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

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

data_tc001
_database_code_depnum_ccdc_archive 'CCDC 2441440'
loop_
_audit_author_name
_audit_author_address
'Alexandre Sobolev'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2025-04-07 deposited with the CCDC.	2025-10-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C82 H118 Br2 O18 P4'
_chemical_formula_sum            'C82 H118 Br2 O18 P4'
_chemical_formula_weight         1675.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      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                   12.827(2)
_cell_length_b                   13.724(2)
_cell_length_c                   15.005(2)
_cell_angle_alpha                66.640(2)
_cell_angle_beta                 88.465(2)
_cell_angle_gamma                64.722(2)
_cell_volume                     2160.2(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4462
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      24.98

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_F_000             884
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.075
_exptl_absorpt_coefficient_mu    1.076
_shelx_estimated_absorpt_T_min   0.673
_shelx_estimated_absorpt_T_max   0.924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6728
_exptl_absorpt_correction_T_max  0.9237
_exptl_absorpt_process_details   
'SADABS - Bruker area detector absorption corrections'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15847
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.501
_diffrn_reflns_theta_max         25.042
_diffrn_reflns_theta_full        25.042
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             7571
_reflns_number_gt                4915
_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 SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL, v. 5.1'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'X-Seed v. 4.0 (Barbour, 2020)'
_computing_publication_material  'SHELXL-2019/2 (Sheldrick, 2019)'
_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)+(0.0500P)²+13.4000P] 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         7571
_refine_ls_number_parameters     496
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.0810
_refine_ls_wR_factor_ref         0.2110
_refine_ls_wR_factor_gt          0.1880
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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 0.2909(3) 0.3605(3) 0.3327(3) 0.0332(9) Uani 1 1 d . . . . .
C1 C 0.4325(6) 0.4171(5) 0.1938(4) 0.0356(13) Uani 1 1 d . . . . .
H1A H 0.357993 0.424485 0.168056 0.043 Uiso 1 1 calc R U . . .
H1B H 0.487422 0.402116 0.147705 0.043 Uiso 1 1 calc R U . . .
C11 C 0.4094(5) 0.2858(5) 0.3604(4) 0.0301(12) Uani 1 1 d . . . . .
C12 C 0.4830(5) 0.3108(5) 0.2940(4) 0.0301(12) Uani 1 1 d . . . . .
C13 C 0.6012(5) 0.2367(5) 0.3210(4) 0.0342(13) Uani 1 1 d . . . . .
H13 H 0.652306 0.253562 0.277109 0.041 Uiso 1 1 calc R U . . .
C14 C 0.6477(5) 0.1368(5) 0.4117(4) 0.0327(13) Uani 1 1 d . . . . .
C15 C 0.5739(5) 0.1156(5) 0.4788(4) 0.0313(12) Uani 1 1 d . . . . .
H15 H 0.605814 0.049543 0.541467 0.038 Uiso 1 1 calc R U . . .
C16 C 0.4536(5) 0.1905(5) 0.4548(4) 0.0297(12) Uani 1 1 d . . . . .
C17 C 0.2244(5) 0.3122(6) 0.3028(5) 0.0429(15) Uani 1 1 d . . . . .
H17A H 0.226814 0.242175 0.359819 0.051 Uiso 1 1 calc R U . . .
H17B H 0.258307 0.286584 0.251157 0.051 Uiso 1 1 calc R U . . .
C18 C 0.1023(6) 0.4065(7) 0.2643(6) 0.064(2) Uani 1 1 d D . . . .
H18A H 0.058295 0.380011 0.233761 0.077 Uiso 1 1 calc R U . A 1
H18B H 0.101733 0.479344 0.212633 0.077 Uiso 1 1 calc R U . A 1
C19 C 0.043(4) 0.435(5) 0.345(2) 0.082(9) Uani 0.5 1 d D . P B 1
H19A H 0.088418 0.460652 0.374496 0.099 Uiso 0.5 1 calc R U P B 1
H19B H 0.047246 0.360126 0.396877 0.099 Uiso 0.5 1 calc R U P B 1
C20 C -0.083(3) 0.528(3) 0.317(2) 0.082(6) Uani 0.5 1 d D U P B 1
H20A H -0.111742 0.538423 0.375698 0.124 Uiso 0.5 1 calc R U P B 1
H20B H -0.089654 0.604120 0.267517 0.124 Uiso 0.5 1 calc R U P B 1
H20C H -0.130994 0.503185 0.289988 0.124 Uiso 0.5 1 calc R U P B 1
C19' C 0.037(4) 0.465(5) 0.328(3) 0.082(9) Uani 0.5 1 d D . P B 2
H19C H 0.078403 0.503094 0.345469 0.099 Uiso 0.5 1 calc R U P B 2
H19D H 0.033315 0.403743 0.390450 0.099 Uiso 0.5 1 calc R U P B 2
C20' C -0.086(3) 0.557(3) 0.2749(19) 0.082(6) Uani 0.5 1 d D . P B 2
H20G H -0.127854 0.594581 0.317052 0.124 Uiso 0.5 1 calc R U P B 2
H20H H -0.081948 0.617736 0.213976 0.124 Uiso 0.5 1 calc R U P B 2
H20I H -0.126941 0.518594 0.258863 0.124 Uiso 0.5 1 calc R U P B 2
P1 P 0.80254(13) 0.03702(13) 0.43933(12) 0.0352(4) Uani 1 1 d . . . . .
O11 O 0.8724(4) 0.0978(4) 0.3969(4) 0.0592(13) Uani 1 1 d . . . . .
O12 O 0.8297(4) -0.0408(4) 0.5492(4) 0.0542(12) Uani 1 1 d . . . . .
C121 C 0.8538(7) 0.0020(7) 0.6177(5) 0.066(2) Uani 1 1 d D . . . .
H12A H 0.802774 0.088731 0.592937 0.080 Uiso 1 1 calc R U . C 1
H12B H 0.936187 -0.011805 0.621817 0.080 Uiso 1 1 calc R U . C 1
C122 C 0.832(2) -0.061(2) 0.7178(11) 0.090(7) Uani 0.5 1 d D . P D 1
H12C H 0.848797 -0.031628 0.762685 0.136 Uiso 0.5 1 calc R U P D 1
H12D H 0.750446 -0.046578 0.713823 0.136 Uiso 0.5 1 calc R U P D 1
H12E H 0.883649 -0.146957 0.742657 0.136 Uiso 0.5 1 calc R U P D 1
C12' C 0.9072(18) -0.098(2) 0.7183(11) 0.090(7) Uani 0.5 1 d D . P D 2
H12F H 0.922553 -0.067321 0.762938 0.136 Uiso 0.5 1 calc R U P D 2
H12G H 0.853079 -0.131659 0.742902 0.136 Uiso 0.5 1 calc R U P D 2
H12H H 0.980799 -0.159468 0.714986 0.136 Uiso 0.5 1 calc R U P D 2
O13 O 0.8049(4) -0.0520(4) 0.3945(3) 0.0516(11) Uani 1 1 d . . . . .
C131 C 0.9167(6) -0.1401(7) 0.3910(7) 0.065(2) Uani 1 1 d . . . . .
H13A H 0.964831 -0.188856 0.457746 0.078 Uiso 1 1 calc R U . . .
H13B H 0.959005 -0.100126 0.346984 0.078 Uiso 1 1 calc R U . . .
C132 C 0.8974(7) -0.2178(7) 0.3537(6) 0.067(2) Uani 1 1 d . . . . .
H13C H 0.973113 -0.277719 0.351261 0.100 Uiso 1 1 calc R U . . .
H13D H 0.856164 -0.257692 0.397956 0.100 Uiso 1 1 calc R U . . .
H13E H 0.850354 -0.169197 0.287486 0.100 Uiso 1 1 calc R U . . .
O2 O 0.3377(3) 0.3485(3) 0.5866(3) 0.0336(9) Uani 1 1 d . . . . .
C2 C 0.3729(5) 0.1687(5) 0.5270(4) 0.0317(12) Uani 1 1 d . . . . .
H2A H 0.360949 0.101564 0.528180 0.038 Uiso 1 1 calc R U . . .
H2B H 0.295894 0.240232 0.503078 0.038 Uiso 1 1 calc R U . . .
C21 C 0.3988(5) 0.2327(5) 0.6579(4) 0.0300(12) Uani 1 1 d . . . . .
C22 C 0.4166(5) 0.1406(5) 0.6312(4) 0.0290(12) Uani 1 1 d . . . . .
C23 C 0.4694(5) 0.0246(5) 0.7041(4) 0.0334(13) Uani 1 1 d . . . . .
H23 H 0.483059 -0.039319 0.687425 0.040 Uiso 1 1 calc R U . . .
C24 C 0.5029(5) 0.0000(5) 0.8015(4) 0.0345(13) Uani 1 1 d . . . . .
C25 C 0.4834(5) 0.0946(5) 0.8252(4) 0.0363(13) Uani 1 1 d . . . . .
H25 H 0.505330 0.078457 0.891415 0.044 Uiso 1 1 calc R U . . .
C26 C 0.4328(5) 0.2114(5) 0.7539(4) 0.0320(12) Uani 1 1 d . . . . .
C27 C 0.4081(5) 0.4053(5) 0.5393(4) 0.0359(13) Uani 1 1 d . . . . .
H27A H 0.471245 0.353352 0.515778 0.043 Uiso 1 1 calc R U . . .
H27B H 0.444342 0.420795 0.586303 0.043 Uiso 1 1 calc R U . . .
C28 C 0.3295(6) 0.5214(5) 0.4532(5) 0.0459(16) Uani 1 1 d . . . . .
H28A H 0.378106 0.559430 0.418149 0.055 Uiso 1 1 calc R U . . .
H28B H 0.295662 0.503347 0.406746 0.055 Uiso 1 1 calc R U . . .
C29 C 0.2309(7) 0.6095(6) 0.4796(6) 0.062(2) Uani 1 1 d . . . . .
H29A H 0.180155 0.677873 0.418098 0.074 Uiso 1 1 calc R U . . .
H29B H 0.183172 0.571189 0.516080 0.074 Uiso 1 1 calc R U . . .
C30 C 0.2703(8) 0.6551(7) 0.5408(6) 0.076(2) Uani 1 1 d . . . . .
H30A H 0.201848 0.711694 0.555076 0.115 Uiso 1 1 calc R U . . .
H30B H 0.319004 0.588312 0.602731 0.115 Uiso 1 1 calc R U . . .
H30C H 0.315983 0.695136 0.504620 0.115 Uiso 1 1 calc R U . . .
P2 P 0.55712(16) -0.14804(13) 0.89692(11) 0.0414(4) Uani 1 1 d . . . . .
O21 O 0.6143(5) -0.2395(4) 0.8626(3) 0.0595(13) Uani 1 1 d . . . . .
O22 O 0.6311(4) -0.1525(4) 0.9821(3) 0.0462(11) Uani 1 1 d . . . . .
C221 C 0.7459(8) -0.1625(9) 0.9714(7) 0.079(2) Uani 1 1 d . . . . .
H22A H 0.799696 -0.244320 0.980139 0.095 Uiso 1 1 calc R U . . .
H22B H 0.743897 -0.106627 0.904005 0.095 Uiso 1 1 calc R U . . .
C222 C 0.7889(11) -0.1368(14) 1.0412(11) 0.148(6) Uani 1 1 d . . . . .
H22C H 0.867449 -0.144458 1.031917 0.222 Uiso 1 1 calc R U . . .
H22D H 0.736510 -0.055374 1.031848 0.222 Uiso 1 1 calc R U . . .
H22E H 0.792265 -0.192959 1.107923 0.222 Uiso 1 1 calc R U . . .
O23 O 0.4512(5) -0.1536(4) 0.9532(3) 0.0567(12) Uani 1 1 d D . . . .
C231 C 0.3672(15) -0.1513(18) 0.8873(10) 0.066(3) Uani 0.5 1 d D . P E 1
H23A H 0.407898 -0.217577 0.867899 0.079 Uiso 0.5 1 calc R U P E 1
H23B H 0.338187 -0.075833 0.826715 0.079 Uiso 0.5 1 calc R U P E 1
C232 C 0.2662(18) -0.162(3) 0.9316(16) 0.125(7) Uani 0.5 1 d D . P E 1
H23C H 0.213577 -0.159688 0.883941 0.188 Uiso 0.5 1 calc R U P E 1
H23D H 0.293917 -0.237290 0.990714 0.188 Uiso 0.5 1 calc R U P E 1
H23E H 0.224142 -0.095417 0.949492 0.188 Uiso 0.5 1 calc R U P E 1
C23' C 0.3729(14) -0.2009(14) 0.9385(12) 0.066(3) Uani 0.5 1 d D . P E 2
H23F H 0.353128 -0.241365 1.002611 0.079 Uiso 0.5 1 calc R U P E 2
H23G H 0.412999 -0.260259 0.911742 0.079 Uiso 0.5 1 calc R U P E 2
C23" C 0.2619(16) -0.101(2) 0.8680(16) 0.125(7) Uani 0.5 1 d D . P E 2
H23H H 0.210457 -0.133694 0.858854 0.188 Uiso 0.5 1 calc R U P E 2
H23I H 0.221804 -0.043003 0.895073 0.188 Uiso 0.5 1 calc R U P E 2
H23J H 0.281567 -0.061862 0.804368 0.188 Uiso 0.5 1 calc R U P E 2
O3 O 0.3860(3) 0.5176(3) 0.7977(3) 0.0342(9) Uani 1 1 d . . . . .
C3 C 0.4110(5) 0.3116(5) 0.7825(4) 0.0341(13) Uani 1 1 d . . . . .
H3A H 0.382623 0.294444 0.846353 0.041 Uiso 1 1 calc R U . . .
H3B H 0.347669 0.386044 0.732697 0.041 Uiso 1 1 calc R U . . .
C31 C 0.4982(5) 0.4382(5) 0.7988(4) 0.0302(12) Uani 1 1 d . . . . .
C32 C 0.5164(5) 0.3328(5) 0.7919(4) 0.0315(13) Uani 1 1 d . . . . .
C33 C 0.6294(5) 0.2542(5) 0.7945(4) 0.0369(14) Uani 1 1 d . . . . .
H33 H 0.644174 0.182541 0.789831 0.044 Uiso 1 1 calc R U . . .
C34 C 0.7212(5) 0.2788(5) 0.8038(5) 0.0417(15) Uani 1 1 d . . . . .
C35 C 0.7027(6) 0.3843(5) 0.8070(4) 0.0403(14) Uani 1 1 d . . . . .
H35 H 0.766679 0.400934 0.811208 0.048 Uiso 1 1 calc R U . . .
C36 C 0.5900(5) 0.4655(5) 0.8040(4) 0.0337(13) Uani 1 1 d . . . . .
C37 C 0.3509(6) 0.4942(6) 0.8929(4) 0.0423(15) Uani 1 1 d . . . . .
H37A H 0.398208 0.506141 0.934938 0.051 Uiso 1 1 calc R U . . .
H37B H 0.363206 0.410829 0.925782 0.051 Uiso 1 1 calc R U . . .
C38 C 0.2240(7) 0.5782(8) 0.8784(6) 0.069(2) Uani 1 1 d . . . . .
H38A H 0.177689 0.562692 0.838744 0.082 Uiso 1 1 calc R U . . .
H38B H 0.212276 0.660875 0.840867 0.082 Uiso 1 1 calc R U . . .
C39 C 0.1794(7) 0.5668(9) 0.9735(6) 0.090(3) Uani 1 1 d D . . . .
H39A H 0.237879 0.560117 1.020257 0.108 Uiso 1 1 calc R U . F 1
H39B H 0.170968 0.492539 1.002410 0.108 Uiso 1 1 calc R U . F 1
C40 C 0.0633(14) 0.671(2) 0.962(3) 0.099(8) Uani 0.5 1 d D U P G 1
H40A H 0.038777 0.658130 1.026285 0.149 Uiso 0.5 1 calc R U P G 1
H40B H 0.071354 0.744320 0.934832 0.149 Uiso 0.5 1 calc R U P G 1
H40C H 0.004396 0.676696 0.916974 0.149 Uiso 0.5 1 calc R U P G 1
C40' C 0.0476(10) 0.623(2) 0.963(3) 0.099(8) Uani 0.5 1 d D . P G 2
H40D H 0.025435 0.611959 1.028281 0.149 Uiso 0.5 1 calc R U P G 2
H40E H 0.014732 0.708407 0.920029 0.149 Uiso 0.5 1 calc R U P G 2
H40F H 0.017139 0.585367 0.934759 0.149 Uiso 0.5 1 calc R U P G 2
Br1 Br 0.87826(8) 0.16319(8) 0.81697(8) 0.0821(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C11 1.379(7) . ?
O1 C17 1.452(7) . ?
C1 C12 1.521(7) . ?
C1 C36 1.524(7) 2_666 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C11 C12 1.398(8) . ?
C11 C16 1.407(7) . ?
C12 C13 1.373(8) . ?
C13 C14 1.398(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.394(8) . ?
C14 P1 1.807(6) . ?
C15 C16 1.396(8) . ?
C15 H15 0.9500 . ?
C16 C2 1.511(7) . ?
C17 C18 1.479(9) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19' 1.506(10) . ?
C18 C19 1.506(10) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.511(10) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C19' C20' 1.511(10) . ?
C19' H19C 0.9900 . ?
C19' H19D 0.9900 . ?
C20' H20G 0.9800 . ?
C20' H20H 0.9800 . ?
C20' H20I 0.9800 . ?
P1 O11 1.446(5) . ?
P1 O12 1.515(5) . ?
P1 O13 1.601(5) . ?
O12 C121 1.465(8) . ?
