# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_tius005
_database_code_depnum_ccdc_archive 'CCDC 2154234'
loop_
_audit_author_name
_audit_author_address
'Glenn P. A. Yap'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-02-23 deposited with the CCDC.	2023-05-29 downloaded from the CCDC.
;
_audit_creation_date             2022-02-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C61 H55 F N3 O4 Rh, 1[CH3COOC2H5]'
_chemical_formula_sum            'C65 H63 F N3 O6 Rh'
_chemical_formula_weight         1104.09
_chemical_absolute_configuration ad
_chemical_melting_point          ?
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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   28.8510(17)
_cell_length_b                   15.3005(9)
_cell_length_c                   12.0037(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.747(2)
_cell_angle_gamma                90
_cell_volume                     5262.2(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9811
_cell_measurement_temperature    100
_cell_measurement_theta_max      65.12
_cell_measurement_theta_min      3.08
_shelx_estimated_absorpt_T_max   0.961
_shelx_estimated_absorpt_T_min   0.684
_exptl_absorpt_coefficient_mu    3.119
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1054 before and 0.0637 after correction.
The Ratio of minimum to maximum transmission is 0.7550.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2304
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2.00 -2.00 -3.00 0.0220
-1.00 0.00 0.00 0.0040
-1.00 -2.00 -2.00 0.0200
-1.00 -2.00 0.00 0.0330
1.00 2.00 2.00 0.0300
1.00 0.00 0.00 0.0060
1.00 0.00 3.00 0.0370
2.00 2.00 1.00 0.0310
2.00 1.00 -3.00 0.0400
2.00 -2.00 1.00 0.0450
2.00 0.00 -1.00 0.0230
3.00 -2.00 -1.00 0.0120
3.00 0.00 1.00 0.0260

_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.013
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            29351
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        65.166
_diffrn_reflns_theta_max         65.166
_diffrn_reflns_theta_min         3.085
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Venture Photon III'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                8278
_reflns_number_total             8808
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 
;
 Flack x determined using 3546 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         8808
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0506
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0765P)²+21.9719P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1340
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Y: Rh1(0.61356)
3.a Ternary CH refined with riding coordinates:
 C9(H9), C31(H31), C33(H33), C36(H36), C54(H54), C56(H56), C59(H59)
3.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C30(H30A,H30B), C32(H32A,H32B), C34(H34A,H34B), C35(H35A,H35B),
 C37(H37A,H37B), C38(H38A,H38B), C53(H53A,H53B), C55(H55A,H55B), C57(H57A,H57B),
  C58(H58A,H58B), C60(H60A,H60B), C61(H61A,H61B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C25(H25), C27(H27), C40(H40),
  C41(H41), C42(H42), C43(H43), C47(H47), C48(H48), C50(H50)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Rh1 Rh 0.30654(2) 0.613560 0.27030(3) 0.01786(16) Uani 1 1 d . . . . .
F1 F 0.42462(16) 0.5909(3) 0.6711(3) 0.0328(13) Uani 1 1 d . . . . .
O1 O 0.3016(2) 0.5101(4) 0.3863(5) 0.0217(14) Uani 1 1 d . . . . .
O2 O 0.44102(19) 0.5829(4) 0.4660(4) 0.0272(13) Uani 1 1 d . . . . .
O3 O 0.3109(2) 0.5172(4) -0.0443(5) 0.0251(14) Uani 1 1 d . . . . .
O4 O 0.22891(19) 0.7722(4) 0.4511(4) 0.0247(12) Uani 1 1 d . . . . .
N1 N 0.37960(19) 0.6064(6) 0.3365(4) 0.0206(13) Uani 1 1 d . . . . .
N2 N 0.3138(3) 0.5334(5) 0.1401(6) 0.0205(17) Uani 1 1 d . . . . .
N3 N 0.2884(3) 0.7034(5) 0.3838(6) 0.0206(16) Uani 1 1 d . . . . .
C1 C 0.3190(3) 0.5193(5) 0.4904(6) 0.0212(16) Uani 1 1 d . . . . .
C2 C 0.2921(3) 0.4961(6) 0.5771(7) 0.0281(19) Uani 1 1 d . . . . .
H2 H 0.261436 0.474203 0.558035 0.034 Uiso 1 1 calc R U . . .
C3 C 0.3094(3) 0.5046(6) 0.6882(7) 0.0307(19) Uani 1 1 d . . . . .
H3 H 0.290338 0.488576 0.744291 0.037 Uiso 1 1 calc R U . . .
C4 C 0.3543(3) 0.5361(6) 0.7204(7) 0.035(2) Uani 1 1 d . . . . .
H4 H 0.366024 0.541528 0.797418 0.042 Uiso 1 1 calc R U . . .
C5 C 0.3810(3) 0.5590(5) 0.6382(6) 0.0271(18) Uani 1 1 d . . . . .
C6 C 0.3658(3) 0.5526(5) 0.5225(6) 0.0213(16) Uani 1 1 d . . . . .
C7 C 0.3936(3) 0.5816(5) 0.4366(6) 0.0215(16) Uani 1 1 d . . . . .
C8 C 0.4621(3) 0.6115(9) 0.3710(5) 0.0322(16) Uani 1 1 d . . . . .
H8A H 0.482229 0.565146 0.345108 0.039 Uiso 1 1 calc R U . . .
H8B H 0.481230 0.664405 0.389268 0.039 Uiso 1 1 calc R U . . .
C9 C 0.4208(3) 0.6320(5) 0.2798(6) 0.025(2) Uani 1 1 d . . . . .
H9 H 0.419747 0.696217 0.264538 0.030 Uiso 1 1 calc R U . . .
C10 C 0.4288(3) 0.6280(8) 0.0730(6) 0.036(2) Uani 1 1 d . . . . .
H10 H 0.426545 0.689964 0.071595 0.043 Uiso 1 1 calc R U . . .
C11 C 0.4357(3) 0.5833(8) -0.0235(7) 0.050(3) Uani 1 1 d . . . . .
H11 H 0.438722 0.614673 -0.090595 0.060 Uiso 1 1 calc R U . . .
C12 C 0.4384(4) 0.4913(10) -0.0232(9) 0.056(3) Uani 1 1 d . . . . .
H12 H 0.443388 0.460479 -0.089469 0.067 Uiso 1 1 calc R U . . .
C13 C 0.4337(4) 0.4465(8) 0.0747(8) 0.047(3) Uani 1 1 d . . . . .
H13 H 0.434746 0.384445 0.075377 0.057 Uiso 1 1 calc R U . . .
C14 C 0.4275(3) 0.4922(7) 0.1732(8) 0.037(2) Uani 1 1 d . . . . .
H14 H 0.424969 0.461029 0.240661 0.045 Uiso 1 1 calc R U . . .
C15 C 0.4249(3) 0.5833(6) 0.1723(7) 0.032(2) Uani 1 1 d . . . . .
C16 C 0.3089(3) 0.7032(6) 0.1493(8) 0.021(2) Uani 1 1 d . . . . .
C17 C 0.3071(3) 0.7932(6) 0.1551(7) 0.0238(19) Uani 1 1 d . . . . .
H17 H 0.306914 0.820840 0.225938 0.029 Uiso 1 1 calc R U . . .
C18 C 0.3056(3) 0.8445(6) 0.0580(7) 0.0273(18) Uani 1 1 d . . . . .
H18 H 0.303991 0.906301 0.064403 0.033 Uiso 1 1 calc R U . . .
C19 C 0.3063(3) 0.8078(6) -0.0465(7) 0.0274(19) Uani 1 1 d . . . . .
H19 H 0.305569 0.844201 -0.110782 0.033 Uiso 1 1 calc R U . . .
C20 C 0.3080(3) 0.7166(7) -0.0582(7) 0.025(2) Uani 1 1 d . . . . .
H20 H 0.308177 0.690302 -0.129828 0.030 Uiso 1 1 calc R U . . .
C21 C 0.3094(3) 0.6660(6) 0.0385(8) 0.023(2) Uani 1 1 d . . . . .
C22 C 0.3111(3) 0.5725(6) 0.0448(7) 0.021(2) Uani 1 1 d . . . . .
C23 C 0.3136(3) 0.4332(5) 0.0038(6) 0.0212(17) Uani 1 1 d . . . . .
C24 C 0.3165(3) 0.3544(5) -0.0474(6) 0.0236(17) Uani 1 1 d . . . . .
H24 H 0.314046 0.348717 -0.126668 0.028 Uiso 1 1 calc R U . . .
C25 C 0.3232(3) 0.2828(6) 0.0235(7) 0.0289(19) Uani 1 1 d . . . . .
H25 H 0.324797 0.226371 -0.008889 0.035 Uiso 1 1 calc R U . . .
C26 C 0.3277(3) 0.2898(5) 0.1417(6) 0.0241(17) Uani 1 1 d . . . . .
C27 C 0.3235(3) 0.3717(5) 0.1905(6) 0.0226(17) Uani 1 1 d . . . . .
