A C31A C30A 4(3) . . . . ?
C32A C31A C30A C29 5(5) . . . . ?
C32A C31A C30A C33A 174.8(16) . . . . ?
C31A C30A C29 C28 -6(5) . . . . ?
C33A C30A C29 C28 -176.2(13) . . . . ?
O3 C27 C28 C29 179.2(5) . . . . ?
C32A C27 C28 C29 9.1(10) . . . . ?
C32B C27 C28 C29 -15.7(12) . . . . ?
C30A C29 C28 C27 -2(2) . . . . ?
C30B C29 C28 C27 1.5(15) . . . . ?
N3B C33B C30B C29 30(11) . . . . ?
N3B C33B C30B C31B -164(8) . . . . ?
C28 C29 C30B C33B 174(3) . . . . ?
C28 C29 C30B C31B 8(2) . . . . ?
C32B C31B C30B C33B -174.7(18) . . . . ?
C32B C31B C30B C29 -6(3) . . . . ?
C30B C31B C32B C27 -5(2) . . . . ?
O3 C27 C32B C31B -175.7(11) . . . . ?
C28 C27 C32B C31B 17.1(17) . . . . ?

_refine_diff_density_max         0.299
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.049




_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetone acetonitrile'
####################################################################### 
# 
# 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_POD_Br
_database_code_depnum_ccdc_archive 'CCDC 2268770'
loop_
_audit_author_name
_audit_author_address
'Sandeep Kumar Dey'
;CSIR Northeast Institute of Science and Technology Jorhat
India
;
_audit_update_record             
;
2023-06-09 deposited with the CCDC.	2023-09-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/2
_shelx_SHELXL_version_number     2019/2
_chemical_name_systematic        1,3,5-tris(4-bromo-phenoxymethyl)mesitylene
_chemical_name_common            ?
_chemical_melting_point          553
_chemical_formula_moiety         ?
_chemical_formula_sum            'C63 H60 Br6 O7'
_chemical_formula_weight         1408.57

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.4811(15)
_cell_length_b                   12.591(2)
_cell_length_c                   13.809(2)
_cell_angle_alpha                107.591(5)
_cell_angle_beta                 95.204(5)
_cell_angle_gamma                91.591(5)
_cell_volume                     1562.3(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9930
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      28.52

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_F_000             704
_exptl_transmission_factor_min   0.4993
_exptl_transmission_factor_max   0.7457
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    3.904
_shelx_estimated_absorpt_T_min   0.430
_shelx_estimated_absorpt_T_max   0.494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-III photon detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43245
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.528
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5502
_reflns_number_gt                3486
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    ?
_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)+(0.1454P)²+5.6747P] 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_number_reflns         5502
_refine_ls_number_parameters     332
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0839
_refine_ls_wR_factor_ref         0.2816
_refine_ls_wR_factor_gt          0.2442
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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 1.33652(10) 0.40652(12) 0.92256(9) 0.0935(5) Uani 1 1 d . . . . .
Br2 Br 0.33542(16) -0.25088(12) -0.00469(10) 0.1074(5) Uani 1 1 d . . . . .
Br3 Br 0.10443(14) 1.12399(9) 0.67739(13) 0.1070(5) Uani 1 1 d . . . . .
O1 O 0.7592(6) 0.4023(6) 0.7005(5) 0.0689(17) Uani 1 1 d . . . . .
O2 O 0.3908(7) 0.1503(6) 0.3700(5) 0.0777(19) Uani 1 1 d . . . . .
O3 O 0.2230(6) 0.6451(5) 0.6317(5) 0.0617(15) Uani 1 1 d . . . . .
O4 O 1.130989 0.264400 1.132969 0.120 Uiso 0.5 1 d . U P . .
C1 C 1.1526(9) 0.4078(7) 0.8568(7) 0.059(2) Uani 1 1 d . . . . .
C2 C 1.1413(9) 0.4197(9) 0.7611(8) 0.075(3) Uani 1 1 d . . . . .
H2 H 1.221730 0.427519 0.729477 0.090 Uiso 1 1 calc R U . . .
C3 C 1.0058(9) 0.4197(10) 0.7124(8) 0.079(3) Uani 1 1 d . . . . .