C121 C122 1.495(9) . ?
C121 C12' 1.496(10) . ?
C121 H12A 0.9900 . ?
C121 H12B 0.9900 . ?
C122 H12C 0.9800 . ?
C122 H12D 0.9800 . ?
C122 H12E 0.9800 . ?
C12' H12F 0.9800 . ?
C12' H12G 0.9800 . ?
C12' H12H 0.9800 . ?
O13 C131 1.444(8) . ?
C131 C132 1.489(10) . ?
C131 H13A 0.9900 . ?
C131 H13B 0.9900 . ?
C132 H13C 0.9800 . ?
C132 H13D 0.9800 . ?
C132 H13E 0.9800 . ?
O2 C21 1.384(6) . ?
O2 C27 1.433(6) . ?
C2 C22 1.514(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C21 C26 1.393(8) . ?
C21 C22 1.399(7) . ?
C22 C23 1.388(8) . ?
C23 C24 1.398(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.399(7) . ?
C24 P2 1.789(6) . ?
C25 C26 1.387(8) . ?
C25 H25 0.9500 . ?
C26 C3 1.514(7) . ?
C27 C28 1.513(8) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.505(10) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.497(10) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
P2 O21 1.444(5) . ?
P2 O22 1.578(5) . ?
P2 O23 1.594(5) . ?
O22 C221 1.430(9) . ?
C221 C222 1.419(13) . ?
C221 H22A 0.9900 . ?
C221 H22B 0.9900 . ?
C222 H22C 0.9800 . ?
C222 H22D 0.9800 . ?
C222 H22E 0.9800 . ?
O23 C231 1.464(12) . ?
O23 C23' 1.470(12) . ?
C231 C232 1.475(9) . ?
C231 H23A 0.9900 . ?
C231 H23B 0.9900 . ?
C232 H23C 0.9800 . ?
C232 H23D 0.9800 . ?
C232 H23E 0.9800 . ?
C23' C23" 1.513(10) . ?
C23' H23F 0.9900 . ?
C23' H23G 0.9900 . ?
C23" H23H 0.9800 . ?
C23" H23I 0.9800 . ?
C23" H23J 0.9800 . ?
O3 C31 1.381(7) . ?
O3 C37 1.440(7) . ?
C3 C32 1.521(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C31 C36 1.392(8) . ?
C31 C32 1.410(7) . ?
C32 C33 1.378(8) . ?
C33 C34 1.380(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.385(8) . ?
C34 Br1 1.913(6) . ?
C35 C36 1.386(8) . ?
C35 H35 0.9500 . ?
C37 C38 1.497(9) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.498(10) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.511(10) . ?
C39 C40' 1.511(10) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C40' H40D 0.9800 . ?
C40' H40E 0.9800 . ?
C40' H40F 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
C11 O1 C17 114.0(4) . . ?
C12 C1 C36 113.7(4) . 2_666 ?
C12 C1 H1A 108.8 . . ?
C36 C1 H1A 108.8 2_666 . ?
C12 C1 H1B 108.8 . . ?
C36 C1 H1B 108.8 2_666 . ?
H1A C1 H1B 107.7 . . ?
O1 C11 C12 118.2(5) . . ?
O1 C11 C16 119.9(5) . . ?
C12 C11 C16 121.9(5) . . ?
C13 C12 C11 118.5(5) . . ?
C13 C12 C1 121.0(5) . . ?
C11 C12 C1 120.5(5) . . ?
C12 C13 C14 121.2(5) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C15 C14 C13 119.6(5) . . ?
C15 C14 P1 121.3(4) . . ?
C13 C14 P1 119.1(4) . . ?
C14 C15 C16 120.7(5) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C15 C16 C11 117.8(5) . . ?
C15 C16 C2 121.2(5) . . ?
C11 C16 C2 121.0(5) . . ?
O1 C17 C18 108.0(5) . . ?
O1 C17 H17A 110.1 . . ?
C18 C17 H17A 110.1 . . ?
O1 C17 H17B 110.1 . . ?
C18 C17 H17B 110.1 . . ?
H17A C17 H17B 108.4 . . ?
C17 C18 C19' 118.9(15) . . ?
C17 C18 C19 111.3(15) . . ?
C17 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C18 C19 C20 117(2) . . ?
C18 C19 H19A 107.9 . . ?
C20 C19 H19A 107.9 . . ?
C18 C19 H19B 107.9 . . ?
C20 C19 H19B 107.9 . . ?
H19A C19 H19B 107.2 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C19' C20' 110(2) . . ?
C18 C19' H19C 109.7 . . ?
C20' C19' H19C 109.7 . . ?
C18 C19' H19D 109.7 . . ?
C20' C19' H19D 109.7 . . ?
H19C C19' H19D 108.2 . . ?
C19' C20' H20G 109.5 . . ?
C19' C20' H20H 109.5 . . ?
H20G C20' H20H 109.5 . . ?
C19' C20' H20I 109.5 . . ?
H20G C20' H20I 109.5 . . ?
H20H C20' H20I 109.5 . . ?
O11 P1 O12 119.1(3) . . ?
O11 P1 O13 114.2(3) . . ?
O12 P1 O13 102.1(3) . . ?
O11 P1 C14 112.9(3) . . ?
O12 P1 C14 105.9(3) . . ?
O13 P1 C14 100.6(2) . . ?
C121 O12 P1 119.5(4) . . ?
O12 C121 C122 110.5(13) . . ?
O12 C121 C12' 110.7(13) . . ?
O12 C121 H12A 109.5 . . ?
C122 C121 H12A 109.5 . . ?
O12 C121 H12B 109.5 . . ?
C122 C121 H12B 109.5 . . ?
H12A C121 H12B 108.1 . . ?
C121 C122 H12C 109.5 . . ?
C121 C122 H12D 109.5 . . ?
H12C C122 H12D 109.5 . . ?
C121 C122 H12E 109.5 . . ?
H12C C122 H12E 109.5 . . ?
H12D C122 H12E 109.5 . . ?
C121 C12' H12F 109.5 . . ?
C121 C12' H12G 109.5 . . ?
H12F C12' H12G 109.5 . . ?
C121 C12' H12H 109.5 . . ?
H12F C12' H12H 109.5 . . ?
H12G C12' H12H 109.5 . . ?
C131 O13 P1 118.8(4) . . ?
O13 C131 C132 109.2(6) . . ?
O13 C131 H13A 109.8 . . ?
C132 C131 H13A 109.8 . . ?
O13 C131 H13B 109.8 . . ?
C132 C131 H13B 109.8 . . ?
H13A C131 H13B 108.3 . . ?
C131 C132 H13C 109.5 . . ?
C131 C132 H13D 109.5 . . ?
H13C C132 H13D 109.5 . . ?
C131 C132 H13E 109.5 . . ?
H13C C132 H13E 109.5 . . ?
H13D C132 H13E 109.5 . . ?
C21 O2 C27 115.5(4) . . ?
C16 C2 C22 114.6(5) . . ?
C16 C2 H2A 108.6 . . ?
C22 C2 H2A 108.6 . . ?
C16 C2 H2B 108.6 . . ?
C22 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
O2 C21 C26 120.0(5) . . ?
O2 C21 C22 117.5(5) . . ?
C26 C21 C22 122.3(5) . . ?
C23 C22 C21 118.0(5) . . ?
C23 C22 C2 121.6(5) . . ?
C21 C22 C2 120.3(5) . . ?
C22 C23 C24 121.2(5) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C23 C24 C25 119.0(5) . . ?
C23 C24 P2 120.7(4) . . ?
C25 C24 P2 120.0(4) . . ?
C26 C25 C24 121.3(5) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C25 C26 C21 118.2(5) . . ?
C25 C26 C3 119.8(5) . . ?
C21 C26 C3 122.0(5) . . ?
O2 C27 C28 108.0(5) . . ?
O2 C27 H27A 110.1 . . ?
C28 C27 H27A 110.1 . . ?
O2 C27 H27B 110.1 . . ?
C28 C27 H27B 110.1 . . ?
H27A C27 H27B 108.4 . . ?
C29 C28 C27 115.3(5) . . ?
C29 C28 H28A 108.5 . . ?
C27 C28 H28A 108.5 . . ?
C29 C28 H28B 108.5 . . ?
C27 C28 H28B 108.5 . . ?
H28A C28 H28B 107.5 . . ?
C30 C29 C28 114.0(7) . . ?
C30 C29 H29A 108.7 . . ?
C28 C29 H29A 108.7 . . ?
C30 C29 H29B 108.7 . . ?
C28 C29 H29B 108.7 . . ?
H29A C29 H29B 107.6 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O21 P2 O22 116.7(3) . . ?
O21 P2 O23 115.7(3) . . ?
O22 P2 O23 96.5(3) . . ?
O21 P2 C24 113.6(3) . . ?
O22 P2 C24 105.8(3) . . ?
O23 P2 C24 106.6(3) . . ?
C221 O22 P2 118.8(4) . . ?
C222 C221 O22 111.5(8) . . ?
C222 C221 H22A 109.3 . . ?
O22 C221 H22A 109.3 . . ?
C222 C221 H22B 109.3 . . ?
O22 C221 H22B 109.3 . . ?
H22A C221 H22B 108.0 . . ?
C221 C222 H22C 109.5 . . ?
C221 C222 H22D 109.5 . . ?
H22C C222 H22D 109.5 . . ?
C221 C222 H22E 109.5 . . ?
H22C C222 H22E 109.5 . . ?
H22D C222 H22E 109.5 . . ?
C231 O23 P2 107.4(6) . . ?
C23' O23 P2 127.1(8) . . ?
O23 C231 C232 113.5(11) . . ?
O23 C231 H23A 108.9 . . ?
C232 C231 H23A 108.9 . . ?
O23 C231 H23B 108.9 . . ?
C232 C231 H23B 108.9 . . ?
H23A C231 H23B 107.7 . . ?
C231 C232 H23C 109.5 . . ?
C231 C232 H23D 109.5 . . ?
H23C C232 H23D 109.5 . . ?
C231 C232 H23E 109.5 . . ?
H23C C232 H23E 109.5 . . ?
H23D C232 H23E 109.5 . . ?
O23 C23' C23" 110.2(10) . . ?
O23 C23' H23F 109.6 . . ?
C23" C23' H23F 109.6 . . ?
O23 C23' H23G 109.6 . . ?
C23" C23' H23G 109.6 . . ?
H23F C23' H23G 108.1 . . ?
C23' C23" H23H 109.5 . . ?
C23' C23" H23I 109.5 . . ?
H23H C23" H23I 109.5 . . ?
C23' C23" H23J 109.5 . . ?
H23H C23" H23J 109.5 . . ?
H23I C23" H23J 109.5 . . ?
C31 O3 C37 114.6(4) . . ?
C26 C3 C32 115.3(5) . . ?
C26 C3 H3A 108.5 . . ?
C32 C3 H3A 108.5 . . ?
C26 C3 H3B 108.5 . . ?
C32 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
O3 C31 C36 119.4(5) . . ?
O3 C31 C32 119.0(5) . . ?
C36 C31 C32 121.6(5) . . ?
C33 C32 C31 117.9(5) . . ?
C33 C32 C3 123.6(5) . . ?
C31 C32 C3 118.5(5) . . ?
C32 C33 C34 120.5(5) . . ?
C32 C33 H33 119.7 . . ?
C34 C33 H33 119.7 . . ?
C33 C34 C35 121.5(6) . . ?
C33 C34 Br1 119.8(4) . . ?
C35 C34 Br1 118.7(5) . . ?
C34 C35 C36 119.3(6) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 H35 120.3 . . ?
C35 C36 C31 119.0(5) . . ?
C35 C36 C1 120.2(5) . 2_666 ?
C31 C36 C1 120.7(5) . 2_666 ?
O3 C37 C38 108.2(5) . . ?
O3 C37 H37A 110.0 . . ?
C38 C37 H37A 110.0 . . ?
O3 C37 H37B 110.0 . . ?
C38 C37 H37B 110.0 . . ?
H37A C37 H37B 108.4 . . ?
C37 C38 C39 113.0(6) . . ?
C37 C38 H38A 109.0 . . ?
C39 C38 H38A 109.0 . . ?
C37 C38 H38B 109.0 . . ?
C39 C38 H38B 109.0 . . ?
H38A C38 H38B 107.8 . . ?
C38 C39 C40 113.3(16) . . ?
C38 C39 C40' 114.4(16) . . ?
C38 C39 H39A 108.9 . . ?
C40 C39 H39A 108.9 . . ?
C38 C39 H39B 108.9 . . ?
C40 C39 H39B 108.9 . . ?
H39A C39 H39B 107.7 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C40' H40D 109.5 . . ?
C39 C40' H40E 109.5 . . ?
H40D C40' H40E 109.5 . . ?
C39 C40' H40F 109.5 . . ?
H40D C40' H40F 109.5 . . ?
H40E C40' H40F 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
C17 O1 C11 C12 103.3(5) . . . . ?
C17 O1 C11 C16 -79.4(6) . . . . ?
O1 C11 C12 C13 -179.9(4) . . . . ?
C16 C11 C12 C13 2.8(7) . . . . ?
O1 C11 C12 C1 -0.6(7) . . . . ?
C16 C11 C12 C1 -177.9(5) . . . . ?
C36 C1 C12 C13 -97.6(6) 2_666 . . . ?
C36 C1 C12 C11 83.1(6) 2_666 . . . ?
C11 C12 C13 C14 1.2(8) . . . . ?
C1 C12 C13 C14 -178.1(5) . . . . ?
C12 C13 C14 C15 -3.8(8) . . . . ?
C12 C13 C14 P1 175.7(4) . . . . ?
C13 C14 C15 C16 2.4(8) . . . . ?
P1 C14 C15 C16 -177.1(4) . . . . ?
C14 C15 C16 C11 1.4(7) . . . . ?
C14 C15 C16 C2 -179.7(5) . . . . ?
O1 C11 C16 C15 178.7(4) . . . . ?
C12 C11 C16 C15 -4.1(7) . . . . ?
O1 C11 C16 C2 -0.2(7) . . . . ?
C12 C11 C16 C2 177.1(5) . . . . ?
C11 O1 C17 C18 -173.4(5) . . . . ?
O1 C17 C18 C19' -55(4) . . . . ?
O1 C17 C18 C19 -68(3) . . . . ?
C17 C18 C19 C20 -179(4) . . . . ?
C17 C18 C19' C20' -180(3) . . . . ?
C15 C14 P1 O11 -146.7(4) . . . . ?
C13 C14 P1 O11 33.8(5) . . . . ?
C15 C14 P1 O12 -14.7(5) . . . . ?
C13 C14 P1 O12 165.7(4) . . . . ?
C15 C14 P1 O13 91.2(5) . . . . ?
C13 C14 P1 O13 -88.3(5) . . . . ?
O11 P1 O12 C121 43.8(6) . . . . ?
O13 P1 O12 C121 170.6(5) . . . . ?
C14 P1 O12 C121 -84.6(5) . . . . ?
P1 O12 C121 C122 158.0(12) . . . . ?
P1 O12 C121 C12' -165.8(10) . . . . ?
O11 P1 O13 C131 51.7(6) . . . . ?
O12 P1 O13 C131 -78.1(5) . . . . ?
C14 P1 O13 C131 172.9(5) . . . . ?
P1 O13 C131 C132 175.9(5) . . . . ?
C15 C16 C2 C22 45.3(7) . . . . ?
C11 C16 C2 C22 -135.9(5) . . . . ?
C27 O2 C21 C26 84.1(6) . . . . ?
C27 O2 C21 C22 -100.4(6) . . . . ?
O2 C21 C22 C23 -175.0(5) . . . . ?
C26 C21 C22 C23 0.5(8) . . . . ?
O2 C21 C22 C2 1.7(7) . . . . ?
C26 C21 C22 C2 177.1(5) . . . . ?
C16 C2 C22 C23 -100.5(6) . . . . ?
C16 C2 C22 C21 83.0(6) . . . . ?
C21 C22 C23 C24 0.7(8) . . . . ?
C2 C22 C23 C24 -175.9(5) . . . . ?
C22 C23 C24 C25 -0.6(9) . . . . ?
C22 C23 C24 P2 173.6(4) . . . . ?
C23 C24 C25 C26 -0.6(9) . . . . ?
P2 C24 C25 C26 -174.8(5) . . . . ?
C24 C25 C26 C21 1.6(9) . . . . ?
C24 C25 C26 C3 178.8(5) . . . . ?
O2 C21 C26 C25 173.7(5) . . . . ?
C22 C21 C26 C25 -1.6(8) . . . . ?
O2 C21 C26 C3 -3.4(8) . . . . ?
C22 C21 C26 C3 -178.7(5) . . . . ?
C21 O2 C27 C28 170.6(4) . . . . ?
O2 C27 C28 C29 60.9(7) . . . . ?
C27 C28 C29 C30 64.7(8) . . . . ?
C23 C24 P2 O21 28.3(6) . . . . ?
C25 C24 P2 O21 -157.6(5) . . . . ?
C23 C24 P2 O22 157.6(5) . . . . ?
C25 C24 P2 O22 -28.3(6) . . . . ?
C23 C24 P2 O23 -100.4(5) . . . . ?
C25 C24 P2 O23 73.7(5) . . . . ?
O21 P2 O22 C221 50.2(6) . . . . ?
O23 P2 O22 C221 173.4(5) . . . . ?
C24 P2 O22 C221 -77.3(6) . . . . ?
P2 O22 C221 C222 165.9(9) . . . . ?
O21 P2 O23 C231 -55.8(9) . . . . ?
O22 P2 O23 C231 -179.7(9) . . . . ?
C24 P2 O23 C231 71.7(9) . . . . ?
O21 P2 O23 C23' -29.0(9) . . . . ?
O22 P2 O23 C23' -152.8(9) . . . . ?
C24 P2 O23 C23' 98.5(9) . . . . ?
P2 O23 C231 C232 177.2(17) . . . . ?
P2 O23 C23' C23" -95.8(16) . . . . ?
C25 C26 C3 C32 81.6(7) . . . . ?
C21 C26 C3 C32 -101.3(6) . . . . ?
C37 O3 C31 C36 -94.2(6) . . . . ?
C37 O3 C31 C32 87.5(6) . . . . ?
O3 C31 C32 C33 -179.2(5) . . . . ?
C36 C31 C32 C33 2.6(8) . . . . ?
O3 C31 C32 C3 0.5(7) . . . . ?
C36 C31 C32 C3 -177.7(5) . . . . ?
C26 C3 C32 C33 -12.8(8) . . . . ?
C26 C3 C32 C31 167.5(5) . . . . ?
C31 C32 C33 C34 0.1(8) . . . . ?
C3 C32 C33 C34 -179.5(5) . . . . ?
C32 C33 C34 C35 -2.5(9) . . . . ?
C32 C33 C34 Br1 175.4(4) . . . . ?
C33 C34 C35 C36 2.1(9) . . . . ?
Br1 C34 C35 C36 -175.8(4) . . . . ?
C34 C35 C36 C31 0.6(8) . . . . ?
C34 C35 C36 C1 -179.3(5) . . . 2_666 ?
O3 C31 C36 C35 178.8(5) . . . . ?
C32 C31 C36 C35 -3.0(8) . . . . ?
O3 C31 C36 C1 -1.3(7) . . . 2_666 ?
C32 C31 C36 C1 176.9(5) . . . 2_666 ?
C31 O3 C37 C38 -173.6(5) . . . . ?
O3 C37 C38 C39 -176.6(7) . . . . ?
C37 C38 C39 C40 164.7(14) . . . . ?
C37 C38 C39 C40' -163.7(14) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C17 H17B O21 0.99 2.41 3.370(8) 162.4 2_656 yes
C121 H12B^a O11 0.99 2.29 3.217(9) 155.2 2_756 yes
C28 H28B O1 0.99 2.63 3.540(7) 153.1 . yes