H27 H 0.325493 0.378654 0.269585 0.027 Uiso 1 1 calc R U . . .
C28 C 0.3163(3) 0.4420(6) 0.1189(6) 0.0198(18) Uani 1 1 d . . . . .
C29 C 0.3413(3) 0.2092(6) 0.2128(7) 0.0263(18) Uani 1 1 d . . . . .
C30 C 0.3057(3) 0.1355(5) 0.1883(7) 0.031(2) Uani 1 1 d . . . . .
H30A H 0.302151 0.121841 0.107099 0.037 Uiso 1 1 calc R U . . .
H30B H 0.275004 0.154719 0.208408 0.037 Uiso 1 1 calc R U . . .
C31 C 0.3217(3) 0.0525(6) 0.2562(8) 0.037(2) Uani 1 1 d . . . . .
H31 H 0.298208 0.004861 0.239301 0.044 Uiso 1 1 calc R U . . .
C32 C 0.3692(4) 0.0224(6) 0.2258(9) 0.038(2) Uani 1 1 d . . . . .
H32A H 0.366535 0.006689 0.145258 0.045 Uiso 1 1 calc R U . . .
H32B H 0.379466 -0.030250 0.270020 0.045 Uiso 1 1 calc R U . . .
C33 C 0.4056(3) 0.0954(5) 0.2501(8) 0.034(2) Uani 1 1 d . . . . .
H33 H 0.436429 0.075556 0.228803 0.041 Uiso 1 1 calc R U . . .
C34 C 0.3894(3) 0.1775(6) 0.1825(7) 0.0290(18) Uani 1 1 d . . . . .
H34A H 0.387003 0.164248 0.101315 0.035 Uiso 1 1 calc R U . . .
H34B H 0.412755 0.224651 0.198665 0.035 Uiso 1 1 calc R U . . .
C35 C 0.3265(4) 0.0742(7) 0.3819(8) 0.041(2) Uani 1 1 d . . . . .
H35A H 0.295989 0.093479 0.403290 0.049 Uiso 1 1 calc R U . . .
H35B H 0.336460 0.021549 0.426295 0.049 Uiso 1 1 calc R U . . .
C36 C 0.3627(4) 0.1470(6) 0.4065(7) 0.039(2) Uani 1 1 d . . . . .
H36 H 0.365724 0.161182 0.488361 0.047 Uiso 1 1 calc R U . . .
C37 C 0.4104(3) 0.1173(9) 0.3749(6) 0.0394(19) Uani 1 1 d . . . . .
H37A H 0.433688 0.164401 0.391687 0.047 Uiso 1 1 calc R U . . .
H37B H 0.421240 0.065124 0.419440 0.047 Uiso 1 1 calc R U . . .
C38 C 0.3467(4) 0.2289(6) 0.3391(7) 0.034(2) Uani 1 1 d . . . . .
H38A H 0.369811 0.276251 0.356157 0.041 Uiso 1 1 calc R U . . .
H38B H 0.316418 0.249141 0.361032 0.041 Uiso 1 1 calc R U . . .
C39 C 0.2371(2) 0.6139(8) 0.2272(5) 0.0235(13) Uani 1 1 d . . . . .
C40 C 0.2101(3) 0.5641(5) 0.1472(6) 0.0260(18) Uani 1 1 d . . . . .
H40 H 0.225071 0.523992 0.102656 0.031 Uiso 1 1 calc R U . . .
C41 C 0.1613(3) 0.5717(5) 0.1307(6) 0.0259(18) Uani 1 1 d . . . . .
H41 H 0.143864 0.535480 0.076817 0.031 Uiso 1 1 calc R U . . .
C42 C 0.1379(3) 0.6316(5) 0.1924(7) 0.029(2) Uani 1 1 d . . . . .
H42 H 0.104988 0.638757 0.178053 0.034 Uiso 1 1 calc R U . . .
C43 C 0.1642(3) 0.6809(6) 0.2760(6) 0.0263(18) Uani 1 1 d . . . . .
H43 H 0.149388 0.721148 0.320603 0.032 Uiso 1 1 calc R U . . .
C44 C 0.2127(3) 0.6698(5) 0.2925(6) 0.0260(18) Uani 1 1 d . . . . .
C45 C 0.2429(3) 0.7154(5) 0.3754(6) 0.0216(16) Uani 1 1 d . . . . .
C46 C 0.2701(3) 0.7989(5) 0.5138(6) 0.0257(17) Uani 1 1 d . . . . .
C47 C 0.2753(3) 0.8592(5) 0.6008(6) 0.0270(18) Uani 1 1 d . . . . .
H47 H 0.249388 0.887158 0.627822 0.032 Uiso 1 1 calc R U . . .
C48 C 0.3206(3) 0.8756(5) 0.6450(6) 0.0248(17) Uani 1 1 d . . . . .
H48 H 0.325909 0.916353 0.704853 0.030 Uiso 1 1 calc R U . . .
C49 C 0.3601(3) 0.8349(5) 0.6064(6) 0.0238(17) Uani 1 1 d . . . . .
C50 C 0.3533(3) 0.7758(5) 0.5181(6) 0.0209(16) Uani 1 1 d . . . . .
H50 H 0.378877 0.748066 0.489471 0.025 Uiso 1 1 calc R U . . .
C51 C 0.3079(3) 0.7588(5) 0.4735(6) 0.0206(16) Uani 1 1 d . . . . .
C52 C 0.4081(3) 0.8558(5) 0.6652(6) 0.0224(16) Uani 1 1 d . . . . .
C53 C 0.4117(3) 0.8280(6) 0.7897(6) 0.0274(18) Uani 1 1 d . . . . .
H53A H 0.386729 0.857443 0.825763 0.033 Uiso 1 1 calc R U . . .
H53B H 0.406671 0.764184 0.794095 0.033 Uiso 1 1 calc R U . . .
C54 C 0.4591(3) 0.8512(6) 0.8535(7) 0.032(2) Uani 1 1 d . . . . .
H54 H 0.460361 0.831614 0.933297 0.039 Uiso 1 1 calc R U . . .
C55 C 0.4983(3) 0.8062(6) 0.7974(7) 0.0322(19) Uani 1 1 d . . . . .
H55A H 0.529066 0.821966 0.837737 0.039 Uiso 1 1 calc R U . . .
H55B H 0.494702 0.741956 0.801072 0.039 Uiso 1 1 calc R U . . .
C56 C 0.4959(3) 0.8346(6) 0.6771(7) 0.0313(19) Uani 1 1 d . . . . .
H56 H 0.520940 0.804397 0.640929 0.038 Uiso 1 1 calc R U . . .
C57 C 0.4479(3) 0.8118(5) 0.6126(6) 0.0249(17) Uani 1 1 d . . . . .
H57A H 0.447073 0.831033 0.533633 0.030 Uiso 1 1 calc R U . . .
H57B H 0.443407 0.747690 0.612854 0.030 Uiso 1 1 calc R U . . .
C58 C 0.4665(4) 0.9492(7) 0.8494(7) 0.041(2) Uani 1 1 d . . . . .
H58A H 0.497054 0.964350 0.891349 0.049 Uiso 1 1 calc R U . . .
H58B H 0.441828 0.979285 0.885639 0.049 Uiso 1 1 calc R U . . .
C59 C 0.4650(4) 0.9802(6) 0.7269(8) 0.040(2) Uani 1 1 d . . . . .
H59 H 0.469988 1.044855 0.724968 0.047 Uiso 1 1 calc R U . . .
C60 C 0.5036(3) 0.9337(6) 0.6734(8) 0.039(2) Uani 1 1 d . . . . .
H60A H 0.534395 0.948655 0.714522 0.046 Uiso 1 1 calc R U . . .
H60B H 0.503380 0.953096 0.594629 0.046 Uiso 1 1 calc R U . . .
C61 C 0.4163(3) 0.9565(6) 0.6614(7) 0.0309(19) Uani 1 1 d . . . . .
H61A H 0.391323 0.987257 0.695513 0.037 Uiso 1 1 calc R U . . .
H61B H 0.415262 0.975888 0.582407 0.037 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
Rh1 O1 2.125(6) . ?
Rh1 N1 2.166(5) . ?
Rh1 N2 2.017(8) . ?
Rh1 N3 2.046(8) . ?
Rh1 C16 2.005(9) . ?
Rh1 C39 2.009(7) . ?
F1 C5 1.363(9) . ?
O1 C1 1.299(10) . ?
O2 C7 1.373(10) . ?
O2 C8 1.423(9) . ?
O3 C22 1.364(11) . ?
O3 C23 1.407(10) . ?
O4 C45 1.353(9) . ?
O4 C46 1.392(10) . ?
N1 C7 1.280(9) . ?
N1 C9 1.490(10) . ?
N2 C22 1.285(12) . ?
N2 C28 1.423(11) . ?
N3 C45 1.317(11) . ?
N3 C51 1.433(10) . ?
C1 C2 1.413(11) . ?
C1 C6 1.452(11) . ?