H3 H 0.995694 0.430302 0.648387 0.095 Uiso 1 1 calc R U . . .
C4 C 0.8859(7) 0.4041(7) 0.7583(6) 0.0492(18) Uani 1 1 d . . . . .
C5 C 0.9007(8) 0.3933(8) 0.8523(7) 0.059(2) Uani 1 1 d . . . . .
H5 H 0.820566 0.386136 0.884529 0.070 Uiso 1 1 calc R U . . .
C6 C 1.0353(8) 0.3927(8) 0.9021(7) 0.060(2) Uani 1 1 d . . . . .
H6 H 1.044822 0.381973 0.966115 0.072 Uiso 1 1 calc R U . . .
C7 C 0.6298(8) 0.3897(8) 0.7456(7) 0.059(2) Uani 1 1 d . . . . .
H7A H 0.622464 0.452220 0.806224 0.071 Uiso 1 1 calc R U . . .
H7B H 0.627508 0.321298 0.764086 0.071 Uiso 1 1 calc R U . . .
C8 C 0.5108(7) 0.3861(7) 0.6642(6) 0.0506(19) Uani 1 1 d . . . . .
C9 C 0.4545(8) 0.2828(7) 0.5983(7) 0.054(2) Uani 1 1 d . . . . .
C10 C 0.5117(10) 0.1750(8) 0.6073(8) 0.072(3) Uani 1 1 d . . . . .
H10A H 0.613528 0.181483 0.614776 0.107 Uiso 1 1 calc R U . . .
H10B H 0.478920 0.114980 0.546908 0.107 Uiso 1 1 calc R U . . .
H10C H 0.479052 0.159913 0.665895 0.107 Uiso 1 1 calc R U . . .
C11 C 0.3430(8) 0.2823(7) 0.5218(6) 0.0518(19) Uani 1 1 d . . . . .
C12 C 0.2930(7) 0.3792(7) 0.5115(6) 0.0491(18) Uani 1 1 d . . . . .
C13 C 0.1687(10) 0.3769(9) 0.4329(8) 0.075(3) Uani 1 1 d . . . . .
H13A H 0.201411 0.360217 0.366412 0.112 Uiso 1 1 calc R U . . .
H13B H 0.128134 0.448393 0.449845 0.112 Uiso 1 1 calc R U . . .
H13C H 0.098232 0.320622 0.432792 0.112 Uiso 1 1 calc R U . . .
C14 C 0.3566(7) 0.4843(7) 0.5753(6) 0.0493(18) Uani 1 1 d . . . . .
C15 C 0.4628(7) 0.4865(7) 0.6527(6) 0.0509(19) Uani 1 1 d . . . . .
C16 C 0.5245(10) 0.5955(8) 0.7229(8) 0.073(3) Uani 1 1 d . . . . .
H16A H 0.494695 0.654432 0.696486 0.110 Uiso 1 1 calc R U . . .
H16B H 0.626159 0.595110 0.728456 0.110 Uiso 1 1 calc R U . . .
H16C H 0.492544 0.607173 0.789184 0.110 Uiso 1 1 calc R U . . .
C17 C 0.2924(9) 0.1716(7) 0.4456(7) 0.059(2) Uani 1 1 d . . . . .
H17A H 0.292154 0.113324 0.478248 0.070 Uiso 1 1 calc R U . . .
H17B H 0.197115 0.175042 0.414919 0.070 Uiso 1 1 calc R U . . .
C18 C 0.3705(9) 0.0556(8) 0.2880(7) 0.064(2) Uani 1 1 d . . . . .
C19 C 0.4793(12) 0.0356(12) 0.2270(9) 0.104(4) Uani 1 1 d . . . . .
H19 H 0.559946 0.083925 0.243504 0.124 Uiso 1 1 calc R U . . .
C20 C 0.4687(13) -0.0559(12) 0.1416(10) 0.105(4) Uani 1 1 d . . . . .
H20 H 0.544026 -0.070673 0.101730 0.126 Uiso 1 1 calc R U . . .
C21 C 0.3484(11) -0.1261(9) 0.1141(8) 0.078(3) Uani 1 1 d . . . . .
C22 C 0.2401(10) -0.1047(8) 0.1760(7) 0.068(2) Uani 1 1 d . . . . .