_refine_diff_density_max         1.348
_refine_diff_density_min         -1.457
_refine_diff_density_rms         0.102

####################################################################### 
# 
# 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_tc031
_database_code_depnum_ccdc_archive 'CCDC 2441442'
loop_
_audit_author_name
_audit_author_address
'Alexandre Sobolev'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2025-04-07 deposited with the CCDC.	2025-10-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H78 O6 Br6, 3(C8 H10)'
_chemical_formula_sum            "C90 H108 Br6 O6'"
_chemical_formula_weight         1765.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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                   27.851(4)
_cell_length_b                   16.790(2)
_cell_length_c                   19.995(3)
_cell_angle_alpha                90
_cell_angle_beta                 113.569(2)
_cell_angle_gamma                90
_cell_volume                     8570(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    5763
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      27.86

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_F_000             3624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    2.861
_shelx_estimated_absorpt_T_min   0.279
_shelx_estimated_absorpt_T_max   0.763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2786
_exptl_absorpt_correction_T_max  0.7629
_exptl_absorpt_process_details   
'SADABS - Bruker area detector absorption corrections'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37060
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.452
_diffrn_reflns_theta_max         28.060
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             10227
_reflns_number_gt                7122
_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 SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL, v. 5.1'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'X-Seed v. 4.0 (Barbour, 2020)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0830P)²+25.0000P] 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         10227
_refine_ls_number_parameters     511
_refine_ls_number_restraints     139
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0598
_refine_ls_wR_factor_ref         0.1674
_refine_ls_wR_factor_gt          0.1546
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.010
_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 0.24459(2) 0.24521(3) 0.08359(2) 0.04022(14) Uani 1 1 d . . . . .
O1 O 0.33318(11) 0.28037(17) 0.41125(14) 0.0270(6) Uani 1 1 d . . . . .
C11 C 0.31202(15) 0.2718(2) 0.3361(2) 0.0232(8) Uani 1 1 d . . . . .
C12 C 0.30498(15) 0.3403(2) 0.2929(2) 0.0247(8) Uani 1 1 d . . . . .
C13 C 0.28499(16) 0.3318(2) 0.2170(2) 0.0281(8) Uani 1 1 d . . . . .
H13 H 0.280299 0.377115 0.186564 0.034 Uiso 1 1 calc R U . . .
C14 C 0.27213(18) 0.2563(2) 0.1870(2) 0.0293(9) Uani 1 1 d . . . . .
C15 C 0.28006(16) 0.1884(2) 0.2297(2) 0.0283(8) Uani 1 1 d . . . . .
H15 H 0.271698 0.137307 0.207545 0.034 Uiso 1 1 calc R U . . .
C16 C 0.30046(15) 0.1960(2) 0.3056(2) 0.0266(8) Uani 1 1 d . . . . .
C10 C 0.29335(17) 0.2860(3) 0.4413(2) 0.0289(8) Uani 1 1 d . . . . .
H10A H 0.269421 0.239736 0.425476 0.035 Uiso 1 1 calc R U . . .
H10B H 0.272423 0.335154 0.423569 0.035 Uiso 1 1 calc R U . . .
C17 C 0.32035(19) 0.2876(3) 0.5232(2) 0.0334(9) Uani 1 1 d . . . . .
H17A H 0.295736 0.309010 0.543326 0.040 Uiso 1 1 calc R U . . .
H17B H 0.350582 0.324437 0.537525 0.040 Uiso 1 1 calc R U . . .
C18 C 0.3398(2) 0.2059(3) 0.5574(2) 0.0413(11) Uani 1 1 d . . . . .
H18A H 0.310273 0.167671 0.539919 0.050 Uiso 1 1 calc R U . . .
H18B H 0.366983 0.186578 0.541226 0.050 Uiso 1 1 calc R U . . .
C19 C 0.3624(2) 0.2090(4) 0.6405(3) 0.0600(15) Uani 1 1 d . . . . .
H19A H 0.374372 0.155781 0.660202 0.090 Uiso 1 1 calc R U . . .
H19B H 0.392066 0.246089 0.658012 0.090 Uiso 1 1 calc R U . . .
H19C H 0.335378 0.227189 0.656706 0.090 Uiso 1 1 calc R U . . .
C1 C 0.31935(15) 0.4220(2) 0.3276(2) 0.0249(8) Uani 1 1 d . . . . .
H1A H 0.327837 0.457425 0.294197 0.030 Uiso 1 1 calc R U . . .
H1B H 0.351102 0.417377 0.373402 0.030 Uiso 1 1 calc R U . . .
Br2 Br 0.11407(2) 0.48629(4) 0.23865(3) 0.05027(17) Uani 1 1 d . . . . .
O2 O 0.33571(10) 0.49409(15) 0.46694(13) 0.0239(5) Uani 1 1 d . . . . .
C21 C 0.28587(15) 0.4941(2) 0.41244(19) 0.0215(7) Uani 1 1 d . . . . .
C22 C 0.24506(15) 0.5240(2) 0.43042(19) 0.0243(8) Uani 1 1 d . . . . .
C23 C 0.19393(16) 0.5205(2) 0.3783(2) 0.0279(8) Uani 1 1 d . . . . .
H23 H 0.165904 0.540420 0.389048 0.033 Uiso 1 1 calc R U . . .
C24 C 0.18403(15) 0.4876(3) 0.3100(2) 0.0286(9) Uani 1 1 d . . . . .
C25 C 0.22381(16) 0.4575(2) 0.29288(19) 0.0268(8) Uani 1 1 d . . . . .
H25 H 0.215938 0.435117 0.246018 0.032 Uiso 1 1 calc R U . . .
C26 C 0.27569(15) 0.4597(2) 0.34428(19) 0.0221(7) Uani 1 1 d . . . . .
C20 C 0.37161(16) 0.5523(2) 0.4591(2) 0.0291(8) Uani 1 1 d . . . . .
H20A H 0.358149 0.606965 0.458720 0.035 Uiso 1 1 calc R U . . .
H20B H 0.376076 0.543556 0.412917 0.035 Uiso 1 1 calc R U . . .
C27 C 0.42350(16) 0.5409(3) 0.5243(2) 0.0340(9) Uani 1 1 d . . . . .
H27A H 0.418226 0.551995 0.569511 0.041 Uiso 1 1 calc R U . . .
H27B H 0.449019 0.580266 0.521229 0.041 Uiso 1 1 calc R U . . .
C28 C 0.44672(18) 0.4574(3) 0.5296(3) 0.0408(11) Uani 1 1 d . . . . .
H28A H 0.419675 0.417673 0.526571 0.049 Uiso 1 1 calc R U . . .
H28B H 0.456139 0.448824 0.487357 0.049 Uiso 1 1 calc R U . . .
C29 C 0.4952(2) 0.4434(4) 0.5998(3) 0.0611(15) Uani 1 1 d . . . . .
H29A H 0.508062 0.389070 0.599785 0.092 Uiso 1 1 calc R U . . .
H29B H 0.522507 0.481614 0.602642 0.092 Uiso 1 1 calc R U . . .
H29C H 0.486011 0.450435 0.641892 0.092 Uiso 1 1 calc R U . . .
C2 C 0.25692(16) 0.5617(2) 0.50454(19) 0.0256(8) Uani 1 1 d . . . . .
H2C H 0.287941 0.596620 0.516814 0.031 Uiso 1 1 calc R U . . .
H2D H 0.226965 0.595973 0.500568 0.031 Uiso 1 1 calc R U . . .
Br3 Br 0.39668(2) 0.41798(3) 0.74139(3) 0.04511(15) Uani 1 1 d . . . . .
O3 O 0.17489(10) 0.48213(16) 0.52959(14) 0.0254(6) Uani 1 1 d . . . . .
C31 C 0.22576(15) 0.4680(2) 0.57874(19) 0.0235(8) Uani 1 1 d . . . . .
C32 C 0.23448(15) 0.4152(2) 0.63704(19) 0.0226(7) Uani 1 1 d . . . . .
C33 C 0.28617(16) 0.3999(2) 0.68476(19) 0.0263(8) Uani 1 1 d . . . . .
H33 H 0.293279 0.364582 0.724735 0.032 Uiso 1 1 calc R U . . .
C34 C 0.32707(15) 0.4362(2) 0.6737(2) 0.0255(8) Uani 1 1 d . . . . .
C35 C 0.31836(16) 0.4875(2) 0.6156(2) 0.0268(8) Uani 1 1 d . . . . .
H35 H 0.347115 0.511358 0.609034 0.032 Uiso 1 1 calc R U . . .
C36 C 0.26726(15) 0.5038(2) 0.56682(19) 0.0225(7) Uani 1 1 d . . . . .
C30 C 0.14677(17) 0.5409(3) 0.5530(2) 0.0325(9) Uani 1 1 d . . . . .
H30A H 0.156451 0.595098 0.543443 0.039 Uiso 1 1 calc R U . . .
H30B H 0.156260 0.535597 0.606124 0.039 Uiso 1 1 calc R U . . .
C37 C 0.08848(19) 0.5283(3) 0.5119(3) 0.0469(12) Uani 1 1 d . . . . .
H37A H 0.079179 0.474781 0.523714 0.056 Uiso 1 1 calc R U . . .
H37B H 0.069545 0.568040 0.528834 0.056 Uiso 1 1 calc R U . . .
C38 C 0.0703(2) 0.5354(4) 0.4303(3) 0.0632(16) Uani 1 1 d . . . . .
H38A H 0.088278 0.494386 0.413073 0.076 Uiso 1 1 calc R U . . .
H38B H 0.080697 0.588232 0.418527 0.076 Uiso 1 1 calc R U . . .
C39 C 0.0111(2) 0.5255(5) 0.3893(4) 0.082(2) Uani 1 1 d . . . . .
H39A H 0.001756 0.530678 0.336772 0.123 Uiso 1 1 calc R U . . .
H39B H 0.000660 0.472806 0.399741 0.123 Uiso 1 1 calc R U . . .
H39C H -0.006926 0.566715 0.405198 0.123 Uiso 1 1 calc R U . . .
C3 C 0.18801(15) 0.3779(2) 0.6466(2) 0.0273(8) Uani 1 1 d . . . . .
H3A H 0.161387 0.363955 0.597757 0.033 Uiso 1 1 calc R U . . .
H3C H 0.172319 0.418582 0.667634 0.033 Uiso 1 1 calc R U . . .
C1A C 0.4997(3) 0.2490(7) 0.4929(4) 0.042(4) Uani 0.5 1 d DG U P A 1
C2A C 0.5543(3) 0.2499(5) 0.5333(4) 0.037(2) Uani 0.5 1 d G U P A 1
H2A H 0.577068 0.262233 0.509946 0.044 Uiso 0.5 1 calc R U P A 1
C3A C 0.5750(3) 0.2326(5) 0.6084(4) 0.033(2) Uani 0.5 1 d DG U P A 1
C4A C 0.5413(3) 0.2143(6) 0.6431(4) 0.044(3) Uani 0.5 1 d G U P A 1
H4A H 0.555294 0.202610 0.693793 0.053 Uiso 0.5 1 calc R U P A 1
C5A C 0.4867(3) 0.2134(6) 0.6026(4) 0.058(3) Uani 0.5 1 d G U P A 1
H5A H 0.463913 0.201096 0.626022 0.070 Uiso 0.5 1 calc R U P A 1
C6A C 0.4660(3) 0.2307(7) 0.5275(4) 0.060(3) Uani 0.5 1 d G U P A 1
H6A H 0.429123 0.230100 0.500211 0.072 Uiso 0.5 1 calc R U P A 1
C11A C 0.4753(8) 0.2694(12) 0.4137(6) 0.065(5) Uani 0.5 1 d D U P A 1
H11A H 0.437152 0.265072 0.396077 0.097 Uiso 0.5 1 calc R U P A 1
H11B H 0.484831 0.323949 0.406623 0.097 Uiso 0.5 1 calc R U P A 1
H11C H 0.487990 0.232416 0.386426 0.097 Uiso 0.5 1 calc R U P A 1
C13A C 0.6330(3) 0.2350(6) 0.6518(5) 0.042(2) Uani 0.5 1 d D U P A 1
H13A H 0.650652 0.248519 0.619611 0.063 Uiso 0.5 1 calc R U P A 1
H13B H 0.641269 0.275353 0.690245 0.063 Uiso 0.5 1 calc R U P A 1
H13C H 0.645103 0.182762 0.674025 0.063 Uiso 0.5 1 calc R U P A 1
C1' C 0.5034(5) 0.2367(10) 0.4908(6) 0.073(7) Uani 0.5 1 d DG U P B 2
C2' C 0.4875(5) 0.2222(9) 0.5466(7) 0.081(5) Uani 0.5 1 d G U P B 2
H2' H 0.451210 0.217394 0.536448 0.097 Uiso 0.5 1 calc R U P B 2
C3' C 0.5241(5) 0.2146(9) 0.6173(6) 0.088(6) Uani 0.5 1 d DG U P B 2
C4' C 0.5767(5) 0.2215(8) 0.6321(6) 0.081(6) Uani 0.5 1 d G U P B 2
H4' H 0.601941 0.216284 0.680764 0.097 Uiso 0.5 1 calc R U P B 2
C5' C 0.5926(5) 0.2360(6) 0.5762(8) 0.080(4) Uani 0.5 1 d G U P B 2
H5' H 0.628883 0.240762 0.586423 0.096 Uiso 0.5 1 calc R U P B 2
C6' C 0.5560(5) 0.2436(9) 0.5056(7) 0.096(6) Uani 0.5 1 d G U P B 2
H6' H 0.566979 0.253574 0.467103 0.115 Uiso 0.5 1 calc R U P B 2
C11' C 0.4623(9) 0.2460(15) 0.4155(9) 0.104(9) Uani 0.5 1 d D U P B 2
H11D H 0.427621 0.238996 0.416439 0.155 Uiso 0.5 1 calc R U P B 2
H11E H 0.464735 0.299379 0.397238 0.155 Uiso 0.5 1 calc R U P B 2
H11F H 0.467470 0.205919 0.383442 0.155 Uiso 0.5 1 calc R U P B 2
C13' C 0.5114(8) 0.1962(16) 0.6810(9) 0.137(8) Uani 0.5 1 d D U P B 2
H13D H 0.473272 0.192473 0.665107 0.206 Uiso 0.5 1 calc R U P B 2
H13E H 0.527477 0.145379 0.702573 0.206 Uiso 0.5 1 calc R U P B 2
H13F H 0.524924 0.238613 0.717458 0.206 Uiso 0.5 1 calc R U P B 2
C1B C -0.0474(2) 0.7643(4) 0.2242(3) 0.0726(19) Uani 1 1 d D U . . .
C2B C -0.0471(3) 0.8471(4) 0.2252(4) 0.108(3) Uani 1 1 d D U . . .
H2B H -0.079155 0.875737 0.208941 0.129 Uiso 1 1 calc R U . . .
C3B C 0.000000 0.8878(8) 0.250000 0.116(4) Uani 1 2 d DS TU P . .
H3B H 0.000001 0.944333 0.250000 0.139 Uiso 1 2 calc R U P . .
C4B C 0.000000 0.7251(5) 0.250000 0.064(2) Uani 1 2 d DS TU P . .
H4B H 0.000000 0.668525 0.249999 0.076 Uiso 1 2 calc R U P . .
C11B C -0.0981(4) 0.7219(8) 0.1995(7) 0.152(4) Uani 1 1 d D U . . .
H11G H -0.126752 0.760720 0.183376 0.228 Uiso 1 1 calc R U . . .
H11H H -0.101544 0.686575 0.158766 0.228 Uiso 1 1 calc R U . . .
H11I H -0.099553 0.690311 0.239810 0.228 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 C14 1.904(4) . ?
O1 C11 1.385(4) . ?
O1 C10 1.461(5) . ?
C11 C16 1.393(5) . ?
C11 C12 1.403(5) . ?
C12 C13 1.399(5) . ?
C12 C1 1.517(5) . ?
C13 C14 1.388(5) . ?
C14 C15 1.389(5) . ?
C15 C16 1.397(5) . ?
C16 C3 1.520(5) 7_556 ?
C10 C17 1.505(5) . ?
C17 C18 1.531(7) . ?
C18 C19 1.525(6) . ?
C1 C26 1.521(5) . ?
Br2 C24 1.900(4) . ?
O2 C21 1.380(4) . ?
O2 C20 1.451(5) . ?
C21 C26 1.402(5) . ?
C21 C22 1.414(5) . ?
C22 C23 1.390(5) . ?
C22 C2 1.521(5) . ?
C23 C24 1.393(5) . ?
C24 C25 1.381(6) . ?
C25 C26 1.399(5) . ?
C20 C27 1.523(6) . ?
C27 C28 1.530(6) . ?
C28 C29 1.526(7) . ?
C2 C36 1.514(5) . ?
Br3 C34 1.894(4) . ?
O3 C31 1.384(5) . ?
O3 C30 1.449(5) . ?
C31 C36 1.406(5) . ?
C31 C32 1.406(5) . ?
C32 C33 1.397(5) . ?
C32 C3 1.517(5) . ?
C33 C34 1.386(5) . ?
C34 C35 1.387(5) . ?
C35 C36 1.393(6) . ?
C30 C37 1.513(6) . ?
C37 C38 1.508(7) . ?
C38 C39 1.528(7) . ?
C1A C2A 1.407(5) . ?
C1A C6A 1.407(5) . ?
C1A C11A 1.491(9) . ?
C2A C3A 1.407(5) . ?
C3A C4A 1.407(5) . ?
C3A C13A 1.497(8) . ?
C4A C5A 1.407(5) . ?
C5A C6A 1.407(5) . ?
C1' C6' 1.378(7) . ?
C1' C2' 1.378(7) . ?
C1' C11' 1.491(9) . ?
C2' C3' 1.378(7) . ?
C3' C4' 1.378(7) . ?
C3' C13' 1.486(10) . ?
C4' C5' 1.378(7) . ?
C5' C6' 1.378(7) . ?
C1B C4B 1.378(4) . ?
C1B C2B 1.391(5) . ?
C1B C11B 1.477(8) . ?
C2B C3B 1.382(5) . ?