C2 H2 0.9500 . ?
C2 C3 1.374(11) . ?
C3 H3 0.9500 . ?
C3 C4 1.393(13) . ?
C4 H4 0.9500 . ?
C4 C5 1.368(12) . ?
C5 C6 1.410(10) . ?
C6 C7 1.448(11) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.551(11) . ?
C9 H9 1.0000 . ?
C9 C15 1.508(11) . ?
C10 H10 0.9500 . ?
C10 C11 1.381(14) . ?
C10 C15 1.390(12) . ?
C11 H11 0.9500 . ?
C11 C12 1.410(17) . ?
C12 H12 0.9500 . ?
C12 C13 1.380(17) . ?
C13 H13 0.9500 . ?
C13 C14 1.403(13) . ?
C14 H14 0.9500 . ?
C14 C15 1.395(14) . ?
C16 C17 1.380(13) . ?
C16 C21 1.448(13) . ?
C17 H17 0.9500 . ?
C17 C18 1.402(11) . ?
C18 H18 0.9500 . ?
C18 C19 1.376(12) . ?
C19 H19 0.9500 . ?
C19 C20 1.403(13) . ?
C20 H20 0.9500 . ?
C20 C21 1.392(13) . ?
C21 C22 1.434(11) . ?
C23 C24 1.360(11) . ?
C23 C28 1.382(11) . ?
C24 H24 0.9500 . ?
C24 C25 1.387(12) . ?
C25 H25 0.9500 . ?
C25 C26 1.413(11) . ?
C26 C27 1.395(11) . ?
C26 C29 1.525(11) . ?
C27 H27 0.9500 . ?
C27 C28 1.378(11) . ?
C29 C30 1.530(12) . ?
C29 C34 1.552(12) . ?
C29 C38 1.536(11) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.550(12) . ?
C31 H31 1.0000 . ?
C31 C32 1.531(14) . ?
C31 C35 1.535(14) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.538(13) . ?
C33 H33 1.0000 . ?
C33 C34 1.539(11) . ?
C33 C37 1.525(12) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.531(14) . ?
C36 H36 1.0000 . ?
C36 C37 1.540(13) . ?
C36 C38 1.534(12) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.391(12) . ?
C39 C44 1.402(13) . ?
C40 H40 0.9500 . ?
C40 C41 1.403(12) . ?
C41 H41 0.9500 . ?
C41 C42 1.402(12) . ?
C42 H42 0.9500 . ?
C42 C43 1.405(12) . ?
C43 H43 0.9500 . ?
C43 C44 1.400(12) . ?
C44 C45 1.427(11) . ?
C46 C47 1.389(11) . ?
C46 C51 1.385(12) . ?
C47 H47 0.9500 . ?
C47 C48 1.376(12) . ?
C48 H48 0.9500 . ?
C48 C49 1.422(11) . ?
C49 C50 1.390(11) . ?
C49 C52 1.513(11) . ?
C50 H50 0.9500 . ?
C50 C51 1.380(11) . ?
C52 C53 1.545(10) . ?
C52 C57 1.528(11) . ?
C52 C61 1.561(12) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.531(12) . ?
C54 H54 1.0000 . ?
C54 C55 1.544(12) . ?
C54 C58 1.515(14) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 C56 1.501(11) . ?
C56 H56 1.0000 . ?
C56 C57 1.546(12) . ?
C56 C60 1.534(13) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C59 1.542(13) . ?
C59 H59 1.0000 . ?
C59 C60 1.525(14) . ?
C59 C61 1.570(13) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?

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
O1 Rh1 N1 81.9(3) . . ?
N2 Rh1 O1 94.4(3) . . ?
N2 Rh1 N1 93.9(3) . . ?
N2 Rh1 N3 169.3(3) . . ?
N3 Rh1 O1 91.2(2) . . ?
N3 Rh1 N1 95.9(3) . . ?
C16 Rh1 O1 174.6(3) . . ?
C16 Rh1 N1 100.7(3) . . ?
C16 Rh1 N2 80.8(3) . . ?
C16 Rh1 N3 93.2(4) . . ?
C16 Rh1 C39 86.0(4) . . ?
C39 Rh1 O1 91.7(3) . . ?
C39 Rh1 N1 172.9(3) . . ?
C39 Rh1 N2 89.7(4) . . ?
C39 Rh1 N3 81.0(4) . . ?
C1 O1 Rh1 120.1(5) . . ?
C7 O2 C8 107.8(5) . . ?
C22 O3 C23 104.5(6) . . ?
C45 O4 C46 104.3(6) . . ?
C7 N1 Rh1 123.0(5) . . ?
C7 N1 C9 109.0(6) . . ?
C9 N1 Rh1 127.9(4) . . ?
C22 N2 Rh1 113.9(6) . . ?
C22 N2 C28 107.3(7) . . ?
C28 N2 Rh1 138.4(6) . . ?
C45 N3 Rh1 111.9(6) . . ?
C45 N3 C51 105.9(7) . . ?
C51 N3 Rh1 142.2(6) . . ?
O1 C1 C2 119.8(8) . . ?
O1 C1 C6 122.4(7) . . ?
C2 C1 C6 117.8(7) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 C1 121.6(8) . . ?
C3 C2 H2 119.2 . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.4(8) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 H4 120.9 . . ?
C5 C4 C3 118.2(7) . . ?
C5 C4 H4 120.9 . . ?
F1 C5 C4 117.5(7) . . ?
F1 C5 C6 118.8(7) . . ?
C4 C5 C6 123.7(8) . . ?
C5 C6 C1 117.3(7) . . ?
C5 C6 C7 123.0(7) . . ?
C7 C6 C1 119.6(6) . . ?
O2 C7 C6 116.2(6) . . ?
N1 C7 O2 115.6(7) . . ?
N1 C7 C6 128.3(7) . . ?
O2 C8 H8A 110.7 . . ?
O2 C8 H8B 110.7 . . ?
O2 C8 C9 105.2(6) . . ?
H8A C8 H8B 108.8 . . ?
C9 C8 H8A 110.7 . . ?
C9 C8 H8B 110.7 . . ?
N1 C9 C8 102.3(6) . . ?
N1 C9 H9 109.4 . . ?
N1 C9 C15 114.1(6) . . ?
C8 C9 H9 109.4 . . ?
C15 C9 C8 111.9(7) . . ?
C15 C9 H9 109.4 . . ?
C11 C10 H10 119.7 . . ?
C11 C10 C15 120.6(11) . . ?
C15 C10 H10 119.7 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.4(10) . . ?
C12 C11 H11 119.8 . . ?
C11 C12 H12 120.4 . . ?
C13 C12 C11 119.2(10) . . ?
C13 C12 H12 120.4 . . ?
C12 C13 H13 119.8 . . ?
C12 C13 C14 120.3(11) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 119.9 . . ?
C15 C14 C13 120.2(9) . . ?
C15 C14 H14 119.9 . . ?
C10 C15 C9 120.9(8) . . ?
C10 C15 C14 119.3(9) . . ?
C14 C15 C9 119.8(8) . . ?
C17 C16 Rh1 129.9(7) . . ?
C17 C16 C21 116.3(8) . . ?
C21 C16 Rh1 113.6(7) . . ?
C16 C17 H17 119.5 . . ?
C16 C17 C18 121.0(8) . . ?
C18 C17 H17 119.5 . . ?
C17 C18 H18 119.1 . . ?
C19 C18 C17 121.8(8) . . ?
C19 C18 H18 119.1 . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.1(8) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 121.1 . . ?
C21 C20 C19 117.8(8) . . ?
C21 C20 H20 121.1 . . ?
C20 C21 C16 123.0(9) . . ?
C20 C21 C22 126.6(10) . . ?
C22 C21 C16 110.4(9) . . ?
O3 C22 C21 125.5(9) . . ?
N2 C22 O3 113.8(8) . . ?
N2 C22 C21 120.7(9) . . ?
C24 C23 O3 128.9(7) . . ?
C24 C23 C28 122.6(8) . . ?
C28 C23 O3 108.3(7) . . ?
C23 C24 H24 122.1 . . ?
C23 C24 C25 115.8(7) . . ?
C25 C24 H24 122.1 . . ?
C24 C25 H25 118.5 . . ?
C24 C25 C26 123.1(8) . . ?
C26 C25 H25 118.5 . . ?
C25 C26 C29 119.2(7) . . ?
C27 C26 C25 119.2(7) . . ?
C27 C26 C29 121.4(7) . . ?
C26 C27 H27 121.5 . . ?
C28 C27 C26 117.0(7) . . ?
C28 C27 H27 121.5 . . ?
C23 C28 N2 106.1(7) . . ?
C27 C28 N2 131.5(7) . . ?
C27 C28 C23 122.3(8) . . ?
C26 C29 C30 111.4(7) . . ?
C26 C29 C34 107.5(7) . . ?
C26 C29 C38 112.5(7) . . ?
C30 C29 C34 108.9(7) . . ?