H22 H 0.157974 -0.151368 0.158318 0.082 Uiso 1 1 calc R U . . .
C23 C 0.2518(9) -0.0156(7) 0.2634(7) 0.063(2) Uani 1 1 d . . . . .
H23 H 0.179287 -0.003484 0.305928 0.076 Uiso 1 1 calc R U . . .
C24 C 0.3145(9) 0.5896(7) 0.5565(7) 0.060(2) Uani 1 1 d . . . . .
H24A H 0.398256 0.637538 0.561014 0.072 Uiso 1 1 calc R U . . .
H24B H 0.265186 0.573327 0.488545 0.072 Uiso 1 1 calc R U . . .
C25 C 0.1940(8) 0.7526(7) 0.6363(7) 0.055(2) Uani 1 1 d . . . . .
C26 C 0.2047(10) 0.7965(7) 0.5561(7) 0.062(2) Uani 1 1 d . . . . .
H26 H 0.232175 0.752237 0.494473 0.075 Uiso 1 1 calc R U . . .
C27 C 0.1746(11) 0.9056(8) 0.5683(9) 0.077(3) Uani 1 1 d . . . . .
H27 H 0.179221 0.934296 0.513994 0.092 Uiso 1 1 calc R U . . .
C28 C 0.1381(10) 0.9719(8) 0.6590(9) 0.068(2) Uani 1 1 d . . . . .
C29 C 0.1254(10) 0.9283(9) 0.7375(8) 0.078(3) Uani 1 1 d . . . . .
H29 H 0.098027 0.973295 0.798872 0.094 Uiso 1 1 calc R U . . .
C30 C 0.1527(9) 0.8184(9) 0.7271(8) 0.070(2) Uani 1 1 d . . . . .
H30 H 0.143231 0.789353 0.780693 0.084 Uiso 1 1 calc R U . . .
C31 C 1.122030 0.178050 1.064751 0.114(9) Uiso 0.5 1 d . . P . .
C32 C 0.984179 0.116241 1.032200 0.137(11) Uiso 0.5 1 d . . P . .
H32A H 0.987894 0.046570 1.047021 0.206 Uiso 0.5 1 calc R U P . .
H32B H 0.961661 0.102195 0.960079 0.206 Uiso 0.5 1 calc R U P . .
H32C H 0.912550 0.159408 1.068145 0.206 Uiso 0.5 1 calc R U P . .
C33 C 1.250381 0.137190 1.017731 0.140 Uiso 0.5 1 d . U P . .
H33A H 1.272039 0.177830 0.971740 0.210 Uiso 0.5 1 calc R U P . .
H33B H 1.235138 0.059225 0.980653 0.210 Uiso 0.5 1 calc R U P . .
H33C H 1.328131 0.147721 1.069966 0.210 Uiso 0.5 1 calc R U P . .


_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 C1 1.894(8) . ?
Br2 C21 1.889(11) . ?
Br3 C28 1.894(9) . ?
O1 C4 1.376(9) . ?
O1 C7 1.451(9) . ?
O2 C18 1.368(11) . ?
O2 C17 1.434(10) . ?
O3 C25 1.373(10) . ?
O3 C24 1.442(10) . ?
O4 C31 1.19918(16) . ?
C1 C6 1.361(12) . ?
C1 C2 1.369(13) . ?
C2 C3 1.395(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.387(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.341(12) . ?
C5 C6 1.396(11) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.508(11) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.401(12) . ?
C8 C15 1.403(11) . ?
C9 C11 1.423(11) . ?
C9 C10 1.511(12) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.364(11) . ?
C11 C17 1.505(12) . ?
C12 C14 1.430(11) . ?
C12 C13 1.521(11) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.394(11) . ?
C14 C24 1.484(12) . ?
C15 C16 1.488(12) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C23 1.370(12) . ?
C18 C19 1.371(13) . ?
C19 C20 1.371(16) . ?
C19 H19 0.9300 . ?
C20 C21 1.375(15) . ?
C20 H20 0.9300 . ?
C21 C22 1.375(13) . ?
C22 C23 1.371(13) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C30 1.375(13) . ?
C25 C26 1.388(12) . ?