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 112.9(3) . . ?
O1 C11 C16 119.6(3) . . ?
O1 C11 C12 118.4(3) . . ?
C16 C11 C12 121.9(3) . . ?
C13 C12 C11 118.7(3) . . ?
C13 C12 C1 120.3(3) . . ?
C11 C12 C1 120.9(3) . . ?
C14 C13 C12 119.0(4) . . ?
C13 C14 C15 122.3(4) . . ?
C13 C14 Br1 118.8(3) . . ?
C15 C14 Br1 118.9(3) . . ?
C14 C15 C16 119.3(4) . . ?
C11 C16 C15 118.8(4) . . ?
C11 C16 C3 121.1(3) . 7_556 ?
C15 C16 C3 120.0(4) . 7_556 ?
O1 C10 C17 108.5(3) . . ?
C10 C17 C18 113.8(4) . . ?
C19 C18 C17 112.0(4) . . ?
C12 C1 C26 112.8(3) . . ?
C21 O2 C20 115.7(3) . . ?
O2 C21 C26 121.1(3) . . ?
O2 C21 C22 117.2(3) . . ?
C26 C21 C22 121.5(3) . . ?
C23 C22 C21 118.7(3) . . ?
C23 C22 C2 120.5(3) . . ?
C21 C22 C2 120.8(3) . . ?
C22 C23 C24 119.6(4) . . ?
C25 C24 C23 121.6(4) . . ?
C25 C24 Br2 119.5(3) . . ?
C23 C24 Br2 118.8(3) . . ?
C24 C25 C26 120.2(3) . . ?
C25 C26 C21 118.2(3) . . ?
C25 C26 C1 120.6(3) . . ?
C21 C26 C1 121.1(3) . . ?
O2 C20 C27 106.3(3) . . ?
C20 C27 C28 113.9(4) . . ?
C29 C28 C27 113.5(4) . . ?
C36 C2 C22 115.4(3) . . ?
C31 O3 C30 114.8(3) . . ?
O3 C31 C36 118.9(3) . . ?
O3 C31 C32 119.0(3) . . ?
C36 C31 C32 122.0(4) . . ?
C33 C32 C31 118.1(3) . . ?
C33 C32 C3 122.4(3) . . ?
C31 C32 C3 119.4(3) . . ?
C34 C33 C32 119.9(3) . . ?
C33 C34 C35 121.8(4) . . ?
C33 C34 Br3 119.1(3) . . ?
C35 C34 Br3 119.0(3) . . ?
C34 C35 C36 119.7(4) . . ?
C35 C36 C31 118.4(3) . . ?
C35 C36 C2 120.5(3) . . ?
C31 C36 C2 121.0(3) . . ?
O3 C30 C37 109.3(4) . . ?
C38 C37 C30 113.6(4) . . ?
C37 C38 C39 113.2(5) . . ?
C32 C3 C16 116.1(3) . 7_556 ?
C2A C1A C6A 120.0 . . ?
C2A C1A C11A 122.4(10) . . ?
C6A C1A C11A 117.5(10) . . ?
C1A C2A C3A 120.0 . . ?
C4A C3A C2A 120.0 . . ?
C4A C3A C13A 119.9(6) . . ?
C2A C3A C13A 120.0(6) . . ?
C3A C4A C5A 120.0 . . ?
C6A C5A C4A 120.0 . . ?
C5A C6A C1A 120.0 . . ?
C6' C1' C2' 120.0 . . ?
C6' C1' C11' 122.0(14) . . ?
C2' C1' C11' 118.0(14) . . ?
C3' C2' C1' 120.0 . . ?
C4' C3' C2' 120.0 . . ?
C4' C3' C13' 115.5(12) . . ?
C2' C3' C13' 124.4(13) . . ?
C3' C4' C5' 120.0 . . ?
C6' C5' C4' 120.0 . . ?
C1' C6' C5' 120.0 . . ?
C4B C1B C2B 118.1(7) . . ?
C4B C1B C11B 122.7(8) . . ?
C2B C1B C11B 119.1(7) . . ?
C3B C2B C1B 119.9(10) . . ?
C2B C3B C2B 120.8(12) 2 . ?
C1B C4B C1B 123.0(8) . 2 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 O1 C11 C16 -87.6(4) . . . . ?
C10 O1 C11 C12 95.0(4) . . . . ?
O1 C11 C12 C13 178.2(3) . . . . ?
C16 C11 C12 C13 1.0(6) . . . . ?
O1 C11 C12 C1 -0.9(5) . . . . ?
C16 C11 C12 C1 -178.2(3) . . . . ?
C11 C12 C13 C14 0.9(6) . . . . ?
C1 C12 C13 C14 -179.9(4) . . . . ?
C12 C13 C14 C15 -2.2(6) . . . . ?
C12 C13 C14 Br1 179.7(3) . . . . ?
C13 C14 C15 C16 1.6(6) . . . . ?
Br1 C14 C15 C16 179.7(3) . . . . ?
O1 C11 C16 C15 -178.8(3) . . . . ?
C12 C11 C16 C15 -1.6(6) . . . . ?
O1 C11 C16 C3 -1.6(5) . . . 7_556 ?
C12 C11 C16 C3 175.6(3) . . . 7_556 ?
C14 C15 C16 C11 0.3(6) . . . . ?
C14 C15 C16 C3 -176.9(4) . . . 7_556 ?
C11 O1 C10 C17 174.9(3) . . . . ?
O1 C10 C17 C18 -77.1(4) . . . . ?
C10 C17 C18 C19 -174.9(4) . . . . ?
C13 C12 C1 C26 95.7(4) . . . . ?
C11 C12 C1 C26 -85.2(4) . . . . ?
C20 O2 C21 C26 77.2(4) . . . . ?
C20 O2 C21 C22 -108.1(4) . . . . ?
O2 C21 C22 C23 -176.1(3) . . . . ?
C26 C21 C22 C23 -1.5(5) . . . . ?
O2 C21 C22 C2 5.8(5) . . . . ?
C26 C21 C22 C2 -179.6(3) . . . . ?
C21 C22 C23 C24 0.3(6) . . . . ?
C2 C22 C23 C24 178.3(4) . . . . ?
C22 C23 C24 C25 0.7(6) . . . . ?
C22 C23 C24 Br2 -178.2(3) . . . . ?
C23 C24 C25 C26 -0.3(6) . . . . ?
Br2 C24 C25 C26 178.5(3) . . . . ?
C24 C25 C26 C21 -0.9(6) . . . . ?
C24 C25 C26 C1 176.2(4) . . . . ?
O2 C21 C26 C25 176.3(3) . . . . ?
C22 C21 C26 C25 1.9(5) . . . . ?
O2 C21 C26 C1 -0.9(5) . . . . ?
C22 C21 C26 C1 -175.3(3) . . . . ?
C12 C1 C26 C25 -44.8(5) . . . . ?
C12 C1 C26 C21 132.3(4) . . . . ?
C21 O2 C20 C27 -179.6(3) . . . . ?
O2 C20 C27 C28 59.3(5) . . . . ?
C20 C27 C28 C29 -173.1(4) . . . . ?
C23 C22 C2 C36 102.9(4) . . . . ?
C21 C22 C2 C36 -79.1(5) . . . . ?
C30 O3 C31 C36 -100.7(4) . . . . ?
C30 O3 C31 C32 82.3(4) . . . . ?
O3 C31 C32 C33 178.1(3) . . . . ?
C36 C31 C32 C33 1.3(5) . . . . ?
O3 C31 C32 C3 -2.7(5) . . . . ?
C36 C31 C32 C3 -179.5(3) . . . . ?
C31 C32 C33 C34 -0.2(5) . . . . ?
C3 C32 C33 C34 -179.4(4) . . . . ?
C32 C33 C34 C35 -0.7(6) . . . . ?
C32 C33 C34 Br3 177.4(3) . . . . ?
C33 C34 C35 C36 0.4(6) . . . . ?
Br3 C34 C35 C36 -177.6(3) . . . . ?
C34 C35 C36 C31 0.6(5) . . . . ?
C34 C35 C36 C2 177.9(3) . . . . ?
O3 C31 C36 C35 -178.4(3) . . . . ?
C32 C31 C36 C35 -1.5(5) . . . . ?
O3 C31 C36 C2 4.3(5) . . . . ?
C32 C31 C36 C2 -178.8(3) . . . . ?
C22 C2 C36 C35 100.7(4) . . . . ?
C22 C2 C36 C31 -82.0(4) . . . . ?
C31 O3 C30 C37 -158.0(3) . . . . ?
O3 C30 C37 C38 -59.6(6) . . . . ?
C30 C37 C38 C39 -178.0(5) . . . . ?
C33 C32 C3 C16 -19.1(5) . . . 7_556 ?
C31 C32 C3 C16 161.7(3) . . . 7_556 ?
C6A C1A C2A C3A 0.0 . . . . ?
C11A C1A C2A C3A 178.0(14) . . . . ?
C1A C2A C3A C4A 0.0 . . . . ?
C1A C2A C3A C13A -178.9(8) . . . . ?
C2A C3A C4A C5A 0.0 . . . . ?
C13A C3A C4A C5A 178.9(8) . . . . ?
C3A C4A C5A C6A 0.0 . . . . ?
C4A C5A C6A C1A 0.0 . . . . ?
C2A C1A C6A C5A 0.0 . . . . ?
C11A C1A C6A C5A -178.1(13) . . . . ?
C6' C1' C2' C3' 0.0 . . . . ?
C11' C1' C2' C3' -178.8(17) . . . . ?
C1' C2' C3' C4' 0.0 . . . . ?
C1' C2' C3' C13' -177.8(18) . . . . ?
C2' C3' C4' C5' 0.0 . . . . ?
C13' C3' C4' C5' 178.0(16) . . . . ?
C3' C4' C5' C6' 0.0 . . . . ?
C2' C1' C6' C5' 0.0 . . . . ?
C11' C1' C6' C5' 178.7(18) . . . . ?
C4' C5' C6' C1' 0.0 . . . . ?
C4B C1B C2B C3B 1.6(10) . . . . ?
C11B C1B C2B C3B 178.3(7) . . . . ?
C1B C2B C3B C2B -0.8(5) . . . 2 ?
C2B C1B C4B C1B -0.8(5) . . . 2 ?
C11B C1B C4B C1B -177.4(8) . . . 2 ?

_refine_diff_density_max         2.697
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.133

####################################################################### 
# 
# 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_120418C
_database_code_depnum_ccdc_archive 'CCDC 2478151'
loop_
_audit_author_name
_audit_author_address
'Alexandre Sobolev'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2025-08-04 deposited with the CCDC.	2025-10-28 downloaded from the CCDC.
;

# Start Validation Reply Form

_vrf_PLAT082_120418C             
;
PROBLEM: High R1 Value ..................................       0.21 Report
          
RESPONSE: The R1 value reflects the challenges in modeling extensive disorder
present in this structure. SQUEEZE treatment was applied to handle diffuse
solvent electron density, and appropriate restraints were used to maintain
chemical reasonableness while achieving convergence.
;

_vrf_PLAT084_120418C             
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.42 Report
          
RESPONSE: The high wR2 value is attributed to poor crystal quality, extensive
disorder in solvent regions, and numerous unlocalized hydrogen atoms. Despite
these challenges, the connectivity and main structural features are clearly
defined. SQUEEZE was applied to remove disordered solvent contributions,
and restraints were used to stabilize the refinement.
;

_vrf_PLAT230_120418C             
;
PROBLEM: Hirshfeld Test Diff for    P1       --C14      .        8.0 s.u.  
          
RESPONSE: The large Hirshfeld difference for P1--C14 likely reflects local
disorder that could not be fully modeled. The overall molecular geometry
remains chemically reasonable
;

_vrf_PLAT420_120418C             
;
PROBLEM: D-H Bond Without Acceptor  O1       --H1       .     Please Check 
          
RESPONSE: The O1--H1 bond lacks a clear acceptor due to disorder in the
solvent region. SQUEEZE was used to remove diffuse electron density, which
likely contained the disordered hydrogen bonding partners.
;

_vrf_PLAT936_120418C             
;
PROBLEM: The Embedded .res File Includes a DAMP Command . 2000.0 Report
          
RESPONSE: Heavy damping was employed as a standard technique to ensure
convergence stability when refining structures with significant disorder
and multiple constrained parameters. 
;

# End Validation Reply Form

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C35 H35 O20 P5), C H4 O, 4(H2 O)'
_chemical_formula_sum            'C71 H82 O45 P10'
_chemical_formula_weight         1965.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

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

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

_cell_length_a                   11.1506(3)
_cell_length_b                   18.4587(5)
_cell_length_c                   12.7509(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.227(3)
_cell_angle_gamma                90
_cell_volume                     2590.50(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9983
_cell_measurement_theta_min      3.469
_cell_measurement_theta_max      66.886
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0406915
_diffrn_orient_matrix_UB_12      -0.0105463
_diffrn_orient_matrix_UB_13      0.1203087
_diffrn_orient_matrix_UB_21      0.1299755
_diffrn_orient_matrix_UB_22      0.0229544
_diffrn_orient_matrix_UB_23      -0.0116989
_diffrn_orient_matrix_UB_31      -0.0321455
_diffrn_orient_matrix_UB_32      0.0795614
_diffrn_orient_matrix_UB_33      0.0193554