C30 C29 C38 108.8(7) . . ?
C38 C29 C34 107.7(7) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 C31 110.5(7) . . ?
H30A C30 H30B 108.1 . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
C30 C31 H31 109.7 . . ?
C32 C31 C30 109.9(8) . . ?
C32 C31 H31 109.7 . . ?
C32 C31 C35 108.7(8) . . ?
C35 C31 C30 109.0(8) . . ?
C35 C31 H31 109.7 . . ?
C31 C32 H32A 109.6 . . ?
C31 C32 H32B 109.6 . . ?
C31 C32 C33 110.3(8) . . ?
H32A C32 H32B 108.1 . . ?
C33 C32 H32A 109.6 . . ?
C33 C32 H32B 109.6 . . ?
C32 C33 H33 109.7 . . ?
C32 C33 C34 109.5(7) . . ?
C34 C33 H33 109.7 . . ?
C37 C33 C32 109.1(8) . . ?
C37 C33 H33 109.7 . . ?
C37 C33 C34 109.0(8) . . ?
C29 C34 H34A 109.5 . . ?
C29 C34 H34B 109.5 . . ?
C33 C34 C29 110.9(7) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
C31 C35 H35A 109.9 . . ?
C31 C35 H35B 109.9 . . ?
H35A C35 H35B 108.3 . . ?
C36 C35 C31 109.1(8) . . ?
C36 C35 H35A 109.9 . . ?
C36 C35 H35B 109.9 . . ?
C35 C36 H36 109.1 . . ?
C35 C36 C37 110.3(9) . . ?
C35 C36 C38 109.7(8) . . ?
C37 C36 H36 109.1 . . ?
C38 C36 H36 109.1 . . ?
C38 C36 C37 109.5(8) . . ?
C33 C37 C36 109.1(7) . . ?
C33 C37 H37A 109.9 . . ?
C33 C37 H37B 109.9 . . ?
C36 C37 H37A 109.9 . . ?
C36 C37 H37B 109.9 . . ?
H37A C37 H37B 108.3 . . ?
C29 C38 H38A 109.6 . . ?
C29 C38 H38B 109.6 . . ?
C36 C38 C29 110.4(7) . . ?
C36 C38 H38A 109.6 . . ?
C36 C38 H38B 109.6 . . ?
H38A C38 H38B 108.1 . . ?
C40 C39 Rh1 129.5(7) . . ?
C40 C39 C44 116.3(7) . . ?
C44 C39 Rh1 114.1(6) . . ?
C39 C40 H40 119.2 . . ?
C39 C40 C41 121.5(8) . . ?
C41 C40 H40 119.2 . . ?
C40 C41 H41 119.4 . . ?
C42 C41 C40 121.2(7) . . ?
C42 C41 H41 119.4 . . ?
C41 C42 H42 120.9 . . ?
C41 C42 C43 118.3(8) . . ?
C43 C42 H42 120.9 . . ?
C42 C43 H43 120.6 . . ?
C44 C43 C42 118.9(8) . . ?
C44 C43 H43 120.6 . . ?
C39 C44 C45 112.5(7) . . ?
C43 C44 C39 123.7(7) . . ?
C43 C44 C45 123.9(8) . . ?
O4 C45 C44 125.2(7) . . ?
N3 C45 O4 114.3(7) . . ?
N3 C45 C44 120.4(7) . . ?
C47 C46 O4 127.6(8) . . ?
C51 C46 O4 109.8(7) . . ?
C51 C46 C47 122.5(8) . . ?
C46 C47 H47 122.5 . . ?
C48 C47 C46 115.0(8) . . ?
C48 C47 H47 122.5 . . ?
C47 C48 H48 118.1 . . ?
C47 C48 C49 123.8(7) . . ?
C49 C48 H48 118.1 . . ?
C48 C49 C52 118.7(7) . . ?
C50 C49 C48 119.1(8) . . ?
C50 C49 C52 122.2(7) . . ?
C49 C50 H50 121.3 . . ?
C51 C50 C49 117.4(7) . . ?
C51 C50 H50 121.3 . . ?
C46 C51 N3 105.6(7) . . ?
C50 C51 N3 132.3(8) . . ?
C50 C51 C46 122.1(7) . . ?
C49 C52 C53 110.3(6) . . ?
C49 C52 C57 113.9(6) . . ?
C49 C52 C61 109.2(6) . . ?
C53 C52 C61 107.9(6) . . ?
C57 C52 C53 108.1(6) . . ?
C57 C52 C61 107.3(7) . . ?
C52 C53 H53A 109.2 . . ?
C52 C53 H53B 109.2 . . ?
H53A C53 H53B 107.9 . . ?
C54 C53 C52 112.0(7) . . ?
C54 C53 H53A 109.2 . . ?
C54 C53 H53B 109.2 . . ?
C53 C54 H54 109.8 . . ?
C53 C54 C55 109.6(7) . . ?
C55 C54 H54 109.8 . . ?
C58 C54 C53 109.5(7) . . ?
C58 C54 H54 109.8 . . ?
C58 C54 C55 108.3(8) . . ?
C54 C55 H55A 109.7 . . ?
C54 C55 H55B 109.7 . . ?
H55A C55 H55B 108.2 . . ?
C56 C55 C54 109.7(7) . . ?
C56 C55 H55A 109.7 . . ?
C56 C55 H55B 109.7 . . ?
C55 C56 H56 109.2 . . ?
C55 C56 C57 110.7(7) . . ?
C55 C56 C60 108.9(7) . . ?
C57 C56 H56 109.2 . . ?
C60 C56 H56 109.2 . . ?
C60 C56 C57 109.5(7) . . ?
C52 C57 C56 111.4(6) . . ?
C52 C57 H57A 109.3 . . ?
C52 C57 H57B 109.3 . . ?
C56 C57 H57A 109.3 . . ?
C56 C57 H57B 109.3 . . ?
H57A C57 H57B 108.0 . . ?
C54 C58 H58A 109.6 . . ?
C54 C58 H58B 109.6 . . ?
C54 C58 C59 110.3(7) . . ?
H58A C58 H58B 108.1 . . ?
C59 C58 H58A 109.6 . . ?
C59 C58 H58B 109.6 . . ?
C58 C59 H59 109.8 . . ?
C58 C59 C61 109.2(8) . . ?
C60 C59 C58 108.6(8) . . ?
C60 C59 H59 109.8 . . ?
C60 C59 C61 109.7(7) . . ?
C61 C59 H59 109.8 . . ?
C56 C60 H60A 109.8 . . ?
C56 C60 H60B 109.8 . . ?
C59 C60 C56 109.4(8) . . ?
C59 C60 H60A 109.8 . . ?
C59 C60 H60B 109.8 . . ?
H60A C60 H60B 108.2 . . ?
C52 C61 C59 110.1(7) . . ?
C52 C61 H61A 109.6 . . ?
C52 C61 H61B 109.6 . . ?
C59 C61 H61A 109.6 . . ?
C59 C61 H61B 109.6 . . ?
H61A C61 H61B 108.2 . . ?

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
Rh1 O1 C1 C2 132.3(7) . . . . ?
Rh1 O1 C1 C6 -48.0(10) . . . . ?
Rh1 N1 C7 O2 -178.4(5) . . . . ?
Rh1 N1 C7 C6 1.3(13) . . . . ?
Rh1 N1 C9 C8 179.7(7) . . . . ?
Rh1 N1 C9 C15 -59.2(10) . . . . ?
Rh1 N2 C22 O3 -173.2(6) . . . . ?
Rh1 N2 C22 C21 7.9(13) . . . . ?
Rh1 N2 C28 C23 170.2(7) . . . . ?
Rh1 N2 C28 C27 -14.8(16) . . . . ?
Rh1 N3 C45 O4 178.0(5) . . . . ?
Rh1 N3 C45 C44 -1.3(9) . . . . ?
Rh1 N3 C51 C46 -177.0(7) . . . . ?
Rh1 N3 C51 C50 3.7(15) . . . . ?
Rh1 C16 C17 C18 -174.9(7) . . . . ?
Rh1 C16 C21 C20 175.8(7) . . . . ?
Rh1 C16 C21 C22 -3.7(11) . . . . ?
Rh1 C39 C40 C41 178.1(7) . . . . ?
Rh1 C39 C44 C43 179.2(6) . . . . ?
Rh1 C39 C44 C45 0.7(10) . . . . ?
F1 C5 C6 C1 -179.3(7) . . . . ?
F1 C5 C6 C7 -2.4(12) . . . . ?
O1 C1 C2 C3 179.7(8) . . . . ?
O1 C1 C6 C5 -179.4(7) . . . . ?
O1 C1 C6 C7 3.6(12) . . . . ?
O2 C8 C9 N1 -3.0(10) . . . . ?
O2 C8 C9 C15 -125.6(8) . . . . ?
O3 C23 C24 C25 174.2(8) . . . . ?
O3 C23 C28 N2 1.4(9) . . . . ?
O3 C23 C28 C27 -174.1(8) . . . . ?