C26 C27 1.374(13) . ?
C26 H26 0.9300 . ?
C27 C28 1.359(14) . ?
C27 H27 0.9300 . ?
C28 C29 1.368(15) . ?
C29 C30 1.381(15) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 C32 1.4634(2) . ?
C31 C33 1.46402(18) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 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 O1 C7 117.4(6) . . ?
C18 O2 C17 119.4(6) . . ?
C25 O3 C24 116.4(6) . . ?
C6 C1 C2 121.2(8) . . ?
C6 C1 Br1 120.6(7) . . ?
C2 C1 Br1 118.2(6) . . ?
C1 C2 C3 118.2(8) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C4 C3 C2 120.8(8) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C5 C4 O1 125.7(7) . . ?
C5 C4 C3 119.5(7) . . ?
O1 C4 C3 114.8(7) . . ?
C4 C5 C6 120.5(8) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C5 119.8(8) . . ?
C1 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
O1 C7 C8 105.3(6) . . ?
O1 C7 H7A 110.7 . . ?
C8 C7 H7A 110.7 . . ?
O1 C7 H7B 110.7 . . ?
C8 C7 H7B 110.7 . . ?
H7A C7 H7B 108.8 . . ?
C9 C8 C15 121.1(7) . . ?
C9 C8 C7 119.5(7) . . ?
C15 C8 C7 119.4(7) . . ?
C8 C9 C11 118.1(7) . . ?
C8 C9 C10 121.0(8) . . ?
C11 C9 C10 120.9(8) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C9 121.3(8) . . ?
C12 C11 C17 120.7(8) . . ?
C9 C11 C17 117.6(7) . . ?
C11 C12 C14 120.1(7) . . ?
C11 C12 C13 120.6(8) . . ?
C14 C12 C13 119.3(7) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C12 119.2(7) . . ?
C15 C14 C24 120.3(7) . . ?
C12 C14 C24 120.4(7) . . ?
C14 C15 C8 119.9(7) . . ?
C14 C15 C16 119.7(8) . . ?
C8 C15 C16 120.3(8) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O2 C17 C11 105.5(6) . . ?
O2 C17 H17A 110.6 . . ?
C11 C17 H17A 110.6 . . ?
O2 C17 H17B 110.6 . . ?
C11 C17 H17B 110.6 . . ?
H17A C17 H17B 108.8 . . ?
O2 C18 C23 125.1(8) . . ?
O2 C18 C19 114.9(8) . . ?
C23 C18 C19 120.0(9) . . ?
C20 C19 C18 119.7(11) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 121.0(10) . . ?
C19 C20 H20 119.5 . . ?
C21 C20 H20 119.5 . . ?
C20 C21 C22 118.6(10) . . ?
C20 C21 Br2 120.2(8) . . ?
C22 C21 Br2 121.2(8) . . ?
C23 C22 C21 120.9(9) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C18 C23 C22 119.8(9) . . ?
C18 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
O3 C24 C14 109.1(7) . . ?
O3 C24 H24A 109.9 . . ?
C14 C24 H24A 109.9 . . ?
O3 C24 H24B 109.9 . . ?
C14 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
O3 C25 C30 116.2(8) . . ?
O3 C25 C26 124.0(8) . . ?
C30 C25 C26 119.8(8) . . ?
C27 C26 C25 119.7(9) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C28 C27 C26 120.7(10) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C27 C28 C29 119.6(9) . . ?
C27 C28 Br3 120.6(8) . . ?
C29 C28 Br3 119.8(8) . . ?
C28 C29 C30 121.0(9) . . ?
C28 C29 H29 119.5 . . ?
C30 C29 H29 119.5 . . ?
C25 C30 C29 119.1(10) . . ?
C25 C30 H30 120.5 . . ?
C29 C30 H30 120.5 . . ?
O4 C31 C32 119.155(7) . . ?
O4 C31 C33 118.672(8) . . ?
C32 C31 C33 122.166(10) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 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
C6 C1 C2 C3 2.1(15) . . . . ?
Br1 C1 C2 C3 179.5(8) . . . . ?
C1 C2 C3 C4 -2.2(17) . . . . ?
C7 O1 C4 C5 1.2(13) . . . . ?