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_F_000             1018
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.497
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.116
_exptl_absorpt_coefficient_mu    2.274
_shelx_estimated_absorpt_T_min   0.398
_shelx_estimated_absorpt_T_max   0.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.64155
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Ruby
_diffrn_detector_area_resol_mean 10.4738
_diffrn_reflns_number            36492
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.791
_diffrn_reflns_theta_max         67.256
_diffrn_reflns_theta_full        67.256
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4788
_reflns_number_gt                3381
_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       'CrysAlisPro 1.171.43.120a (Rigaku OD, 2024)'
_computing_cell_refinement       'CrysAlisPro 1.171.43.120a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.120a (Rigaku OD, 2024)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'X-Seed v. 4 (Barbour, 2020)'
_computing_publication_material  'SHELXL-2019/2 (Sheldrick, 2019)'
_refine_special_details          
;
Residual electron density in the crystal which could not be interpreted
as chemically reasonable moieties was effectively removed by use
of the program 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)+(0.0500P)²+39.0000P] 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     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.0058(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4788
_refine_ls_number_parameters     331
_refine_ls_number_restraints     449
_refine_ls_R_factor_all          0.2382
_refine_ls_R_factor_gt           0.2104
_refine_ls_wR_factor_ref         0.4237
_refine_ls_wR_factor_gt          0.4144
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.004
_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 0.5986(6) 0.6752(4) 0.5770(5) 0.129(2) Uani 1 1 d . U . . .
H1 H 0.554449 0.676721 0.624518 0.194 Uiso 1 1 calc R U . . .
C10 C 0.3853(9) 0.750000 0.4789(9) 0.098(3) Uani 1 2 d S TU P . .
H10A H 0.409506 0.750000 0.557096 0.118 Uiso 1 2 calc R U P . .
H10B H 0.295383 0.749999 0.463417 0.118 Uiso 1 2 calc R U P . .
C11 C 0.5347(6) 0.6458(5) 0.4869(6) 0.0952(17) Uani 1 1 d . U . . .
C12 C 0.5768(6) 0.5815(4) 0.4463(6) 0.0910(15) Uani 1 1 d . U . . .
C13 C 0.5124(6) 0.5563(5) 0.3517(6) 0.0955(17) Uani 1 1 d . U . . .
H13A H 0.539909 0.513134 0.322658 0.115 Uiso 1 1 calc R U . . .
C14 C 0.4101(4) 0.5898(3) 0.2964(3) 0.0965(16) Uani 1 1 d D U . . .
C15 C 0.3751(6) 0.6531(5) 0.3407(6) 0.0950(18) Uani 1 1 d . U . . .
H15A H 0.306893 0.678113 0.303188 0.114 Uiso 1 1 calc R U . . .
C16 C 0.4314(6) 0.6829(5) 0.4349(6) 0.0962(16) Uani 1 1 d . U . . .
P1 P 0.32583(11) 0.55582(7) 0.17450(11) 0.0917(6) Uani 1 1 d D U . . .
O11 O 0.4048(4) 0.5649(7) 0.0895(3) 0.1401(15) Uiso 0.25 1 d D U P A 1
O12 O 0.3015(10) 0.47386(17) 0.1895(9) 0.1401(15) Uiso 0.25 1 d D U P A 1
H12 H 0.350045 0.458031 0.241719 0.210 Uiso 0.25 1 calc R U P A 1
O13 O 0.2103(3) 0.6031(3) 0.1448(10) 0.1401(15) Uiso 0.25 1 d D U P A 1
H13 H 0.207148 0.633839 0.192838 0.210 Uiso 0.25 1 calc R U P A 1
O14 O 0.4108(4) 0.5062(3) 0.1271(4) 0.1401(15) Uiso 0.25 1 d D U P A 2
O15 O 0.2143(3) 0.5125(3) 0.1982(7) 0.1401(15) Uiso 0.25 1 d D U P A 2
H15 H 0.172527 0.498949 0.140814 0.210 Uiso 0.25 1 calc R U P A 2
O16 O 0.2924(12) 0.6211(2) 0.0987(4) 0.1401(15) Uiso 0.25 1 d D U P A 2
H16 H 0.340807 0.655432 0.116993 0.210 Uiso 0.25 1 calc R U P A 2
O11' O 0.4197(3) 0.5282(4) 0.1107(4) 0.1401(15) Uiso 0.25 1 d D U P A 3
O12' O 0.2493(4) 0.4909(2) 0.2043(6) 0.1401(15) Uiso 0.25 1 d D U P A 3
H12' H 0.282273 0.473375 0.262604 0.210 Uiso 0.25 1 calc R U P A 3
O13' O 0.2588(6) 0.6209(2) 0.1141(5) 0.1401(15) Uiso 0.25 1 d D U P A 3
H13' H 0.302912 0.657928 0.123691 0.210 Uiso 0.25 1 calc R U P A 3
O14' O 0.3638(8) 0.47852(17) 0.1599(9) 0.1401(15) Uiso 0.25 1 d D U P A 4
O15' O 0.1878(3) 0.5599(8) 0.1780(10) 0.1401(15) Uiso 0.25 1 d D U P A 4
H15' H 0.149027 0.544909 0.120108 0.210 Uiso 0.25 1 calc R U P A 4
O16' O 0.3587(8) 0.6026(3) 0.0818(3) 0.1401(15) Uiso 0.25 1 d D U P A 4
H16' H 0.413888 0.632030 0.105598 0.210 Uiso 0.25 1 calc R U P A 4
O2 O 0.8759(4) 0.6370(2) 0.4930(3) 0.0817(14) Uani 1 1 d . U . . .
H2 H 0.947345 0.652777 0.507592 0.123 Uiso 1 1 calc R U . . .
C20 C 0.6862(6) 0.5391(4) 0.5077(6) 0.0913(17) Uani 1 1 d . U . . .
H20A H 0.722259 0.567319 0.570924 0.110 Uiso 1 1 calc R U . . .
H20B H 0.657094 0.492450 0.532582 0.110 Uiso 1 1 calc R U . . .
C21 C 0.8754(6) 0.5741(4) 0.4359(5) 0.0756(15) Uani 1 1 d . U . . .
C22 C 0.9667(6) 0.5610(4) 0.3769(5) 0.0819(15) Uani 1 1 d . U . . .
C23 C 0.9603(7) 0.4949(4) 0.3185(6) 0.0963(18) Uani 1 1 d . U . . .
H23A H 1.022492 0.483947 0.278066 0.116 Uiso 1 1 calc R U . . .
C24 C 0.8686(6) 0.4478(2) 0.3190(4) 0.1108(17) Uani 1 1 d D U . . .
C25 C 0.7854(8) 0.4605(4) 0.3819(6) 0.0997(18) Uani 1 1 d . U . . .
H25A H 0.725889 0.424524 0.387414 0.120 Uiso 1 1 calc R U . . .
C26 C 0.7829(6) 0.5244(4) 0.4393(5) 0.0847(15) Uani 1 1 d . U . . .
P2 P 0.85847(12) 0.36593(9) 0.24177(11) 0.1499(10) Uani 1 1 d D U . . .
O21 O 0.9868(3) 0.3418(5) 0.2380(9) 0.1568(16) Uiso 0.25 1 d D U P B 1
O22 O 0.7863(5) 0.3081(2) 0.2942(5) 0.1568(16) Uiso 0.25 1 d D U P B 1
H22A H 0.733583 0.289277 0.247727 0.235 Uiso 0.25 1 calc R U P B 1
O23 O 0.7936(7) 0.3855(6) 0.1281(3) 0.1568(16) Uiso 0.25 1 d D U P B 1
H23B H 0.758661 0.425730 0.129568 0.235 Uiso 0.25 1 calc R U P B 1
O24 O 0.9526(3) 0.3697(8) 0.1692(3) 0.1568(16) Uiso 0.25 1 d D U P B 2
O25 O 0.8950(13) 0.3031(2) 0.3221(4) 0.1568(16) Uiso 0.25 1 d D U P B 2
H25B H 0.892337 0.317822 0.384069 0.235 Uiso 0.25 1 calc R U P B 2
O26 O 0.7299(3) 0.3641(10) 0.1733(5) 0.1568(16) Uiso 0.25 1 d D U P B 2
H26A H 0.682643 0.340215 0.205201 0.235 Uiso 0.25 1 calc R U P B 2
O21' O 0.9676(4) 0.3199(3) 0.2828(8) 0.1568(16) Uiso 0.25 1 d D U P B 3
O22' O 0.7426(3) 0.3237(3) 0.2589(8) 0.1568(16) Uiso 0.25 1 d D U P B 3
H22B H 0.746574 0.281001 0.236910 0.235 Uiso 0.25 1 calc R U P B 3
O23' O 0.8529(15) 0.3847(6) 0.1226(2) 0.1568(16) Uiso 0.25 1 d D U P B 3
H23C H 0.793752 0.412407 0.103042 0.235 Uiso 0.25 1 calc R U P B 3
O24' O 0.9802(3) 0.3588(7) 0.2047(5) 0.1568(16) Uiso 0.25 1 d D U P B 4
O25' O 0.8515(11) 0.3036(2) 0.3230(4) 0.1568(16) Uiso 0.25 1 d D U P B 4
H25C H 0.921060 0.295860 0.357478 0.235 Uiso 0.25 1 calc R U P B 4
O26' O 0.7623(5) 0.3807(7) 0.1413(3) 0.1568(16) Uiso 0.25 1 d D U P B 4
H26B H 0.760162 0.425227 0.127723 0.235 Uiso 0.25 1 calc R U P B 4
O3 O 1.0639(7) 0.750000 0.4845(5) 0.115(3) Uani 1 2 d S TU P . .
H3A H 1.083234 0.708256 0.507405 0.173 Uiso 0.5 1 calc R U P . .
C30 C 1.0734(6) 0.6139(4) 0.3807(6) 0.0847(16) Uani 1 1 d . U . . .
H30A H 1.139499 0.589287 0.351302 0.102 Uiso 1 1 calc R U . . .
H30B H 1.104403 0.625483 0.455998 0.102 Uiso 1 1 calc R U . . .
C31 C 1.0499(8) 0.750000 0.3748(7) 0.080(2) Uani 1 2 d S TU P . .
C34 C 1.0025(9) 0.750000 0.1558(4) 0.094(2) Uani 1 2 d DS TU P C .
C35 C 1.0192(6) 0.6857(4) 0.2137(5) 0.0843(16) Uani 1 1 d . U . . .
H35A H 1.013168 0.640879 0.176634 0.101 Uiso 1 1 calc R U . . .
C36 C 1.0436(6) 0.6854(4) 0.3200(5) 0.0799(14) Uani 1 1 d . U . . .
P3 P 0.9679(2) 0.750000 0.01377(19) 0.1089(11) Uani 1 2 d DS TU P . .
O31 O 0.9598(10) 0.82600(17) -0.0290(5) 0.158(3) Uiso 0.5 1 d D U P C -1
O32 O 0.8410(3) 0.7135(3) -0.0139(8) 0.158(3) Uiso 0.5 1 d D U P C -1
H32 H 0.793705 0.731163 0.024433 0.237 Uiso 0.5 1 calc R U P C -1
O33 O 1.0726(3) 0.7069(3) -0.0239(5) 0.158(3) Uiso 0.5 1 d D U P C -1
H33 H 1.139656 0.722323 0.007818 0.237 Uiso 0.5 1 calc R U P C -1
C01 C 0.6922(17) 0.750000 0.2819(15) 0.077(5) Uiso 0.5 2 d S . P . .
O02 O 0.6520(19) 0.750000 0.1662(17) 0.156(7) Uiso 0.5 2 d S . P . .
O03 O 1.000000 0.500000 0.000000 0.147(7) Uiso 0.5 2 d S . P . .
O05 O 0.358(2) 0.750000 0.054(2) 0.182(9) Uiso 0.5 2 d S . P . .
O04 O 0.6868(13) 0.5722(9) 0.1106(12) 0.158(5) Uiso 0.5 1 d . . 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
O1 C11 1.364(9) . ?
O1 H1 0.8400 . ?
C10 C16 1.485(10) . ?
C10 C16 1.485(10) 4_575 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.406(11) . ?
C11 C16 1.411(10) . ?
C12 C13 1.382(10) . ?
C12 C20 1.551(10) . ?
C13 C14 1.387(8) . ?
C13 H13A 0.9500 . ?
C14 C15 1.381(10) . ?
C14 P1 1.796(4) . ?
C15 C16 1.378(10) . ?
C15 H15A 0.9500 . ?
P1 O14' 1.508(4) . ?
P1 O11 1.511(4) . ?
P1 O14 1.511(4) . ?
P1 O11' 1.513(4) . ?
P1 O15' 1.548(3) . ?
P1 O15 1.549(4) . ?
P1 O13 1.551(4) . ?
P1 O13' 1.552(4) . ?
P1 O16 1.553(4) . ?
P1 O12' 1.554(4) . ?
P1 O16' 1.554(4) . ?
P1 O12 1.554(3) . ?
O12 H12 0.8400 . ?
O13 H13 0.8400 . ?
O15 H15 0.8400 . ?
O16 H16 0.8400 . ?
O12' H12' 0.8400 . ?
O13' H13' 0.8400 . ?
O15' H15' 0.8400 . ?
O16' H16' 0.8400 . ?
O2 C21 1.371(8) . ?
O2 H2 0.8400 . ?
C20 C26 1.516(10) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.380(10) . ?
C21 C26 1.387(9) . ?
C22 C23 1.425(10) . ?
C22 C30 1.534(10) . ?
C23 C24 1.343(9) . ?
C23 H23A 0.9500 . ?
C24 C25 1.341(10) . ?
C24 P2 1.797(4) . ?
C25 C26 1.391(10) . ?
C25 H25A 0.9500 . ?
P2 O21 1.507(4) . ?
P2 O21' 1.507(4) . ?
P2 O24 1.509(4) . ?
P2 O24' 1.513(4) . ?
P2 O23' 1.550(4) . ?
P2 O22 1.551(4) . ?
P2 O23 1.555(4) . ?
P2 O26 1.555(4) . ?
P2 O22' 1.555(4) . ?
P2 O26' 1.557(4) . ?
P2 O25 1.557(4) . ?
P2 O25' 1.558(4) . ?
O22 H22A 0.8400 . ?
O23 H23B 0.8400 . ?
O25 H25B 0.8400 . ?
O26 H26A 0.8400 . ?
O22' H22B 0.8400 . ?
O23' H23C 0.8400 . ?
O25' H25C 0.8400 . ?
O26' H26B 0.8400 . ?
O3 C31 1.382(11) . ?
O3 H3A 0.8400 . ?
O3 H3A 0.84(7) 4_575 ?
C30 C36 1.539(10) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C36 1.378(8) . ?
C31 C36 1.378(8) 4_575 ?
C34 C35 1.394(7) 4_575 ?
C34 C35 1.394(7) . ?
C34 P3 1.790(5) . ?
C35 C36 1.339(9) . ?
C35 H35A 0.9500 . ?
P3 O31 1.503(3) . ?
P3 O33 1.551(4) . ?
P3 O32 1.556(4) . ?
O32 H32 0.8400 . ?
O33 H33 0.8400 . ?
C01 O02 1.47(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 O1 H1 109.5 . . ?
C16 C10 C16 113.0(10) . 4_575 ?
C16 C10 H10A 109.0 . . ?
C16 C10 H10A 109.0 4_575 . ?
C16 C10 H10B 109.0 . . ?
C16 C10 H10B 109.0 4_575 . ?
H10A C10 H10B 107.8 . . ?
O1 C11 C12 119.0(6) . . ?
O1 C11 C16 118.7(8) . . ?
C12 C11 C16 122.2(7) . . ?
C13 C12 C11 116.6(7) . . ?
C13 C12 C20 121.8(7) . . ?
C11 C12 C20 121.5(6) . . ?
C12 C13 C14 124.3(7) . . ?
C12 C13 H13A 117.8 . . ?
C14 C13 H13A 117.8 . . ?
C15 C14 C13 115.7(5) . . ?
C15 C14 P1 120.4(4) . . ?
C13 C14 P1 123.9(5) . . ?
C16 C15 C14 125.1(7) . . ?
C16 C15 H15A 117.5 . . ?
C14 C15 H15A 117.5 . . ?
C15 C16 C11 116.1(8) . . ?
C15 C16 C10 121.7(7) . . ?
C11 C16 C10 122.2(7) . . ?
O14' P1 O15' 110.4(6) . . ?
O14 P1 O15 109.9(3) . . ?
O11 P1 O13 108.6(5) . . ?
O11' P1 O13' 108.3(4) . . ?
O14 P1 O16 108.9(4) . . ?
O15 P1 O16 113.7(5) . . ?
O11' P1 O12' 109.0(4) . . ?
O13' P1 O12' 118.6(3) . . ?
O14' P1 O16' 109.1(5) . . ?
O15' P1 O16' 110.6(6) . . ?
O11 P1 O12 109.2(6) . . ?
O13 P1 O12 115.0(5) . . ?
P1 O12 H12 109.5 . . ?
P1 O13 H13 109.5 . . ?
P1 O15 H15 109.5 . . ?
P1 O16 H16 109.5 . . ?
P1 O12' H12' 109.5 . . ?
P1 O13' H13' 109.5 . . ?
P1 O15' H15' 109.5 . . ?
P1 O16' H16' 109.5 . . ?
C21 O2 H2 109.5 . . ?
C26 C20 C12 112.0(6) . . ?
C26 C20 H20A 109.2 . . ?
C12 C20 H20A 109.2 . . ?
C26 C20 H20B 109.2 . . ?
C12 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
O2 C21 C22 119.9(6) . . ?
O2 C21 C26 118.9(6) . . ?
C22 C21 C26 121.2(6) . . ?
C21 C22 C23 117.1(7) . . ?
C21 C22 C30 120.4(6) . . ?
C23 C22 C30 122.3(6) . . ?
C24 C23 C22 121.8(7) . . ?
C24 C23 H23A 119.1 . . ?
C22 C23 H23A 119.1 . . ?
C25 C24 C23 119.3(5) . . ?
C25 C24 P2 119.1(5) . . ?
C23 C24 P2 121.6(5) . . ?
C24 C25 C26 122.6(7) . . ?
C24 C25 H25A 118.7 . . ?
C26 C25 H25A 118.7 . . ?
C21 C26 C25 117.8(7) . . ?
C21 C26 C20 120.1(6) . . ?
C25 C26 C20 122.1(7) . . ?
O21' P2 O23' 111.7(7) . . ?
O21 P2 O22 111.8(4) . . ?
O21 P2 O23 110.0(5) . . ?
O22 P2 O23 111.5(5) . . ?
O24 P2 O26 109.0(3) . . ?
O21' P2 O22' 108.1(3) . . ?
O23' P2 O22' 110.3(7) . . ?
O24' P2 O26' 107.0(3) . . ?
O24 P2 O25 107.7(6) . . ?
O26 P2 O25 118.3(8) . . ?
O24' P2 O25' 106.7(6) . . ?
O26' P2 O25' 125.1(6) . . ?
P2 O22 H22A 109.5 . . ?
P2 O23 H23B 109.5 . . ?
P2 O25 H25B 109.5 . . ?
P2 O26 H26A 109.5 . . ?
P2 O22' H22B 109.5 . . ?
P2 O23' H23C 109.5 . . ?
P2 O25' H25C 109.5 . . ?
P2 O26' H26B 109.5 . . ?
C31 O3 H3A 109.5 . . ?
C31 O3 H3A 109.5(18) . 4_575 ?
H3A O3 H3A 133.1 . 4_575 ?
C22 C30 C36 115.3(5) . . ?
C22 C30 H30A 108.5 . . ?
C36 C30 H30A 108.5 . . ?
C22 C30 H30B 108.5 . . ?
C36 C30 H30B 108.5 . . ?
H30A C30 H30B 107.5 . . ?
C36 C31 C36 119.8(9) . 4_575 ?
C36 C31 O3 120.1(4) . . ?
C36 C31 O3 120.1(4) 4_575 . ?
C35 C34 C35 116.7(6) 4_575 . ?
C35 C34 P3 121.6(3) 4_575 . ?
C35 C34 P3 121.6(3) . . ?
C36 C35 C34 121.8(6) . . ?
C36 C35 H35A 119.1 . . ?
C34 C35 H35A 119.1 . . ?
C35 C36 C31 119.7(7) . . ?
C35 C36 C30 120.3(6) . . ?
C31 C36 C30 119.8(6) . . ?
O31 P3 O33 111.7(5) . . ?
O31 P3 O32 108.8(5) . . ?
O33 P3 O32 114.2(3) . . ?
O31 P3 C34 111.0(3) . . ?
O33 P3 C34 105.2(4) . . ?
O32 P3 C34 105.7(5) . . ?
P3 O32 H32 109.5 . . ?
P3 O33 H33 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C11 C12 C13 -176.6(7) . . . . ?
C16 C11 C12 C13 0.5(11) . . . . ?
O1 C11 C12 C20 6.5(11) . . . . ?
C16 C11 C12 C20 -176.5(7) . . . . ?
C11 C12 C13 C14 -0.6(11) . . . . ?
C20 C12 C13 C14 176.4(6) . . . . ?
C12 C13 C14 C15 1.3(10) . . . . ?
C12 C13 C14 P1 -179.1(6) . . . . ?
C13 C14 C15 C16 -2.0(10) . . . . ?
P1 C14 C15 C16 178.3(6) . . . . ?
C14 C15 C16 C11 2.0(12) . . . . ?
C14 C15 C16 C10 -177.8(7) . . . . ?
O1 C11 C16 C15 175.9(7) . . . . ?
C12 C11 C16 C15 -1.1(11) . . . . ?
O1 C11 C16 C10 -4.3(12) . . . . ?
C12 C11 C16 C10 178.7(8) . . . . ?
C16 C10 C16 C15 -85.2(10) 4_575 . . . ?
C16 C10 C16 C11 95.0(10) 4_575 . . . ?
C13 C12 C20 C26 56.0(9) . . . . ?
C11 C12 C20 C26 -127.2(7) . . . . ?
O2 C21 C22 C23 -179.4(6) . . . . ?
C26 C21 C22 C23 1.2(10) . . . . ?
O2 C21 C22 C30 4.1(9) . . . . ?
C26 C21 C22 C30 -175.4(6) . . . . ?
C21 C22 C23 C24 1.0(10) . . . . ?
C30 C22 C23 C24 177.5(6) . . . . ?
C22 C23 C24 C25 -4.8(10) . . . . ?
C22 C23 C24 P2 178.0(5) . . . . ?
C23 C24 C25 C26 6.5(10) . . . . ?
P2 C24 C25 C26 -176.2(5) . . . . ?
O2 C21 C26 C25 -179.1(6) . . . . ?
C22 C21 C26 C25 0.4(10) . . . . ?
O2 C21 C26 C20 -1.5(9) . . . . ?
C22 C21 C26 C20 177.9(6) . . . . ?
C24 C25 C26 C21 -4.3(10) . . . . ?
C24 C25 C26 C20 178.2(6) . . . . ?
C12 C20 C26 C21 89.3(8) . . . . ?
C12 C20 C26 C25 -93.2(8) . . . . ?
C21 C22 C30 C36 -74.3(8) . . . . ?
C23 C22 C30 C36 109.4(7) . . . . ?
C35 C34 C35 C36 3.6(14) 4_575 . . . ?
P3 C34 C35 C36 -179.2(6) . . . . ?
C34 C35 C36 C31 1.5(12) . . . . ?
C34 C35 C36 C30 -174.3(7) . . . . ?
C36 C31 C36 C35 -6.7(13) 4_575 . . . ?
O3 C31 C36 C35 174.0(7) . . . . ?
C36 C31 C36 C30 169.1(5) 4_575 . . . ?
O3 C31 C36 C30 -10.2(12) . . . . ?
C22 C30 C36 C35 -69.3(9) . . . . ?
C22 C30 C36 C31 114.9(8) . . . . ?
C35 C34 P3 O31 -0.4(10) 4_575 . . . ?
C35 C34 P3 O31 -177.5(8) . . . . ?
C35 C34 P3 O33 120.7(8) 4_575 . . . ?
C35 C34 P3 O33 -56.5(8) . . . . ?
C35 C34 P3 O32 -118.1(8) 4_575 . . . ?
C35 C34 P3 O32 64.7(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C15 H15A O13^a 0.95 2.54 2.999(12) 109.8 . yes
O15^b H15^b O03 0.84 2.41 3.196(7) 155.6 1_455 yes
O16^b H16^b O05 0.84 1.95 2.579(12) 131.4 . yes
O13'^c H13'^c O05 0.84 2.06 2.787(15) 144.7 . yes
O15'^d H15'^d O03 0.84 2.23 3.039(10) 161.3 1_455 yes
O16'^d H16'^d O05 0.84 2.33 2.744(6) 110.6 . yes
O2 H2 O3 0.84 2.26 2.971(7) 142.1 . yes
C23 H23A O15^b 0.95 2.57 3.445(10) 154.0 1_655 yes
O25^b H25B^b O3 0.84 2.09 2.625(7) 121.5 3_766 yes
O22'^c H22B^c O22'^c 0.84 1.95 2.720(12) 151.1 4_565 yes
O25'^d H25C^d O3 0.84 2.17 2.674(8) 118.7 3_766 yes
O3 H3A O2 0.84 2.64 2.971(7) 105.0 . yes
O3 H3A O25^b 0.84 2.16 2.625(7) 114.9 3_766 yes
O3 H3A O25'^d 0.84 2.18 2.674(8) 117.6 3_766 yes
C35 H35A O15'^d 0.95 2.45 3.068(14) 122.3 1_655 yes
O32^a H32^a O02 0.84 2.61 3.42(2) 164.0 . yes
O33^a H33^a O05 0.84 2.46 3.27(2) 162.3 1_655 yes