O4 C46 C47 C48 -177.5(7) . . . . ?
O4 C46 C51 N3 -1.5(9) . . . . ?
O4 C46 C51 C50 177.9(7) . . . . ?
N1 C9 C15 C10 125.8(8) . . . . ?
N1 C9 C15 C14 -57.6(10) . . . . ?
C1 C2 C3 C4 -0.3(14) . . . . ?
C1 C6 C7 O2 -158.0(7) . . . . ?
C1 C6 C7 N1 22.3(13) . . . . ?
C2 C1 C6 C5 0.3(11) . . . . ?
C2 C1 C6 C7 -176.7(7) . . . . ?
C2 C3 C4 C5 0.2(14) . . . . ?
C3 C4 C5 F1 179.1(8) . . . . ?
C3 C4 C5 C6 0.0(14) . . . . ?
C4 C5 C6 C1 -0.3(12) . . . . ?
C4 C5 C6 C7 176.6(8) . . . . ?
C5 C6 C7 O2 25.2(11) . . . . ?
C5 C6 C7 N1 -154.5(9) . . . . ?
C6 C1 C2 C3 0.0(13) . . . . ?
C7 O2 C8 C9 2.6(10) . . . . ?
C7 N1 C9 C8 2.4(10) . . . . ?
C7 N1 C9 C15 123.5(8) . . . . ?
C8 O2 C7 N1 -1.1(10) . . . . ?
C8 O2 C7 C6 179.1(8) . . . . ?
C8 C9 C15 C10 -118.6(9) . . . . ?
C8 C9 C15 C14 57.9(10) . . . . ?
C9 N1 C7 O2 -1.0(10) . . . . ?
C9 N1 C7 C6 178.8(8) . . . . ?
C10 C11 C12 C13 0.4(15) . . . . ?
C11 C10 C15 C9 175.5(8) . . . . ?
C11 C10 C15 C14 -1.0(12) . . . . ?
C11 C12 C13 C14 -1.5(15) . . . . ?
C12 C13 C14 C15 1.4(15) . . . . ?
C13 C14 C15 C9 -176.7(8) . . . . ?
C13 C14 C15 C10 -0.1(13) . . . . ?
C15 C10 C11 C12 0.9(14) . . . . ?
C16 C17 C18 C19 -0.7(14) . . . . ?
C16 C21 C22 O3 178.4(7) . . . . ?
C16 C21 C22 N2 -2.8(16) . . . . ?
C17 C16 C21 C20 -0.2(14) . . . . ?
C17 C16 C21 C22 -179.7(9) . . . . ?
C17 C18 C19 C20 0.8(14) . . . . ?
C18 C19 C20 C21 -0.6(14) . . . . ?
C19 C20 C21 C16 0.3(14) . . . . ?
C19 C20 C21 C22 179.8(11) . . . . ?
C20 C21 C22 O3 -1.1(19) . . . . ?
C20 C21 C22 N2 177.7(8) . . . . ?
C21 C16 C17 C18 0.4(13) . . . . ?
C22 O3 C23 C24 -177.1(9) . . . . ?
C22 O3 C23 C28 -1.1(9) . . . . ?
C22 N2 C28 C23 -1.2(10) . . . . ?
C22 N2 C28 C27 173.8(9) . . . . ?
C23 O3 C22 N2 0.3(10) . . . . ?
C23 O3 C22 C21 179.1(11) . . . . ?
C23 C24 C25 C26 -1.1(13) . . . . ?
C24 C23 C28 N2 177.7(8) . . . . ?
C24 C23 C28 C27 2.2(13) . . . . ?
C24 C25 C26 C27 2.6(13) . . . . ?
C24 C25 C26 C29 -172.0(8) . . . . ?
C25 C26 C27 C28 -1.7(12) . . . . ?
C25 C26 C29 C30 -59.9(10) . . . . ?
C25 C26 C29 C34 59.3(10) . . . . ?
C25 C26 C29 C38 177.6(8) . . . . ?
C26 C27 C28 N2 -174.9(9) . . . . ?
C26 C27 C28 C23 -0.6(12) . . . . ?
C26 C29 C30 C31 176.7(7) . . . . ?
C26 C29 C34 C33 -179.5(7) . . . . ?
C26 C29 C38 C36 -177.3(8) . . . . ?
C27 C26 C29 C30 125.6(8) . . . . ?
C27 C26 C29 C34 -115.2(8) . . . . ?
C27 C26 C29 C38 3.2(12) . . . . ?
C28 N2 C22 O3 0.6(11) . . . . ?
C28 N2 C22 C21 -178.3(10) . . . . ?
C28 C23 C24 C25 -1.3(12) . . . . ?
C29 C26 C27 C28 172.8(8) . . . . ?
C29 C30 C31 C32 -59.1(10) . . . . ?
C29 C30 C31 C35 60.0(10) . . . . ?
C30 C29 C34 C33 -58.7(9) . . . . ?
C30 C29 C38 C36 58.8(10) . . . . ?
C30 C31 C32 C33 58.6(10) . . . . ?
C30 C31 C35 C36 -60.0(10) . . . . ?
C31 C32 C33 C34 -58.5(10) . . . . ?
C31 C32 C33 C37 60.7(10) . . . . ?
C31 C35 C36 C37 -60.2(9) . . . . ?
C31 C35 C36 C38 60.5(10) . . . . ?
C32 C31 C35 C36 59.9(10) . . . . ?
C32 C33 C34 C29 58.7(10) . . . . ?
C32 C33 C37 C36 -59.3(11) . . . . ?
C34 C29 C30 C31 58.3(9) . . . . ?
C34 C29 C38 C36 -59.1(10) . . . . ?
C34 C33 C37 C36 60.2(11) . . . . ?
C35 C31 C32 C33 -60.7(10) . . . . ?
C35 C36 C37 C33 60.0(11) . . . . ?
C35 C36 C38 C29 -60.2(11) . . . . ?
C37 C33 C34 C29 -60.5(9) . . . . ?
C37 C36 C38 C29 60.9(11) . . . . ?
C38 C29 C30 C31 -58.8(10) . . . . ?
C38 C29 C34 C33 59.1(9) . . . . ?
C38 C36 C37 C33 -60.8(11) . . . . ?
C39 C40 C41 C42 1.7(12) . . . . ?
C39 C44 C45 O4 -178.7(7) . . . . ?
C39 C44 C45 N3 0.5(11) . . . . ?
C40 C39 C44 C43 -4.0(13) . . . . ?
C40 C39 C44 C45 177.5(8) . . . . ?
C40 C41 C42 C43 -3.5(11) . . . . ?
C41 C42 C43 C44 1.5(11) . . . . ?
C42 C43 C44 C39 2.3(12) . . . . ?
C42 C43 C44 C45 -179.3(7) . . . . ?
C43 C44 C45 O4 2.8(12) . . . . ?
C43 C44 C45 N3 -178.0(7) . . . . ?
C44 C39 C40 C41 2.0(13) . . . . ?
C45 O4 C46 C47 178.0(8) . . . . ?
C45 O4 C46 C51 0.9(8) . . . . ?
C45 N3 C51 C46 1.6(9) . . . . ?
C45 N3 C51 C50 -177.7(8) . . . . ?
C46 O4 C45 N3 0.1(8) . . . . ?
C46 O4 C45 C44 179.4(7) . . . . ?
C46 C47 C48 C49 0.1(12) . . . . ?
C47 C46 C51 N3 -178.8(7) . . . . ?
C47 C46 C51 C50 0.6(12) . . . . ?
C47 C48 C49 C50 0.7(12) . . . . ?
C47 C48 C49 C52 -177.6(7) . . . . ?
C48 C49 C50 C51 -0.9(11) . . . . ?
C48 C49 C52 C53 61.1(9) . . . . ?
C48 C49 C52 C57 -177.1(7) . . . . ?
C48 C49 C52 C61 -57.2(9) . . . . ?
C49 C50 C51 N3 179.5(8) . . . . ?
C49 C50 C51 C46 0.3(11) . . . . ?
C49 C52 C53 C54 -177.8(7) . . . . ?
C49 C52 C57 C56 -179.3(6) . . . . ?
C49 C52 C61 C59 177.3(7) . . . . ?
C50 C49 C52 C53 -117.1(8) . . . . ?
C50 C49 C52 C57 4.7(10) . . . . ?
C50 C49 C52 C61 124.6(8) . . . . ?
C51 N3 C45 O4 -1.1(9) . . . . ?
C51 N3 C45 C44 179.6(7) . . . . ?
C51 C46 C47 C48 -0.7(12) . . . . ?
C52 C49 C50 C51 177.3(7) . . . . ?
C52 C53 C54 C55 -58.5(9) . . . . ?
C52 C53 C54 C58 60.2(9) . . . . ?
C53 C52 C57 C56 -56.4(9) . . . . ?
C53 C52 C61 C59 57.5(9) . . . . ?
C53 C54 C55 C56 58.4(10) . . . . ?