C7 O1 C4 C3 -178.2(9) . . . . ?
C2 C3 C4 C5 2.6(16) . . . . ?
C2 C3 C4 O1 -177.9(10) . . . . ?
O1 C4 C5 C6 177.8(8) . . . . ?
C3 C4 C5 C6 -2.8(14) . . . . ?
C2 C1 C6 C5 -2.4(14) . . . . ?
Br1 C1 C6 C5 -179.7(7) . . . . ?
C4 C5 C6 C1 2.7(14) . . . . ?
C4 O1 C7 C8 -177.8(7) . . . . ?
O1 C7 C8 C9 93.9(9) . . . . ?
O1 C7 C8 C15 -83.3(9) . . . . ?
C15 C8 C9 C11 -2.4(11) . . . . ?
C7 C8 C9 C11 -179.5(7) . . . . ?
C15 C8 C9 C10 176.8(8) . . . . ?
C7 C8 C9 C10 -0.3(11) . . . . ?
C8 C9 C11 C12 0.8(11) . . . . ?
C10 C9 C11 C12 -178.4(8) . . . . ?
C8 C9 C11 C17 174.6(7) . . . . ?
C10 C9 C11 C17 -4.6(11) . . . . ?
C9 C11 C12 C14 2.8(12) . . . . ?
C17 C11 C12 C14 -170.8(7) . . . . ?
C9 C11 C12 C13 -176.9(8) . . . . ?
C17 C11 C12 C13 9.5(12) . . . . ?
C11 C12 C14 C15 -4.8(11) . . . . ?
C13 C12 C14 C15 174.9(7) . . . . ?
C11 C12 C14 C24 172.7(7) . . . . ?
C13 C12 C14 C24 -7.7(11) . . . . ?
C12 C14 C15 C8 3.1(11) . . . . ?
C24 C14 C15 C8 -174.3(7) . . . . ?
C12 C14 C15 C16 -176.9(7) . . . . ?
C24 C14 C15 C16 5.7(11) . . . . ?
C9 C8 C15 C14 0.4(11) . . . . ?
C7 C8 C15 C14 177.6(7) . . . . ?
C9 C8 C15 C16 -179.6(7) . . . . ?
C7 C8 C15 C16 -2.5(11) . . . . ?
C18 O2 C17 C11 -178.3(8) . . . . ?
C12 C11 C17 O2 91.8(9) . . . . ?
C9 C11 C17 O2 -82.1(9) . . . . ?
C17 O2 C18 C23 9.3(15) . . . . ?
C17 O2 C18 C19 -172.1(10) . . . . ?
O2 C18 C19 C20 -178.8(13) . . . . ?
C23 C18 C19 C20 0(2) . . . . ?
C18 C19 C20 C21 2(2) . . . . ?
C19 C20 C21 C22 -2(2) . . . . ?
C19 C20 C21 Br2 179.3(12) . . . . ?
C20 C21 C22 C23 -0.2(17) . . . . ?
Br2 C21 C22 C23 178.4(8) . . . . ?
O2 C18 C23 C22 176.4(9) . . . . ?
C19 C18 C23 C22 -2.1(16) . . . . ?
C21 C22 C23 C18 2.3(16) . . . . ?
C25 O3 C24 C14 169.2(7) . . . . ?
C15 C14 C24 O3 -78.6(9) . . . . ?
C12 C14 C24 O3 104.0(9) . . . . ?
C24 O3 C25 C30 -157.3(8) . . . . ?
C24 O3 C25 C26 22.4(12) . . . . ?
O3 C25 C26 C27 -179.4(8) . . . . ?
C30 C25 C26 C27 0.3(14) . . . . ?
C25 C26 C27 C28 1.8(15) . . . . ?
C26 C27 C28 C29 -2.8(16) . . . . ?
C26 C27 C28 Br3 177.3(8) . . . . ?
C27 C28 C29 C30 1.7(15) . . . . ?
Br3 C28 C29 C30 -178.4(7) . . . . ?
O3 C25 C30 C29 178.4(8) . . . . ?
C26 C25 C30 C29 -1.4(13) . . . . ?
C28 C29 C30 C25 0.4(14) . . . . ?

_refine_diff_density_max         1.011
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.132

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetone ethanol'