_refine_diff_density_max         1.495
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.161



####################################################################### 
# 
# 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_tc030
_database_code_depnum_ccdc_archive 'CCDC 2441441'
loop_
_audit_author_name
_audit_author_address
'Alexandre Sobolev'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2025-04-07 deposited with the CCDC.	2025-10-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H78 O6 Br6, 2(C8 H10)'
_chemical_formula_sum            'C82 H98 Br6 O6'
_chemical_formula_weight         1659.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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                   12.440(2)
_cell_length_b                   12.492(2)
_cell_length_c                   13.378(2)
_cell_angle_alpha                87.009(3)
_cell_angle_beta                 84.350(3)
_cell_angle_gamma                68.214(2)
_cell_volume                     1920.8(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    8156
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      27.96

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_F_000             848
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    3.186
_shelx_estimated_absorpt_T_min   0.328
_shelx_estimated_absorpt_T_max   0.646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3282
_exptl_absorpt_correction_T_max  0.6465
_exptl_absorpt_process_details   
'SADABS - Bruker area detector absorption corrections'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17149
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.530
_diffrn_reflns_theta_max         28.020
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             8932
_reflns_number_gt                7126
_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 SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL, v. 5.1'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'X-Seed v. 4.0 (Barbour, 2020)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0872P)²+2.2796P] 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         8932
_refine_ls_number_parameters     449
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0511
_refine_ls_wR_factor_ref         0.1567
_refine_ls_wR_factor_gt          0.1497
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br -0.07503(5) 0.31527(4) 0.35985(4) 0.05632(16) Uani 1 1 d . . . . .
O1 O -0.1642(2) -0.1211(2) 0.32139(16) 0.0245(5) Uani 1 1 d D . . . .
C11 C -0.1440(3) -0.0211(3) 0.3328(2) 0.0218(6) Uani 1 1 d . . . . .
C12 C -0.0342(3) -0.0279(3) 0.3556(2) 0.0219(6) Uani 1 1 d . . . . .
C13 C -0.0143(3) 0.0736(3) 0.3619(3) 0.0269(7) Uani 1 1 d . . . . .
H13D H 0.059433 0.071299 0.377454 0.032 Uiso 1 1 calc R U . . .
C14 C -0.1030(3) 0.1790(3) 0.3454(3) 0.0306(7) Uani 1 1 d . . . . .
C15 C -0.2096(3) 0.1846(3) 0.3211(2) 0.0268(7) Uani 1 1 d . . . . .
H15A H -0.268259 0.257345 0.308660 0.032 Uiso 1 1 calc R U . . .
C16 C -0.2320(3) 0.0847(3) 0.3145(2) 0.0233(6) Uani 1 1 d . . . . .
C10 C -0.1922(15) -0.1760(7) 0.4125(5) 0.0332(15) Uani 0.696(5) 1 d D . P A 1
H10A H -0.264762 -0.124266 0.448553 0.040 Uiso 0.696(5) 1 calc R U P A 1
H10B H -0.128664 -0.196608 0.457544 0.040 Uiso 0.696(5) 1 calc R U P A 1
C17 C -0.2070(4) -0.2833(4) 0.3791(5) 0.0370(12) Uani 0.696(5) 1 d D . P A 1
H17A H -0.260506 -0.261838 0.325027 0.044 Uiso 0.696(5) 1 calc R U P A 1
H17B H -0.243327 -0.315028 0.436319 0.044 Uiso 0.696(5) 1 calc R U P A 1
C18 C -0.0929(5) -0.3765(5) 0.3410(4) 0.0392(12) Uani 0.696(5) 1 d D . P A 1
H18A H -0.109467 -0.435048 0.304845 0.047 Uiso 0.696(5) 1 calc R U P A 1
H18B H -0.048847 -0.341624 0.293063 0.047 Uiso 0.696(5) 1 calc R U P A 1
C19 C -0.0193(7) -0.4347(7) 0.4276(6) 0.070(2) Uani 0.696(5) 1 d D . P A 1
H19A H 0.053370 -0.494114 0.401014 0.105 Uiso 0.696(5) 1 calc R U P A 1
H19B H -0.001759 -0.377047 0.462747 0.105 Uiso 0.696(5) 1 calc R U P A 1
H19C H -0.062318 -0.470377 0.474517 0.105 Uiso 0.696(5) 1 calc R U P A 1
C10' C -0.182(4) -0.1717(13) 0.4188(9) 0.0332(15) Uani 0.304(5) 1 d D . P A 2
H10C H -0.141244 -0.147026 0.467780 0.040 Uiso 0.304(5) 1 calc R U P A 2
H10D H -0.265783 -0.140417 0.440771 0.040 Uiso 0.304(5) 1 calc R U P A 2
C17' C -0.1395(10) -0.3028(10) 0.4219(9) 0.0370(12) Uani 0.304(5) 1 d D . P A 2
H17C H -0.054905 -0.334843 0.402512 0.044 Uiso 0.304(5) 1 calc R U P A 2
H17D H -0.152569 -0.329004 0.491578 0.044 Uiso 0.304(5) 1 calc R U P A 2
C18' C -0.2003(11) -0.3496(12) 0.3529(9) 0.0392(12) Uani 0.304(5) 1 d D . P A 2
H18C H -0.281991 -0.295832 0.351510 0.047 Uiso 0.304(5) 1 calc R U P A 2
H18D H -0.200889 -0.424555 0.380202 0.047 Uiso 0.304(5) 1 calc R U P A 2
C19' C -0.1430(17) -0.3661(18) 0.2460(9) 0.070(2) Uani 0.304(5) 1 d D . P A 2
H19D H -0.185776 -0.396403 0.204766 0.105 Uiso 0.304(5) 1 calc R U P A 2
H19E H -0.143655 -0.291834 0.217790 0.105 Uiso 0.304(5) 1 calc R U P A 2
H19F H -0.062513 -0.420621 0.246496 0.105 Uiso 0.304(5) 1 calc R U P A 2
C1 C 0.0623(3) -0.1443(3) 0.3715(2) 0.0241(6) Uani 1 1 d . . . . .
H1A H 0.064781 -0.162110 0.444403 0.029 Uiso 1 1 calc R U . . .
H1B H 0.044136 -0.204764 0.339794 0.029 Uiso 1 1 calc R U . . .
Br2 Br 0.46471(3) -0.10197(4) 0.42872(3) 0.03467(12) Uani 1 1 d . . . . .
O2 O 0.1451(2) -0.2043(2) 0.17115(17) 0.0268(5) Uani 1 1 d D . . . .
C21 C 0.2159(3) -0.1739(3) 0.2271(2) 0.0219(6) Uani 1 1 d . . . . .
C22 C 0.3255(3) -0.1800(3) 0.1849(2) 0.0224(6) Uani 1 1 d . . . . .
C23 C 0.3988(3) -0.1570(3) 0.2458(2) 0.0251(7) Uani 1 1 d . . . . .
H23A H 0.473145 -0.159283 0.218772 0.030 Uiso 1 1 calc R U . . .
C24 C 0.3630(3) -0.1310(3) 0.3456(2) 0.0234(6) Uani 1 1 d . . . . .
C25 C 0.2552(3) -0.1265(3) 0.3880(2) 0.0224(6) Uani 1 1 d . . . . .
H25A H 0.232832 -0.108879 0.456972 0.027 Uiso 1 1 calc R U . . .
C26 C 0.1801(3) -0.1480(3) 0.3285(2) 0.0208(6) Uani 1 1 d . . . . .
C20 C 0.0730(3) -0.1134(3) 0.1083(3) 0.0318(8) Uani 1 1 d D . . . .
H20A H 0.121800 -0.087963 0.056991 0.038 Uiso 1 1 calc R U . . .
H20B H 0.023765 -0.046374 0.149417 0.038 Uiso 1 1 calc R U . . .
C27 C -0.0016(4) -0.1631(5) 0.0587(3) 0.0515(12) Uani 1 1 d D . . . .
H27A H -0.060576 -0.100914 0.022851 0.062 Uiso 1 1 calc R U . . .
H27B H -0.042898 -0.196541 0.110756 0.062 Uiso 1 1 calc R U . . .
C28 C 0.0731(5) -0.2575(6) -0.0163(4) 0.0764(19) Uani 1 1 d D . . . .
H28A H 0.113083 -0.223001 -0.068468 0.092 Uiso 1 1 calc R U . . .
H28B H 0.133491 -0.317916 0.019857 0.092 Uiso 1 1 calc R U . . .
C29 C 0.0040(7) -0.3131(9) -0.0669(6) 0.119(3) Uani 1 1 d D U . . .
H29A H 0.056393 -0.371851 -0.113272 0.178 Uiso 1 1 calc R U . . .
H29B H -0.034295 -0.349285 -0.015928 0.178 Uiso 1 1 calc R U . . .
H29C H -0.054724 -0.254274 -0.104342 0.178 Uiso 1 1 calc R U . . .
C2 C 0.3667(3) -0.2185(3) 0.0779(2) 0.0261(7) Uani 1 1 d . . . . .
H2A H 0.322153 -0.264216 0.058337 0.031 Uiso 1 1 calc R U . . .
H2B H 0.449331 -0.270326 0.075967 0.031 Uiso 1 1 calc R U . . .
Br3 Br 0.32826(4) 0.21813(4) -0.01474(3) 0.03907(13) Uani 1 1 d . . . . .
O3 O 0.35619(19) -0.2520(2) -0.12888(17) 0.0243(5) Uani 1 1 d D . . . .
C31 C 0.3560(3) -0.1466(3) -0.1020(2) 0.0209(6) Uani 1 1 d . . . . .
C32 C 0.3492(3) -0.0626(3) -0.1771(2) 0.0228(6) Uani 1 1 d . . . . .
C33 C 0.3415(3) 0.0457(3) -0.1499(2) 0.0246(7) Uani 1 1 d . . . . .
H33A H 0.336479 0.103794 -0.199974 0.029 Uiso 1 1 calc R U . . .
C34 C 0.3410(3) 0.0691(3) -0.0503(2) 0.0249(7) Uani 1 1 d . . . . .
C35 C 0.3472(3) -0.0137(3) 0.0247(2) 0.0244(7) Uani 1 1 d . . . . .
H35A H 0.345807 0.004508 0.093029 0.029 Uiso 1 1 calc R U . . .
C36 C 0.3555(3) -0.1228(3) -0.0003(2) 0.0222(6) Uani 1 1 d . . . . .
C30 C 0.4667(9) -0.3486(8) -0.1335(17) 0.0296(10) Uani 0.5 1 d D . P B 1
H30A H 0.489811 -0.374040 -0.064898 0.036 Uiso 0.5 1 calc R U P B 1
H30B H 0.527938 -0.325731 -0.170635 0.036 Uiso 0.5 1 calc R U P B 1
C37 C 0.4517(7) -0.4456(7) -0.1872(7) 0.0427(13) Uani 0.5 1 d D . P B 1
H37A H 0.439836 -0.422141 -0.258341 0.051 Uiso 0.5 1 calc R U P B 1
H37B H 0.524439 -0.514271 -0.186077 0.051 Uiso 0.5 1 calc R U P B 1
C38 C 0.3515(19) -0.479(3) -0.1427(13) 0.046(2) Uani 0.5 1 d D . P B 1
H38A H 0.279976 -0.409245 -0.134375 0.055 Uiso 0.5 1 calc R U P B 1
H38B H 0.368660 -0.515482 -0.075671 0.055 Uiso 0.5 1 calc R U P B 1
C39 C 0.3323(10) -0.5629(10) -0.2110(9) 0.062(2) Uani 0.5 1 d D . P B 1
H39A H 0.267400 -0.583903 -0.181510 0.094 Uiso 0.5 1 calc R U P B 1
H39B H 0.314336 -0.526400 -0.277112 0.094 Uiso 0.5 1 calc R U P B 1
H39C H 0.402863 -0.632449 -0.218511 0.094 Uiso 0.5 1 calc R U P B 1
C30' C 0.4707(8) -0.3427(8) -0.1374(17) 0.0296(10) Uani 0.5 1 d D . P B 2
H30C H 0.522521 -0.326338 -0.093843 0.036 Uiso 0.5 1 calc R U P B 2
H30D H 0.505390 -0.347600 -0.207639 0.036 Uiso 0.5 1 calc R U P B 2
C37' C 0.4564(8) -0.4554(7) -0.1047(7) 0.0427(13) Uani 0.5 1 d D . P B 2
H37C H 0.428229 -0.450822 -0.032667 0.051 Uiso 0.5 1 calc R U P B 2
H37D H 0.533481 -0.518547 -0.111917 0.051 Uiso 0.5 1 calc R U P B 2
C38' C 0.3735(19) -0.486(3) -0.1631(12) 0.046(2) Uani 0.5 1 d D . P B 2
H38C H 0.298558 -0.419368 -0.162513 0.055 Uiso 0.5 1 calc R U P B 2
H38D H 0.358492 -0.551919 -0.129716 0.055 Uiso 0.5 1 calc R U P B 2
C39' C 0.4213(10) -0.5159(10) -0.2715(7) 0.062(2) Uani 0.5 1 d D . P B 2
H39D H 0.365220 -0.534868 -0.306499 0.094 Uiso 0.5 1 calc R U P B 2
H39E H 0.434818 -0.449960 -0.305305 0.094 Uiso 0.5 1 calc R U P B 2
H39F H 0.494738 -0.582477 -0.272517 0.094 Uiso 0.5 1 calc R U P B 2
C3 C 0.3500(3) -0.0906(3) -0.2870(2) 0.0245(7) Uani 1 1 d . . . . .
H3A H 0.374466 -0.035638 -0.330399 0.029 Uiso 1 1 calc R U . . .
H3B H 0.407831 -0.169041 -0.300508 0.029 Uiso 1 1 calc R U . . .
C1A C 0.2730(4) 0.3008(4) 0.2894(3) 0.0414(9) Uani 1 1 d . . . . .
C2A C 0.3274(4) 0.3294(4) 0.3632(3) 0.0425(10) Uani 1 1 d . . . . .
H2AA H 0.371006 0.270406 0.407144 0.051 Uiso 1 1 calc R U . . .
C3A C 0.3204(5) 0.4411(6) 0.3752(4) 0.0608(15) Uani 1 1 d . . . . .
C4A C 0.2621(6) 0.5240(6) 0.3114(7) 0.082(2) Uani 1 1 d . . . . .
H4AA H 0.258103 0.600650 0.318886 0.098 Uiso 1 1 calc R U . . .
C5A C 0.2086(6) 0.5004(5) 0.2360(6) 0.084(2) Uani 1 1 d . . . . .
H5AA H 0.168663 0.560495 0.191292 0.100 Uiso 1 1 calc R U . . .
C6A C 0.2116(5) 0.3891(5) 0.2236(4) 0.0576(12) Uani 1 1 d . . . . .
H6AA H 0.172907 0.373152 0.171721 0.069 Uiso 1 1 calc R U . . .
C11A C 0.2805(5) 0.1795(5) 0.2786(4) 0.0613(14) Uani 1 1 d . . . . .
H11A H 0.236864 0.175857 0.222627 0.092 Uiso 1 1 calc R U . . .
H11B H 0.362096 0.128848 0.265423 0.092 Uiso 1 1 calc R U . . .
H11C H 0.247624 0.154226 0.340814 0.092 Uiso 1 1 calc R U . . .
C13A C 0.3760(7) 0.4689(8) 0.4602(6) 0.100(3) Uani 1 1 d . U . . .
H13A H 0.414452 0.398296 0.498700 0.151 Uiso 1 1 calc R U . . .
H13B H 0.433432 0.501612 0.432993 0.151 Uiso 1 1 calc R U . . .
H13C H 0.316169 0.524914 0.504236 0.151 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 C14 1.882(4) . ?
O1 C11 1.380(4) . ?
O1 C10 1.444(6) . ?
O1 C10' 1.451(10) . ?
C11 C16 1.396(5) . ?
C11 C12 1.400(4) . ?
C12 C13 1.388(5) . ?
C12 C1 1.524(5) . ?
C13 C14 1.392(5) . ?
C13 H13D 0.9500 . ?
C14 C15 1.372(5) . ?
C15 C16 1.385(5) . ?