C53 C54 C58 C59 -59.8(10) . . . . ?
C54 C55 C56 C57 -58.6(9) . . . . ?
C54 C55 C56 C60 61.8(10) . . . . ?
C54 C58 C59 C60 -59.9(10) . . . . ?
C54 C58 C59 C61 59.7(10) . . . . ?
C55 C54 C58 C59 59.7(9) . . . . ?
C55 C56 C57 C52 59.1(9) . . . . ?
C55 C56 C60 C59 -61.7(9) . . . . ?
C57 C52 C53 C54 57.1(9) . . . . ?
C57 C52 C61 C59 -58.8(8) . . . . ?
C57 C56 C60 C59 59.6(9) . . . . ?
C58 C54 C55 C56 -61.0(9) . . . . ?
C58 C59 C60 C56 59.7(10) . . . . ?
C58 C59 C61 C52 -58.9(10) . . . . ?
C60 C56 C57 C52 -61.0(9) . . . . ?
C60 C59 C61 C52 60.0(10) . . . . ?
C61 C52 C53 C54 -58.7(9) . . . . ?
C61 C52 C57 C56 59.7(8) . . . . ?
C61 C59 C60 C56 -59.5(10) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 168 electrons were 
found in a volume of 822Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH3COOC2H5] per Asymmetric Unit 
which account for 192 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.241 -0.957 410.5 83.7 '2 CH3COOC2H5'
2 0.500 0.259 -0.232 410.5 83.7 '2 CH3COOC2H5'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_tius007
_database_code_depnum_ccdc_archive 'CCDC 2154236'
loop_
_audit_author_name
_audit_author_address
'Glenn P. A. Yap'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-02-23 deposited with the CCDC.	2023-05-29 downloaded from the CCDC.
;
_audit_creation_date             2022-02-22
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H40 O7'
_chemical_formula_sum            'C32 H40 O7'
_chemical_formula_weight         536.64
_chemical_absolute_configuration rm
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   6.7321(2)
_cell_length_b                   9.8995(3)
_cell_length_c                   41.9029(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2792.59(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9269
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      64.80
_cell_measurement_theta_min      4.22
_shelx_estimated_absorpt_T_max   0.979
_shelx_estimated_absorpt_T_min   0.898
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1409 before and 0.0623 after correction.
The Ratio of minimum to maximum transmission is 0.8328.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1152
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2.00 1.00 0.00 0.0560
-1.00 1.00 1.00 0.0490
0.00 1.00 1.00 0.0120
0.00 -1.00 -1.00 0.0060
0.00 2.00 -1.00 0.0140
0.00 0.00 1.00 0.0060
0.00 0.00 -1.00 0.0150
1.00 -1.00 -1.00 0.0560
1.00 1.00 2.00 0.0660

_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.029
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            27183
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        65.012
_diffrn_reflns_theta_max         65.012
_diffrn_reflns_theta_min         2.109
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Venture Photon III'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.707
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                4232
_reflns_number_total             4710
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 
;
 Flack x determined using 1469 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         4710
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0505
_refine_ls_restrained_S_all      1.199
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0367P)²+1.2386P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1059
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.5663(4) 0.7056(3) 0.28778(5) 0.0214(6) Uani 1 1 d . . . . .
O2 O 0.6292(4) 0.7909(3) 0.23930(6) 0.0300(7) Uani 1 1 d . . . . .
O3 O 0.6210(4) 0.7218(3) 0.34984(5) 0.0213(6) Uani 1 1 d . . . . .
O4 O 0.3300(4) 0.6198(4) 0.36006(6) 0.0457(9) Uani 1 1 d . . . . .
O5 O 0.4504(4) 0.8880(3) 0.40072(6) 0.0292(7) Uani 1 1 d . . . . .
O6 O 0.8945(4) 0.9407(2) 0.41522(5) 0.0209(6) Uani 1 1 d . . . . .
O7 O 0.8823(4) 0.9296(3) 0.46873(6) 0.0292(7) Uani 1 1 d . . . . .
C1 C 0.5130(6) 0.7750(4) 0.26071(8) 0.0223(9) Uani 1 1 d . . . . .
C2 C 0.2971(6) 0.8131(4) 0.26410(8) 0.0220(9) Uani 1 1 d . . . . .
C3 C 0.2916(6) 0.8402(4) 0.30071(8) 0.0213(9) Uani 1 1 d . . . . .
C4 C 0.3867(6) 0.7018(4) 0.30752(8) 0.0201(8) Uani 1 1 d . . . . .
C5 C 0.2494(6) 0.5990(4) 0.29193(8) 0.0222(9) Uani 1 1 d . . . . .
H5A H 0.133081 0.578807 0.305585 0.027 Uiso 1 1 calc R U . . .
H5B H 0.320117 0.513967 0.286906 0.027 Uiso 1 1 calc R U . . .
C6 C 0.1875(6) 0.6759(4) 0.26106(8) 0.0252(9) Uani 1 1 d . . . . .
H6A H 0.230866 0.626477 0.241735 0.030 Uiso 1 1 calc R U . . .
H6B H 0.041843 0.688952 0.260188 0.030 Uiso 1 1 calc R U . . .
C7 C 0.2278(6) 0.9234(4) 0.24179(9) 0.0300(10) Uani 1 1 d . . . . .
H7A H 0.289705 1.009218 0.247897 0.045 Uiso 1 1 calc R U . . .
H7B H 0.083039 0.931923 0.243132 0.045 Uiso 1 1 calc R U . . .
H7C H 0.265829 0.900660 0.219859 0.045 Uiso 1 1 calc R U . . .
C8 C 0.0833(6) 0.8577(4) 0.31481(10) 0.0313(10) Uani 1 1 d . . . . .
H8A H 0.027779 0.944317 0.307844 0.047 Uiso 1 1 calc R U . . .
H8B H 0.091291 0.855972 0.338157 0.047 Uiso 1 1 calc R U . . .
H8C H -0.002320 0.783969 0.307448 0.047 Uiso 1 1 calc R U . . .
C9 C 0.4206(6) 0.9605(4) 0.31073(9) 0.0267(9) Uani 1 1 d . . . . .
H9A H 0.556349 0.947387 0.302889 0.040 Uiso 1 1 calc R U . . .
H9B H 0.422197 0.967390 0.334062 0.040 Uiso 1 1 calc R U . . .
H9C H 0.365685 1.043793 0.301653 0.040 Uiso 1 1 calc R U . . .
C10 C 0.4405(6) 0.6735(4) 0.34170(9) 0.0238(9) Uani 1 1 d . . . . .
C11 C 0.6648(5) 0.7111(4) 0.38252(8) 0.0189(8) Uani 1 1 d . . . . .
C12 C 0.7879(5) 0.6208(4) 0.39518(8) 0.0177(8) Uani 1 1 d . . . . .
C13 C 0.7982(5) 0.6362(4) 0.43137(8) 0.0187(8) Uani 1 1 d . . . . .
C14 C 0.6810(6) 0.7752(4) 0.43741(8) 0.0210(8) Uani 1 1 d . . . . .
C15 C 0.5780(5) 0.8034(4) 0.40540(8) 0.0198(8) Uani 1 1 d . . . . .
C16 C 0.8969(6) 0.5154(4) 0.37710(9) 0.0240(9) Uani 1 1 d . . . . .
H16A H 0.857520 0.425890 0.384826 0.036 Uiso 1 1 calc R U . . .
H16B H 1.040104 0.527516 0.380169 0.036 Uiso 1 1 calc R U . . .
H16C H 0.865066 0.523177 0.354349 0.036 Uiso 1 1 calc R U . . .
C17 C 0.5031(5) 0.4686(4) 0.43008(8) 0.0183(8) Uani 1 1 d . . . . .
H17A H 0.416074 0.547705 0.426412 0.022 Uiso 1 1 calc R U . . .
H17B H 0.542715 0.432381 0.408998 0.022 Uiso 1 1 calc R U . . .
C18 C 0.3874(6) 0.3607(4) 0.44826(8) 0.0214(8) Uani 1 1 d . . . . .
H18A H 0.338767 0.398715 0.468660 0.026 Uiso 1 1 calc R U . . .
H18B H 0.270680 0.332505 0.435521 0.026 Uiso 1 1 calc R U . . .
C19 C 0.5180(6) 0.2382(4) 0.45499(9) 0.0242(9) Uani 1 1 d . . . . .
H19A H 0.556864 0.195028 0.434617 0.029 Uiso 1 1 calc R U . . .
H19B H 0.442735 0.171383 0.467741 0.029 Uiso 1 1 calc R U . . .
C20 C 0.7037(6) 0.2817(4) 0.47324(8) 0.0219(8) Uani 1 1 d . . . . .
H20A H 0.789740 0.202012 0.476758 0.026 Uiso 1 1 calc R U . . .
H20B H 0.664250 0.317346 0.494384 0.026 Uiso 1 1 calc R U . . .
C21 C 0.8217(5) 0.3904(4) 0.45523(8) 0.0211(8) Uani 1 1 d . . . . .
H21A H 0.871817 0.352618 0.434889 0.025 Uiso 1 1 calc R U . . .
H21B H 0.937511 0.418492 0.468197 0.025 Uiso 1 1 calc R U . . .
C22 C 0.6899(6) 0.5142(4) 0.44828(8) 0.0186(8) Uani 1 1 d . . . . .
H22 H 0.643285 0.548520 0.469440 0.022 Uiso 1 1 calc R U . . .
C23 C 0.8292(6) 0.8897(4) 0.44303(9) 0.0226(9) Uani 1 1 d . . . . .
C24 C 1.0349(6) 1.0521(4) 0.41693(9) 0.0237(9) Uani 1 1 d . . . . .
H24A H 1.169811 1.017704 0.421659 0.028 Uiso 1 1 calc R U . . .
H24B H 0.995831 1.115730 0.434034 0.028 Uiso 1 1 calc R U . . .
C25 C 0.8623(6) 1.1285(4) 0.36650(9) 0.0241(9) Uani 1 1 d . . . . .
H25 H 0.742958 1.087759 0.373838 0.029 Uiso 1 1 calc R U . . .
C26 C 0.8660(7) 1.1949(4) 0.33698(9) 0.0278(9) Uani 1 1 d . . . . .
H26 H 0.749660 1.198005 0.324180 0.033 Uiso 1 1 calc R U . . .
C27 C 1.0383(7) 1.2558(4) 0.32646(9) 0.0285(10) Uani 1 1 d . . . . .
H27 H 1.040325 1.300817 0.306440 0.034 Uiso 1 1 calc R U . . .
C28 C 1.2076(6) 1.2513(4) 0.34496(9) 0.0279(10) Uani 1 1 d . . . . .
H28 H 1.325453 1.294644 0.337835 0.033 Uiso 1 1 calc R U . . .
C29 C 1.2063(6) 1.1835(4) 0.37400(9) 0.0263(9) Uani 1 1 d . . . . .
H29 H 1.324116 1.178697 0.386419 0.032 Uiso 1 1 calc R U . . .
C30 C 1.0326(5) 1.1224(4) 0.38499(8) 0.0199(8) Uani 1 1 d . . . . .
C31 C 0.5334(6) 0.7795(4) 0.46517(8) 0.0254(9) Uani 1 1 d . . . . .
H31A H 0.604375 0.764897 0.485297 0.038 Uiso 1 1 calc R U . . .
H31B H 0.433502 0.708495 0.462332 0.038 Uiso 1 1 calc R U . . .
H31C H 0.467765 0.867842 0.465666 0.038 Uiso 1 1 calc R U . . .
C32 C 1.0160(5) 0.6457(4) 0.44204(9) 0.0233(9) Uani 1 1 d . . . . .
H32A H 1.085352 0.561935 0.436434 0.035 Uiso 1 1 calc R U . . .
H32B H 1.021576 0.659056 0.465194 0.035 Uiso 1 1 calc R U . . .
H32C H 1.079980 0.722084 0.431300 0.035 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
O1 C1 1.373(4) . ?
O1 C4 1.465(4) . ?
O2 C1 1.201(4) . ?
O3 C10 1.350(4) . ?
O3 C11 1.405(4) . ?
O4 C10 1.195(4) . ?
O5 C15 1.215(4) . ?
O6 C23 1.344(4) . ?
O6 C24 1.454(5) . ?
O7 C23 1.201(4) . ?
C1 C2 1.508(6) . ?
C2 C3 1.558(5) . ?
C2 C6 1.551(5) . ?
C2 C7 1.511(5) . ?
C3 C4 1.540(5) . ?
C3 C8 1.531(5) . ?
C3 C9 1.533(5) . ?
C4 C5 1.522(5) . ?
C4 C10 1.503(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.557(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 C12 1.329(5) . ?
C11 C15 1.448(5) . ?
C12 C13 1.526(5) . ?
C12 C16 1.484(5) . ?
C13 C14 1.607(5) . ?
C13 C22 1.579(5) . ?
C13 C32 1.535(5) . ?
C14 C15 1.536(5) . ?
C14 C23 1.528(6) . ?
C14 C31 1.531(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.526(5) . ?
C17 C22 1.538(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.523(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.528(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.536(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.541(5) . ?
C22 H22 1.0000 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C30 1.509(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.401(5) . ?
C25 C30 1.385(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.379(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.379(6) . ?
C28 H28 0.9500 . ?
C28 C29 1.390(6) . ?
C29 H29 0.9500 . ?
C29 C30 1.395(5) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 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
C1 O1 C4 105.3(3) . . ?
C10 O3 C11 114.1(3) . . ?
C23 O6 C24 117.0(3) . . ?
O1 C1 C2 107.4(3) . . ?
O2 C1 O1 120.8(4) . . ?
O2 C1 C2 131.7(3) . . ?
C1 C2 C3 99.2(3) . . ?
C1 C2 C6 103.4(3) . . ?
C1 C2 C7 114.8(3) . . ?
C6 C2 C3 102.7(3) . . ?
C7 C2 C3 118.5(3) . . ?
C7 C2 C6 115.8(3) . . ?
C4 C3 C2 91.1(3) . . ?
C8 C3 C2 114.9(3) . . ?
C8 C3 C4 114.2(3) . . ?
C8 C3 C9 109.0(3) . . ?
C9 C3 C2 113.0(3) . . ?
C9 C3 C4 113.9(3) . . ?
O1 C4 C3 102.4(3) . . ?
O1 C4 C5 106.0(3) . . ?
O1 C4 C10 110.1(3) . . ?
C5 C4 C3 105.2(3) . . ?
C10 C4 C3 116.3(3) . . ?
C10 C4 C5 115.5(3) . . ?
C4 C5 H5A 111.6 . . ?
C4 C5 H5B 111.6 . . ?
C4 C5 C6 101.1(3) . . ?
H5A C5 H5B 109.4 . . ?
C6 C5 H5A 111.6 . . ?
C6 C5 H5B 111.6 . . ?
C2 C6 C5 103.5(3) . . ?
C2 C6 H6A 111.1 . . ?
C2 C6 H6B 111.1 . . ?
C5 C6 H6A 111.1 . . ?
C5 C6 H6B 111.1 . . ?
H6A C6 H6B 109.0 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C9 H9A 109.5 . . ?
C3 C9 H9B 109.5 . . ?
C3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 C4 113.1(3) . . ?
O4 C10 O3 123.8(3) . . ?
O4 C10 C4 123.1(3) . . ?
O3 C11 C15 120.9(3) . . ?
C12 C11 O3 124.8(3) . . ?
C12 C11 C15 114.3(3) . . ?
C11 C12 C13 111.0(3) . . ?
C11 C12 C16 125.3(3) . . ?
C16 C12 C13 123.7(3) . . ?
C12 C13 C14 102.7(3) . . ?
C12 C13 C22 110.4(3) . . ?
C12 C13 C32 109.8(3) . . ?
C22 C13 C14 110.9(3) . . ?
C32 C13 C14 111.7(3) . . ?
C32 C13 C22 110.9(3) . . ?
C15 C14 C13 103.9(3) . . ?
C23 C14 C13 109.8(3) . . ?
C23 C14 C15 107.2(3) . . ?
C23 C14 C31 106.6(3) . . ?
C31 C14 C13 117.5(3) . . ?
C31 C14 C15 111.5(3) . . ?
O5 C15 C11 127.8(3) . . ?
O5 C15 C14 125.8(3) . . ?
C11 C15 C14 106.3(3) . . ?
C12 C16 H16A 109.5 . . ?
C12 C16 H16B 109.5 . . ?
C12 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
H17A C17 H17B 107.9 . . ?
C18 C17 H17A 109.2 . . ?
C18 C17 H17B 109.2 . . ?
C18 C17 C22 112.0(3) . . ?
C22 C17 H17A 109.2 . . ?
C22 C17 H17B 109.2 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C19 C18 C17 110.8(3) . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
C18 C19 H19A 109.7 . . ?
C18 C19 H19B 109.7 . . ?
C18 C19 C20 109.9(3) . . ?
H19A C19 H19B 108.2 . . ?
C20 C19 H19A 109.7 . . ?
C20 C19 H19B 109.7 . . ?
C19 C20 H20A 109.2 . . ?
C19 C20 H20B 109.2 . . ?
C19 C20 C21 112.0(3) . . ?
H20A C20 H20B 107.9 . . ?
C21 C20 H20A 109.2 . . ?
C21 C20 H20B 109.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 C22 110.6(3) . . ?
H21A C21 H21B 108.1 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C13 C22 H22 106.4 . . ?
C17 C22 C13 112.3(3) . . ?
C17 C22 C21 109.3(3) . . ?
C17 C22 H22 106.4 . . ?
C21 C22 C13 115.3(3) . . ?
C21 C22 H22 106.4 . . ?
O6 C23 C14 111.0(3) . . ?
O7 C23 O6 123.8(4) . . ?