C15 H15A 0.9500 . ?
C16 C3 1.523(4) 2 ?
C10 C17 1.514(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C17 C18 1.524(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.528(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C10' C17' 1.523(10) . ?
C10' H10C 0.9900 . ?
C10' H10D 0.9900 . ?
C17' C18' 1.512(9) . ?
C17' H17C 0.9900 . ?
C17' H17D 0.9900 . ?
C18' C19' 1.522(9) . ?
C18' H18C 0.9900 . ?
C18' H18D 0.9900 . ?
C19' H19D 0.9800 . ?
C19' H19E 0.9800 . ?
C19' H19F 0.9800 . ?
C1 C26 1.506(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
Br2 C24 1.904(3) . ?
O2 C21 1.374(4) . ?
O2 C20 1.447(4) . ?
C21 C22 1.400(4) . ?
C21 C26 1.401(4) . ?
C22 C23 1.394(5) . ?
C22 C2 1.512(4) . ?
C23 C24 1.382(4) . ?
C23 H23A 0.9500 . ?
C24 C25 1.386(4) . ?
C25 C26 1.391(4) . ?
C25 H25A 0.9500 . ?
C20 C27 1.510(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C27 C28 1.545(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.512(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C2 C36 1.522(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
Br3 C34 1.891(4) . ?
O3 C31 1.382(4) . ?
O3 C30' 1.453(8) . ?
O3 C30 1.453(8) . ?
C31 C32 1.400(5) . ?
C31 C36 1.406(4) . ?
C32 C33 1.385(5) . ?
C32 C3 1.528(4) . ?
C33 C34 1.379(5) . ?
C33 H33A 0.9500 . ?
C34 C35 1.390(5) . ?
C35 C36 1.385(5) . ?
C35 H35A 0.9500 . ?
C30 C37 1.518(10) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C37 C38 1.516(9) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.522(9) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C30' C37' 1.520(10) . ?
C30' H30C 0.9900 . ?
C30' H30D 0.9900 . ?
C37' C38' 1.515(9) . ?
C37' H37C 0.9900 . ?
C37' H37D 0.9900 . ?
C38' C39' 1.523(9) . ?
C38' H38C 0.9900 . ?
C38' H38D 0.9900 . ?
C39' H39D 0.9800 . ?
C39' H39E 0.9800 . ?
C39' H39F 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C1A C2A 1.382(6) . ?
C1A C6A 1.407(7) . ?
C1A C11A 1.497(7) . ?
C2A C3A 1.383(7) . ?
C2A H2AA 0.9500 . ?
C3A C4A 1.341(10) . ?
C3A C13A 1.505(8) . ?
C4A C5A 1.363(10) . ?
C4A H4AA 0.9500 . ?
C5A C6A 1.396(9) . ?
C5A H5AA 0.9500 . ?
C6A H6AA 0.9500 . ?
C11A H11A 0.9800 . ?
C11A H11B 0.9800 . ?
C11A H11C 0.9800 . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C13A H13C 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
C11 O1 C10 116.4(3) . . ?
C11 O1 C10' 110.4(7) . . ?
O1 C11 C16 118.7(3) . . ?
O1 C11 C12 119.6(3) . . ?
C16 C11 C12 121.5(3) . . ?
C13 C12 C11 118.6(3) . . ?
C13 C12 C1 120.6(3) . . ?
C11 C12 C1 120.9(3) . . ?
C12 C13 C14 119.7(3) . . ?
C12 C13 H13D 120.2 . . ?
C14 C13 H13D 120.2 . . ?
C15 C14 C13 121.3(3) . . ?
C15 C14 Br1 120.2(3) . . ?
C13 C14 Br1 118.5(3) . . ?
C14 C15 C16 120.3(3) . . ?
C14 C15 H15A 119.8 . . ?
C16 C15 H15A 119.8 . . ?
C15 C16 C11 118.6(3) . . ?
C15 C16 C3 120.4(3) . 2 ?
C11 C16 C3 121.0(3) . 2 ?
O1 C10 C17 105.5(5) . . ?
O1 C10 H10A 110.6 . . ?
C17 C10 H10A 110.6 . . ?
O1 C10 H10B 110.6 . . ?
C17 C10 H10B 110.6 . . ?
H10A C10 H10B 108.8 . . ?
C10 C17 C18 113.2(7) . . ?
C10 C17 H17A 108.9 . . ?
C18 C17 H17A 108.9 . . ?
C10 C17 H17B 108.9 . . ?
C18 C17 H17B 108.9 . . ?
H17A C17 H17B 107.8 . . ?
C19 C18 C17 111.2(5) . . ?
C19 C18 H18A 109.4 . . ?
C17 C18 H18A 109.4 . . ?
C19 C18 H18B 109.4 . . ?
C17 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17' C10' O1 115.1(11) . . ?
C17' C10' H10C 108.5 . . ?
O1 C10' H10C 108.5 . . ?
C17' C10' H10D 108.5 . . ?
O1 C10' H10D 108.5 . . ?
H10C C10' H10D 107.5 . . ?
C18' C17' C10' 112.8(10) . . ?
C18' C17' H17C 109.0 . . ?
C10' C17' H17C 109.0 . . ?
C18' C17' H17D 109.0 . . ?
C10' C17' H17D 109.0 . . ?
H17C C17' H17D 107.8 . . ?
C17' C18' C19' 113.0(8) . . ?
C17' C18' H18C 109.0 . . ?
C19' C18' H18C 109.0 . . ?
C17' C18' H18D 109.0 . . ?
C19' C18' H18D 109.0 . . ?
H18C C18' H18D 107.8 . . ?
C18' C19' H19D 109.5 . . ?
C18' C19' H19E 109.5 . . ?
H19D C19' H19E 109.5 . . ?
C18' C19' H19F 109.5 . . ?
H19D C19' H19F 109.5 . . ?
H19E C19' H19F 109.5 . . ?
C26 C1 C12 113.0(3) . . ?
C26 C1 H1A 109.0 . . ?
C12 C1 H1A 109.0 . . ?
C26 C1 H1B 109.0 . . ?
C12 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C21 O2 C20 115.5(3) . . ?
O2 C21 C22 119.8(3) . . ?
O2 C21 C26 118.3(3) . . ?
C22 C21 C26 121.6(3) . . ?
C23 C22 C21 118.4(3) . . ?
C23 C22 C2 120.7(3) . . ?
C21 C22 C2 120.8(3) . . ?
C24 C23 C22 119.8(3) . . ?
C24 C23 H23A 120.1 . . ?
C22 C23 H23A 120.1 . . ?
C23 C24 C25 122.0(3) . . ?
C23 C24 Br2 119.5(2) . . ?
C25 C24 Br2 118.6(2) . . ?
C24 C25 C26 119.3(3) . . ?
C24 C25 H25A 120.4 . . ?
C26 C25 H25A 120.4 . . ?
C25 C26 C21 118.9(3) . . ?
C25 C26 C1 121.0(3) . . ?
C21 C26 C1 120.0(3) . . ?
O2 C20 C27 106.6(3) . . ?
O2 C20 H20A 110.4 . . ?
C27 C20 H20A 110.4 . . ?
O2 C20 H20B 110.4 . . ?
C27 C20 H20B 110.4 . . ?
H20A C20 H20B 108.6 . . ?
C20 C27 C28 110.9(4) . . ?
C20 C27 H27A 109.5 . . ?
C28 C27 H27A 109.5 . . ?
C20 C27 H27B 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
C29 C28 C27 113.7(5) . . ?
C29 C28 H28A 108.8 . . ?
C27 C28 H28A 108.8 . . ?
C29 C28 H28B 108.8 . . ?
C27 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
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 . . ?
C22 C2 C36 115.9(3) . . ?
C22 C2 H2A 108.3 . . ?
C36 C2 H2A 108.3 . . ?
C22 C2 H2B 108.3 . . ?
C36 C2 H2B 108.3 . . ?
H2A C2 H2B 107.4 . . ?
C31 O3 C30' 114.0(5) . . ?
C31 O3 C30 117.3(5) . . ?
O3 C31 C32 118.6(3) . . ?
O3 C31 C36 120.1(3) . . ?
C32 C31 C36 121.2(3) . . ?
C33 C32 C31 118.9(3) . . ?
C33 C32 C3 120.9(3) . . ?
C31 C32 C3 120.1(3) . . ?
C34 C33 C32 120.0(3) . . ?
C34 C33 H33A 120.0 . . ?
C32 C33 H33A 120.0 . . ?
C33 C34 C35 121.4(3) . . ?
C33 C34 Br3 119.3(3) . . ?
C35 C34 Br3 119.3(2) . . ?
C36 C35 C34 119.8(3) . . ?
C36 C35 H35A 120.1 . . ?
C34 C35 H35A 120.1 . . ?
C35 C36 C31 118.7(3) . . ?
C35 C36 C2 122.4(3) . . ?
C31 C36 C2 118.9(3) . . ?
O3 C30 C37 107.7(8) . . ?
O3 C30 H30A 110.2 . . ?
C37 C30 H30A 110.2 . . ?
O3 C30 H30B 110.2 . . ?
C37 C30 H30B 110.2 . . ?
H30A C30 H30B 108.5 . . ?
C38 C37 C30 114.6(10) . . ?
C38 C37 H37A 108.6 . . ?
C30 C37 H37A 108.6 . . ?
C38 C37 H37B 108.6 . . ?
C30 C37 H37B 108.6 . . ?
H37A C37 H37B 107.6 . . ?
C37 C38 C39 110.3(10) . . ?
C37 C38 H38A 109.6 . . ?
C39 C38 H38A 109.6 . . ?
C37 C38 H38B 109.6 . . ?
C39 C38 H38B 109.6 . . ?
H38A C38 H38B 108.1 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O3 C30' C37' 107.6(9) . . ?
O3 C30' H30C 110.2 . . ?
C37' C30' H30C 110.2 . . ?
O3 C30' H30D 110.2 . . ?
C37' C30' H30D 110.2 . . ?
H30C C30' H30D 108.5 . . ?
C30' C37' C38' 114.6(14) . . ?
C30' C37' H37C 108.6 . . ?
C38' C37' H37C 108.6 . . ?
C30' C37' H37D 108.6 . . ?
C38' C37' H37D 108.6 . . ?
H37C C37' H37D 107.6 . . ?
C37' C38' C39' 112.1(9) . . ?
C37' C38' H38C 109.2 . . ?
C39' C38' H38C 109.2 . . ?
C37' C38' H38D 109.2 . . ?
C39' C38' H38D 109.2 . . ?
H38C C38' H38D 107.9 . . ?
C38' C39' H39D 109.5 . . ?
C38' C39' H39E 109.5 . . ?
H39D C39' H39E 109.5 . . ?
C38' C39' H39F 109.5 . . ?
H39D C39' H39F 109.5 . . ?
H39E C39' H39F 109.5 . . ?
C16 C3 C32 112.9(2) 2 . ?
C16 C3 H3A 109.0 2 . ?
C32 C3 H3A 109.0 . . ?
C16 C3 H3B 109.0 2 . ?
C32 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C2A C1A C6A 117.9(4) . . ?
C2A C1A C11A 121.1(5) . . ?
C6A C1A C11A 121.0(5) . . ?
C3A C2A C1A 122.0(5) . . ?
C3A C2A H2AA 119.0 . . ?
C1A C2A H2AA 119.0 . . ?
C4A C3A C2A 119.3(5) . . ?
C4A C3A C13A 120.8(6) . . ?
C2A C3A C13A 120.0(7) . . ?
C3A C4A C5A 121.2(6) . . ?
C3A C4A H4AA 119.4 . . ?
C5A C4A H4AA 119.4 . . ?
C4A C5A C6A 120.9(6) . . ?
C4A C5A H5AA 119.6 . . ?
C6A C5A H5AA 119.6 . . ?
C5A C6A C1A 118.7(5) . . ?
C5A C6A H6AA 120.7 . . ?
C1A C6A H6AA 120.7 . . ?
C1A C11A H11A 109.5 . . ?
C1A C11A H11B 109.5 . . ?
H11A C11A H11B 109.5 . . ?
C1A C11A H11C 109.5 . . ?
H11A C11A H11C 109.5 . . ?
H11B C11A H11C 109.5 . . ?
C3A C13A H13A 109.5 . . ?
C3A C13A H13B 109.5 . . ?
H13A C13A H13B 109.5 . . ?
C3A C13A H13C 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 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
C10 O1 C11 C16 -101.5(8) . . . . ?
C10' O1 C11 C16 -106.2(17) . . . . ?
C10 O1 C11 C12 82.8(8) . . . . ?
C10' O1 C11 C12 78.1(17) . . . . ?
O1 C11 C12 C13 176.9(3) . . . . ?
C16 C11 C12 C13 1.3(4) . . . . ?
O1 C11 C12 C1 -2.1(4) . . . . ?
C16 C11 C12 C1 -177.7(3) . . . . ?
C11 C12 C13 C14 -0.2(5) . . . . ?
C1 C12 C13 C14 178.8(3) . . . . ?
C12 C13 C14 C15 -1.2(5) . . . . ?
C12 C13 C14 Br1 177.5(2) . . . . ?
C13 C14 C15 C16 1.4(5) . . . . ?
Br1 C14 C15 C16 -177.3(2) . . . . ?
C14 C15 C16 C11 -0.2(5) . . . . ?
C14 C15 C16 C3 -179.7(3) . . . 2 ?
O1 C11 C16 C15 -176.8(3) . . . . ?
C12 C11 C16 C15 -1.1(4) . . . . ?
O1 C11 C16 C3 2.7(4) . . . 2 ?
C12 C11 C16 C3 178.3(3) . . . 2 ?
C11 O1 C10 C17 -178.7(6) . . . . ?
O1 C10 C17 C18 71.2(10) . . . . ?
C10 C17 C18 C19 73.2(7) . . . . ?
C11 O1 C10' C17' -147.6(18) . . . . ?
O1 C10' C17' C18' -61(3) . . . . ?
C10' C17' C18' C19' 86.4(16) . . . . ?
C13 C12 C1 C26 -37.3(4) . . . . ?
C11 C12 C1 C26 141.7(3) . . . . ?
C20 O2 C21 C22 -86.3(4) . . . . ?
C20 O2 C21 C26 99.7(3) . . . . ?
O2 C21 C22 C23 -175.2(3) . . . . ?
C26 C21 C22 C23 -1.4(5) . . . . ?
O2 C21 C22 C2 0.7(5) . . . . ?
C26 C21 C22 C2 174.5(3) . . . . ?
C21 C22 C23 C24 1.1(5) . . . . ?
C2 C22 C23 C24 -174.8(3) . . . . ?
C22 C23 C24 C25 -0.2(5) . . . . ?
C22 C23 C24 Br2 179.1(3) . . . . ?
C23 C24 C25 C26 -0.4(5) . . . . ?
Br2 C24 C25 C26 -179.7(3) . . . . ?
C24 C25 C26 C21 0.1(5) . . . . ?
C24 C25 C26 C1 179.8(3) . . . . ?
O2 C21 C26 C25 174.7(3) . . . . ?
C22 C21 C26 C25 0.8(5) . . . . ?
O2 C21 C26 C1 -5.0(5) . . . . ?
C22 C21 C26 C1 -178.9(3) . . . . ?
C12 C1 C26 C25 94.9(4) . . . . ?
C12 C1 C26 C21 -85.4(4) . . . . ?
C21 O2 C20 C27 -176.9(3) . . . . ?
O2 C20 C27 C28 -67.4(5) . . . . ?
C20 C27 C28 C29 178.6(6) . . . . ?
C23 C22 C2 C36 -84.5(4) . . . . ?
C21 C22 C2 C36 99.7(4) . . . . ?
C30' O3 C31 C32 100.4(10) . . . . ?
C30 O3 C31 C32 103.7(11) . . . . ?
C30' O3 C31 C36 -83.4(10) . . . . ?
C30 O3 C31 C36 -80.1(11) . . . . ?
O3 C31 C32 C33 175.9(3) . . . . ?
C36 C31 C32 C33 -0.2(5) . . . . ?
O3 C31 C32 C3 -3.9(4) . . . . ?
C36 C31 C32 C3 180.0(3) . . . . ?
C31 C32 C33 C34 0.2(5) . . . . ?
C3 C32 C33 C34 -180.0(3) . . . . ?
C32 C33 C34 C35 -0.5(5) . . . . ?
C32 C33 C34 Br3 -179.2(2) . . . . ?
C33 C34 C35 C36 0.7(5) . . . . ?
Br3 C34 C35 C36 179.4(2) . . . . ?
C34 C35 C36 C31 -0.7(5) . . . . ?
C34 C35 C36 C2 177.9(3) . . . . ?
O3 C31 C36 C35 -175.6(3) . . . . ?
C32 C31 C36 C35 0.5(5) . . . . ?
O3 C31 C36 C2 5.7(4) . . . . ?
C32 C31 C36 C2 -178.2(3) . . . . ?
C22 C2 C36 C35 21.4(5) . . . . ?
C22 C2 C36 C31 -160.0(3) . . . . ?
C31 O3 C30 C37 -166.9(8) . . . . ?
O3 C30 C37 C38 -54(2) . . . . ?
C30 C37 C38 C39 171.1(16) . . . . ?
C31 O3 C30' C37' 146.5(9) . . . . ?
O3 C30' C37' C38' 56.8(17) . . . . ?
C30' C37' C38' C39' 69(2) . . . . ?
C33 C32 C3 C16 -99.8(4) . . . 2 ?
C31 C32 C3 C16 80.0(4) . . . 2 ?
C6A C1A C2A C3A 1.7(6) . . . . ?
C11A C1A C2A C3A -179.2(4) . . . . ?
C1A C2A C3A C4A -2.1(7) . . . . ?
C1A C2A C3A C13A 176.7(5) . . . . ?
C2A C3A C4A C5A 0.8(9) . . . . ?
C13A C3A C4A C5A -178.0(6) . . . . ?
C3A C4A C5A C6A 0.8(10) . . . . ?
C4A C5A C6A C1A -1.2(9) . . . . ?
C2A C1A C6A C5A 0.0(7) . . . . ?
C11A C1A C6A C5A -179.1(5) . . . . ?

_refine_diff_density_max         1.416
_refine_diff_density_min         -1.564
_refine_diff_density_rms         0.115

####################################################################### 
# 
# 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_iy090622
_database_code_depnum_ccdc_archive 'CCDC 2441443'
loop_
_audit_author_name
_audit_author_address
'Alexandre Sobolev'
;The University of Western Australia
Australia
;
_audit_update_record             
;
2025-04-07 deposited with the CCDC.	2025-10-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/2
_shelx_SHELXL_version_number     2019/2
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C40 H49 Na O17 P4, Na4 H26 O13, 10(H2 O) [+ solvent]'
_chemical_formula_sum            'C40 H95 Na5 O40 P4 [+ solvent]'
_chemical_formula_weight         1454.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_H-M_alt        'I m m m'
_space_group_name_Hall           '-I 2 2'

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

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

_cell_length_a                   14.5981(4)
_cell_length_b                   22.6256(5)
_cell_length_c                   29.1419(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9625.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6329
_cell_measurement_theta_min      3.340
_cell_measurement_theta_max      66.485
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0770988
_diffrn_orient_matrix_UB_12      -0.0276378
_diffrn_orient_matrix_UB_13      -0.0290057
_diffrn_orient_matrix_UB_21      -0.0332573
_diffrn_orient_matrix_UB_22      0.0621939
_diffrn_orient_matrix_UB_23      -0.0135981
_diffrn_orient_matrix_UB_31      0.0639506
_diffrn_orient_matrix_UB_32      -0.0010042
_diffrn_orient_matrix_UB_33      -0.0420666

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.004
_exptl_crystal_F_000             3080
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.539
_shelx_estimated_absorpt_T_min   0.585
_shelx_estimated_absorpt_T_max   0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.35692
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Ruby
_diffrn_detector_area_resol_mean 10.4738
_diffrn_reflns_number            36792
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.386
_diffrn_reflns_theta_max         67.327
_diffrn_reflns_theta_full        67.327
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             4643
_reflns_number_gt                2821
_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       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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)+(0.0500P)²+120.0000P] 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         4643
_refine_ls_number_parameters     288
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.2224
_refine_ls_R_factor_gt           0.1687
_refine_ls_wR_factor_ref         0.3704
_refine_ls_wR_factor_gt          0.3431
_refine_ls_goodness_of_fit_ref   1.337
_refine_ls_restrained_S_all      1.367
_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 0.3433(5) 0.500000 0.2048(2) 0.059(2) Uani 1 2 d DS T P . .
C10 C 0.3263(7) 0.3866(4) 0.2497(3) 0.064(2) Uani 1 1 d . . . . .
H10A H 0.320711 0.355160 0.273090 0.077 Uiso 1 1 calc R U . . .
H10B H 0.276688 0.380475 0.226994 0.077 Uiso 1 1 calc R U . . .
C11 C 0.3208(9) 0.500000 0.2511(3) 0.054(3) Uani 1 2 d S T P B .
C12 C 0.3106(6) 0.4462(3) 0.2731(3) 0.060(2) Uani 1 1 d . . . . .
C13 C 0.2881(7) 0.4477(4) 0.3200(3) 0.065(2) Uani 1 1 d . . . . .
H13 H 0.281184 0.411392 0.336019 0.078 Uiso 1 1 calc R U . . .
C14 C 0.2757(9) 0.500000 0.3437(4) 0.062(3) Uani 1 2 d S T P . .
P1 P 0.2506(4) 0.500000 0.40509(13) 0.0938(15) Uani 1 2 d DS TU P . .
O11 O 0.3507(8) 0.500000 0.4337(4) 0.109(4) Uani 1 2 d DS T P . .
H11 H 0.340425 0.500000 0.462109 0.163 Uiso 1 2 calc R U P . .
O12 O 0.2143(6) 0.4437(3) 0.4178(2) 0.096(3) Uani 1 1 d D . . . .
O2 O 0.500000 0.3959(3) 0.2958(2) 0.069(2) Uani 1 2 d DS T P . .
C21 C 0.500000 0.3839(5) 0.2477(4) 0.056(3) Uani 1 2 d S T P C .
C22 C 0.4157(6) 0.3792(3) 0.2258(3) 0.056(2) Uani 1 1 d . . . . .
C23 C 0.4180(7) 0.3656(3) 0.1792(3) 0.062(2) Uani 1 1 d . . . . .
H23 H 0.361983 0.361410 0.162964 0.074 Uiso 1 1 calc R U . . .
C24 C 0.500000 0.3579(5) 0.1560(4) 0.057(3) Uani 1 2 d S T P A .
P2 P 0.500000 0.34458(15) 0.09340(11) 0.0655(9) Uani 1 2 d DS T P . .
O21 O 0.3930(8) 0.3302(7) 0.0804(4) 0.084(4) Uani 0.5 1 d D . P A -1
H21 H 0.389620 0.320040 0.052691 0.125 Uiso 0.5 1 calc R U P A -1
O22 O 0.5590(9) 0.2946(5) 0.0859(4) 0.070(3) Uani 0.5 1 d D . P A -1
O23 O 0.5307(9) 0.3988(4) 0.0715(4) 0.081(6) Uani 0.5 1 d D . P A -1
C1 C 0.2729(8) 0.5180(6) 0.1719(5) 0.061(6) Uani 0.5 1 d D . P B -1
H1A H 0.301470 0.526362 0.141792 0.074 Uiso 0.5 1 calc R U P B -1
H1B H 0.242307 0.554409 0.182769 0.074 Uiso 0.5 1 calc R U P B -1
C2 C 0.2045(11) 0.4696(7) 0.1671(8) 0.112(9) Uani 0.5 1 d D . P B -1
H2A H 0.174393 0.462497 0.197001 0.135 Uiso 0.5 1 calc R U P B -1
H2B H 0.235954 0.432746 0.157766 0.135 Uiso 0.5 1 calc R U P B -1
C3 C 0.1316(11) 0.4857(9) 0.1310(7) 0.100(9) Uani 0.5 1 d D . P B -1
H3A H 0.087317 0.453368 0.128353 0.150 Uiso 0.5 1 calc R U P B -1
H3B H 0.099855 0.521884 0.140456 0.150 Uiso 0.5 1 calc R U P B -1
H3C H 0.161333 0.492174 0.101274 0.150 Uiso 0.5 1 calc R U P B -1
C4 C 0.5201(14) 0.3426(6) 0.3229(5) 0.079(6) Uani 0.5 1 d D U P C -1
H4A H 0.586900 0.338932 0.328196 0.094 Uiso 0.5 1 calc R U P C -1
H4B H 0.498486 0.306847 0.306666 0.094 Uiso 0.5 1 calc R U P C -1
C5 C 0.471(3) 0.3497(11) 0.3676(7) 0.205(19) Uani 0.5 1 d D U P C -1
H5A H 0.406060 0.360508 0.361592 0.246 Uiso 0.5 1 calc R U P C -1
H5B H 0.499115 0.382100 0.385408 0.246 Uiso 0.5 1 calc R U P C -1
C6 C 0.474(3) 0.2926(11) 0.3958(8) 0.197(18) Uani 0.5 1 d D U P C -1
H6A H 0.440809 0.298557 0.424803 0.296 Uiso 0.5 1 calc R U P C -1
H6B H 0.444555 0.260624 0.378491 0.296 Uiso 0.5 1 calc R U P C -1
H6C H 0.537527 0.282196 0.402286 0.296 Uiso 0.5 1 calc R U P C -1
Na1 Na 0.500000 0.500000 0.1880(3) 0.090(3) Uani 1 4 d S T P B .
Na2 Na 0.3579(6) 0.3234(3) 0.500000 0.107(2) Uani 1 2 d S T P . .
Na3 Na 0.1209(4) 0.3261(2) 0.500000 0.0814(16) Uani 1 2 d S T P . .
O01 O 0.500000 0.500000 0.1159(5) 0.092(4) Uiso 1 4 d S . P . .
H01 H 0.500000 0.500000 0.083320 0.111 Uiso 1 4 calc R U P B .
O01W O 0.2510(6) 0.3330(3) 0.4418(2) 0.093(2) Uani 1 1 d . . . . .
O02W O 0.3996(8) 0.4241(5) 0.500000 0.097(3) Uani 1 2 d S T P . .
O03W O 0.1411(8) 0.2231(5) 0.500000 0.091(3) Uani 1 2 d S T P . .
O04W O 0.000000 0.3178(4) 0.4434(3) 0.082(3) Uani 1 2 d S T P . .
O05W O 0.1342(6) 0.4238(4) 0.500000 0.093(3) Uani 1 2 d DS T P . .
O06W O 0.3303(12) 0.2192(8) 0.500000 0.070(5) Uiso 0.5 2 d S . P . .
O07W O 0.000000 0.4107(17) 0.6140(13) 0.079(10) Uiso 0.25 2 d S . P . .
O08W O 0.000000 0.500000 0.500000 0.047(3) Uiso 1 8 d DS . P . .
O09W O 0.2644(12) 0.2668(6) 0.1169(5) 0.078(4) Uani 0.5 1 d . . P D 1
O10W O 0.3083(17) 0.2375(11) 0.1282(8) 0.141(8) Uani 0.5 1 d . U P E 2
O11W O 0.2992(10) 0.4320(7) 0.0505(4) 0.093(4) Uani 0.5 1 d . U P . .
O12W O 0.6547(13) 0.1510(7) 0.5786(6) 0.110(5) Uani 0.5 1 d . U P . .
O13W O 0.2805(18) 0.2421(11) 0.2912(9) 0.076(7) Uiso 0.25 1 d . . 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
O1 C11 1.388(12) . ?
O1 C1 1.462(8) . ?
O1 Na1 2.340(8) . ?
C10 C22 1.490(12) . ?
C10 C12 1.528(11) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.385(9) . ?
C11 C12 1.385(9) 11_565 ?
C12 C13 1.405(11) . ?
C13 C14 1.382(10) . ?
C13 H13 0.9500 . ?
C14 P1 1.826(12) . ?
P1 O12 1.428(6) . ?
P1 O12 1.428(6) 11_565 ?
P1 O11 1.683(11) . ?
O11 H11 0.8400 . ?
O2 C21 1.427(12) . ?
O2 C4 1.472(9) . ?
C21 C22 1.391(10) 12_655 ?
C21 C22 1.391(10) . ?
C22 C23 1.391(10) . ?
C23 C24 1.386(10) . ?
C23 H23 0.9500 . ?
C24 P2 1.848(11) . ?
P2 O22 1.437(8) . ?
P2 O23 1.455(8) . ?
P2 O21 1.640(11) . ?
O21 H21 0.8400 . ?
C1 C2 1.489(9) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.539(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.498(10) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.531(10) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
Na1 O01 2.100(18) . ?
Na2 O01W 2.315(9) . ?
Na2 O01W 2.316(9) 10_556 ?
Na2 O02W 2.359(13) . ?
Na2 O06W 2.392(19) . ?
Na2 Na3 3.461(10) . ?
Na2 Na2 4.147(16) 3_656 ?
Na3 O05W 2.218(11) . ?
Na3 O03W 2.350(12) . ?
Na3 O04W 2.423(8) 10_556 ?
Na3 O04W 2.423(8) . ?
Na3 O01W 2.551(9) . ?
Na3 O01W 2.552(9) 10_556 ?
Na3 Na3 3.530(12) 3_556 ?
O01 H01 0.9500 . ?

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 C1 118.1(10) . . ?
C11 O1 Na1 115.8(7) . . ?
C1 O1 Na1 123.3(7) . . ?
C22 C10 C12 116.2(7) . . ?
C22 C10 H10A 108.2 . . ?
C12 C10 H10A 108.2 . . ?
C22 C10 H10B 108.2 . . ?
C12 C10 H10B 108.2 . . ?
H10A C10 H10B 107.4 . . ?
C12 C11 C12 123.1(10) . 11_565 ?
C12 C11 O1 118.5(5) . . ?
C12 C11 O1 118.5(5) 11_565 . ?
C11 C12 C13 117.1(8) . . ?
C11 C12 C10 123.4(7) . . ?
C13 C12 C10 119.5(7) . . ?
C14 C13 C12 122.5(8) . . ?
C14 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?
C13 C14 C13 117.8(11) . 11_565 ?
C13 C14 P1 121.0(5) . . ?
C13 C14 P1 121.0(5) 11_565 . ?
O12 P1 O12 126.2(7) . 11_565 ?
O12 P1 O11 101.2(4) . . ?
O12 P1 O11 101.2(4) 11_565 . ?
O12 P1 C14 109.2(3) . . ?
O12 P1 C14 109.2(3) 11_565 . ?
O11 P1 C14 108.2(6) . . ?
P1 O11 H11 109.5 . . ?
C21 O2 C4 111.8(9) . . ?
C22 C21 C22 124.3(10) 12_655 . ?
C22 C21 O2 117.8(5) 12_655 . ?
C22 C21 O2 117.8(5) . . ?
C21 C22 C23 116.4(9) . . ?
C21 C22 C10 123.4(7) . . ?
C23 C22 C10 120.1(8) . . ?
C24 C23 C22 121.7(9) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C23 C24 C23 119.4(10) 12_655 . ?
C23 C24 P2 120.2(5) 12_655 . ?
C23 C24 P2 120.2(5) . . ?
O22 P2 O23 114.3(8) . . ?
O22 P2 O21 112.3(9) . . ?
O23 P2 O21 111.0(8) . . ?
O22 P2 C24 106.2(6) . . ?
O23 P2 C24 107.2(6) . . ?
O21 P2 C24 105.1(4) . . ?
P2 O21 H21 109.5 . . ?
O1 C1 C2 109.2(8) . . ?
O1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
O1 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.3 . . ?
C1 C2 C3 110.8(9) . . ?
C1 C2 H2A 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O2 C4 C5 106.5(9) . . ?
O2 C4 H4A 110.4 . . ?
C5 C4 H4A 110.4 . . ?
O2 C4 H4B 110.4 . . ?
C5 C4 H4B 110.4 . . ?
H4A C4 H4B 108.6 . . ?
C4 C5 C6 111.3(10) . . ?
C4 C5 H5A 109.4 . . ?
C6 C5 H5A 109.4 . . ?
C4 C5 H5B 109.4 . . ?
C6 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O01 Na1 O1 102.1(3) . . ?
O01 Na1 O1 102.1(3) . 2_665 ?
O1 Na1 O1 155.8(5) . 2_665 ?
O01W Na2 O01W 94.2(5) . 10_556 ?
O01W Na2 O02W 94.7(3) . . ?
O01W Na2 O02W 94.7(3) 10_556 . ?
O01W Na2 O06W 88.8(4) . . ?
O01W Na2 O06W 88.8(4) 10_556 . ?
O02W Na2 O06W 174.8(7) . . ?
O01W Na2 Na3 47.5(2) . . ?
O01W Na2 Na3 47.5(2) 10_556 . ?
O02W Na2 Na3 103.9(4) . . ?
O06W Na2 Na3 81.3(5) . . ?
O01W Na2 Na2 132.4(2) . 3_656 ?
O01W Na2 Na2 132.4(2) 10_556 3_656 ?
O02W Na2 Na2 75.1(4) . 3_656 ?
O06W Na2 Na2 99.7(5) . 3_656 ?
Na3 Na2 Na2 178.97(15) . 3_656 ?
O05W Na3 O03W 167.8(5) . . ?
O05W Na3 O04W 98.1(3) . 10_556 ?
O03W Na3 O04W 90.8(3) . 10_556 ?
O05W Na3 O04W 98.1(3) . . ?
O03W Na3 O04W 90.8(3) . . ?
O04W Na3 O04W 85.8(4) 10_556 . ?
O05W Na3 O01W 82.8(3) . . ?
O03W Na3 O01W 88.1(3) . . ?
O04W Na3 O01W 178.4(4) 10_556 . ?
O04W Na3 O01W 95.4(2) . . ?
O05W Na3 O01W 82.8(3) . 10_556 ?
O03W Na3 O01W 88.1(3) . 10_556 ?
O04W Na3 O01W 95.4(2) 10_556 10_556 ?
O04W Na3 O01W 178.4(4) . 10_556 ?
O01W Na3 O01W 83.3(4) . 10_556 ?
O05W Na3 Na2 86.0(3) . . ?
O03W Na3 Na2 81.7(4) . . ?
O04W Na3 Na2 136.64(19) 10_556 . ?
O04W Na3 Na2 136.64(19) . . ?
O01W Na3 Na2 41.99(19) . . ?
O01W Na3 Na2 41.99(19) 10_556 . ?
O05W Na3 Na3 95.0(3) . 3_556 ?
O03W Na3 Na3 97.2(3) . 3_556 ?
O04W Na3 Na3 43.23(19) 10_556 3_556 ?
O04W Na3 Na3 43.23(19) . 3_556 ?
O01W Na3 Na3 138.11(19) . 3_556 ?
O01W Na3 Na3 138.11(19) 10_556 3_556 ?
Na2 Na3 Na3 178.97(15) . 3_556 ?
Na1 O01 H01 180.0 . . ?
Na2 O01W Na3 90.5(3) . . ?
Na3 O04W Na3 93.5(4) 3_556 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 O1 C11 C12 108.7(11) . . . . ?
Na1 O1 C11 C12 -89.7(10) . . . . ?
C1 O1 C11 C12 -71.9(12) . . . 11_565 ?
Na1 O1 C11 C12 89.7(10) . . . 11_565 ?
C12 C11 C12 C13 0.4(19) 11_565 . . . ?
O1 C11 C12 C13 179.8(9) . . . . ?
C12 C11 C12 C10 -176.9(8) 11_565 . . . ?
O1 C11 C12 C10 2.5(16) . . . . ?
C22 C10 C12 C11 52.6(13) . . . . ?
C22 C10 C12 C13 -124.7(9) . . . . ?
C11 C12 C13 C14 0.5(16) . . . . ?
C10 C12 C13 C14 178.0(10) . . . . ?
C12 C13 C14 C13 -1(2) . . . 11_565 ?
C12 C13 C14 P1 -177.8(9) . . . . ?
C13 C14 P1 O12 -21.1(13) . . . . ?
C13 C14 P1 O12 162.6(10) 11_565 . . . ?
C13 C14 P1 O12 -162.6(10) . . . 11_565 ?
C13 C14 P1 O12 21.1(13) 11_565 . . 11_565 ?
C13 C14 P1 O11 88.1(11) . . . . ?
C13 C14 P1 O11 -88.1(11) 11_565 . . . ?
C4 O2 C21 C22 -78.4(13) . . . 12_655 ?
C4 O2 C21 C22 103.2(12) . . . . ?
C22 C21 C22 C23 3.7(16) 12_655 . . . ?
O2 C21 C22 C23 -178.0(8) . . . . ?
C22 C21 C22 C10 -177.6(7) 12_655 . . . ?
O2 C21 C22 C10 0.7(14) . . . . ?
C12 C10 C22 C21 59.1(12) . . . . ?
C12 C10 C22 C23 -122.2(8) . . . . ?
C21 C22 C23 C24 -0.8(12) . . . . ?
C10 C22 C23 C24 -179.6(8) . . . . ?
C22 C23 C24 C23 -1.8(16) . . . 12_655 ?
C22 C23 C24 P2 -176.1(6) . . . . ?
C23 C24 P2 O22 54.3(11) 12_655 . . . ?
C23 C24 P2 O22 -131.5(10) . . . . ?
C23 C24 P2 O23 -68.3(11) 12_655 . . . ?
C23 C24 P2 O23 105.9(10) . . . . ?
C23 C24 P2 O21 173.5(10) 12_655 . . . ?
C23 C24 P2 O21 -12.2(11) . . . . ?
C11 O1 C1 C2 -74.6(16) . . . . ?
Na1 O1 C1 C2 125.3(13) . . . . ?
O1 C1 C2 C3 -177.4(16) . . . . ?
C21 O2 C4 C5 -150(2) . . . . ?
O2 C4 C5 C6 171(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O11 H11 O02W 0.84 2.22 2.681(12) 114.9 . yes
O11 H11 O02W 0.84 2.22 2.681(12) 114.9 11_565 yes
C23 H23 O21^a 0.95 2.55 3.012(14) 110.2 . yes
O21^a H21^a O03W 0.84 1.87 2.681(12) 160.7 13 yes

_refine_diff_density_max         1.772
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.138