O7 C23 C14 125.2(3) . . ?
O6 C24 H24A 110.2 . . ?
O6 C24 H24B 110.2 . . ?
O6 C24 C30 107.4(3) . . ?
H24A C24 H24B 108.5 . . ?
C30 C24 H24A 110.2 . . ?
C30 C24 H24B 110.2 . . ?
C26 C25 H25 120.0 . . ?
C30 C25 H25 120.0 . . ?
C30 C25 C26 120.0(4) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 C25 120.2(4) . . ?
C27 C26 H26 119.9 . . ?
C26 C27 H27 120.0 . . ?
C26 C27 C28 120.1(4) . . ?
C28 C27 H27 120.0 . . ?
C27 C28 H28 119.9 . . ?
C27 C28 C29 120.1(4) . . ?
C29 C28 H28 119.9 . . ?
C28 C29 H29 119.9 . . ?
C28 C29 C30 120.3(4) . . ?
C30 C29 H29 119.9 . . ?
C25 C30 C24 121.7(3) . . ?
C25 C30 C29 119.4(3) . . ?
C29 C30 C24 119.0(3) . . ?
C14 C31 H31A 109.5 . . ?
C14 C31 H31B 109.5 . . ?
C14 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C13 C32 H32A 109.5 . . ?
C13 C32 H32B 109.5 . . ?
C13 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 35.3(4) . . . . ?
O1 C1 C2 C6 -70.2(3) . . . . ?
O1 C1 C2 C7 162.7(3) . . . . ?
O1 C4 C5 C6 -70.5(3) . . . . ?
O1 C4 C10 O3 30.5(4) . . . . ?
O1 C4 C10 O4 -153.0(4) . . . . ?
O2 C1 C2 C3 -147.6(4) . . . . ?
O2 C1 C2 C6 106.8(5) . . . . ?
O2 C1 C2 C7 -20.3(6) . . . . ?
O3 C11 C12 C13 -179.1(3) . . . . ?
O3 C11 C12 C16 -1.0(6) . . . . ?
O3 C11 C15 O5 7.4(6) . . . . ?
O3 C11 C15 C14 -172.0(3) . . . . ?
O6 C24 C30 C25 31.9(5) . . . . ?
O6 C24 C30 C29 -148.6(3) . . . . ?
C1 O1 C4 C3 -35.9(3) . . . . ?
C1 O1 C4 C5 74.2(3) . . . . ?
C1 O1 C4 C10 -160.1(3) . . . . ?
C1 C2 C3 C4 -51.9(3) . . . . ?
C1 C2 C3 C8 -169.3(3) . . . . ?
C1 C2 C3 C9 64.8(4) . . . . ?
C1 C2 C6 C5 67.9(3) . . . . ?
C2 C3 C4 O1 53.9(3) . . . . ?
C2 C3 C4 C5 -56.8(3) . . . . ?
C2 C3 C4 C10 174.0(3) . . . . ?
C3 C2 C6 C5 -34.8(4) . . . . ?
C3 C4 C5 C6 37.6(3) . . . . ?
C3 C4 C10 O3 -85.3(4) . . . . ?
C3 C4 C10 O4 91.2(5) . . . . ?
C4 O1 C1 O2 -177.6(3) . . . . ?
C4 O1 C1 C2 -0.2(4) . . . . ?
C4 C5 C6 C2 -1.0(4) . . . . ?
C5 C4 C10 O3 150.6(3) . . . . ?
C5 C4 C10 O4 -32.9(6) . . . . ?
C6 C2 C3 C4 54.2(3) . . . . ?
C6 C2 C3 C8 -63.3(4) . . . . ?
C6 C2 C3 C9 170.8(3) . . . . ?
C7 C2 C3 C4 -176.7(3) . . . . ?
C7 C2 C3 C8 65.8(5) . . . . ?
C7 C2 C3 C9 -60.1(5) . . . . ?
C7 C2 C6 C5 -165.6(3) . . . . ?
C8 C3 C4 O1 172.0(3) . . . . ?
C8 C3 C4 C5 61.3(4) . . . . ?
C8 C3 C4 C10 -67.9(4) . . . . ?
C9 C3 C4 O1 -61.9(4) . . . . ?
C9 C3 C4 C5 -172.6(3) . . . . ?
C9 C3 C4 C10 58.2(4) . . . . ?
C10 O3 C11 C12 104.8(4) . . . . ?
C10 O3 C11 C15 -76.5(4) . . . . ?
C10 C4 C5 C6 167.2(3) . . . . ?
C11 O3 C10 O4 -3.7(6) . . . . ?
C11 O3 C10 C4 172.8(3) . . . . ?
C11 C12 C13 C14 -9.7(4) . . . . ?
C11 C12 C13 C22 108.7(3) . . . . ?
C11 C12 C13 C32 -128.7(3) . . . . ?
C12 C11 C15 O5 -173.8(4) . . . . ?
C12 C11 C15 C14 6.8(4) . . . . ?
C12 C13 C14 C15 12.8(4) . . . . ?
C12 C13 C14 C23 -101.5(3) . . . . ?
C12 C13 C14 C31 136.5(3) . . . . ?
C12 C13 C22 C17 -37.1(4) . . . . ?
C12 C13 C22 C21 89.1(4) . . . . ?
C13 C14 C15 O5 168.5(4) . . . . ?
C13 C14 C15 C11 -12.1(4) . . . . ?
C13 C14 C23 O6 83.7(3) . . . . ?
C13 C14 C23 O7 -96.1(4) . . . . ?
C14 C13 C22 C17 76.1(4) . . . . ?
C14 C13 C22 C21 -157.8(3) . . . . ?
C15 C11 C12 C13 2.2(4) . . . . ?
C15 C11 C12 C16 -179.7(3) . . . . ?
C15 C14 C23 O6 -28.5(4) . . . . ?
C15 C14 C23 O7 151.7(4) . . . . ?
C16 C12 C13 C14 172.2(3) . . . . ?
C16 C12 C13 C22 -69.4(4) . . . . ?
C16 C12 C13 C32 53.2(5) . . . . ?
C17 C18 C19 C20 56.4(4) . . . . ?
C18 C17 C22 C13 -174.1(3) . . . . ?
C18 C17 C22 C21 56.6(4) . . . . ?
C18 C19 C20 C21 -56.8(4) . . . . ?
C19 C20 C21 C22 56.9(4) . . . . ?
C20 C21 C22 C13 177.0(3) . . . . ?
C20 C21 C22 C17 -55.4(4) . . . . ?
C22 C13 C14 C15 -105.1(3) . . . . ?
C22 C13 C14 C23 140.6(3) . . . . ?
C22 C13 C14 C31 18.5(4) . . . . ?
C22 C17 C18 C19 -57.7(4) . . . . ?
C23 O6 C24 C30 -160.9(3) . . . . ?
C23 C14 C15 O5 -75.3(4) . . . . ?
C23 C14 C15 C11 104.1(3) . . . . ?
C24 O6 C23 O7 -1.0(5) . . . . ?
C24 O6 C23 C14 179.2(3) . . . . ?
C25 C26 C27 C28 0.1(6) . . . . ?
C26 C25 C30 C24 179.9(3) . . . . ?
C26 C25 C30 C29 0.4(5) . . . . ?
C26 C27 C28 C29 1.1(6) . . . . ?
C27 C28 C29 C30 -1.6(6) . . . . ?
C28 C29 C30 C24 -178.7(3) . . . . ?
C28 C29 C30 C25 0.8(6) . . . . ?
C30 C25 C26 C27 -0.9(6) . . . . ?
C31 C14 C15 O5 41.0(5) . . . . ?
C31 C14 C15 C11 -139.6(3) . . . . ?
C31 C14 C23 O6 -148.0(3) . . . . ?
C31 C14 C23 O7 32.2(5) . . . . ?
C32 C13 C14 C15 130.5(3) . . . . ?
C32 C13 C14 C23 16.2(4) . . . . ?
C32 C13 C14 C31 -105.9(4) . . . . ?
C32 C13 C22 C17 -159.1(3) . . . . ?
C32 C13 C22 C21 -32.9(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# 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_tius006
_database_code_depnum_ccdc_archive 'CCDC 2154235'
loop_
_audit_author_name
_audit_author_address
'Glenn P. A. Yap'
;University of Delaware
United States of America
;
_audit_update_record             
;
2022-02-23 deposited with the CCDC.	2023-05-29 downloaded from the CCDC.
;
_audit_creation_date             2022-02-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H38 O7'
_chemical_formula_sum            'C31 H38 O7'
_chemical_formula_weight         522.61
_chemical_absolute_configuration rmad
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   6.4651(2)
_cell_length_b                   9.9755(3)
_cell_length_c                   41.8034(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2696.01(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      66.60
_cell_measurement_theta_min      4.23
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.821
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1176 before and 0.0534 after correction.
The Ratio of minimum to maximum transmission is 0.7928.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1120
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3.00 1.00 -2.00 0.1330
0.00 -1.00 -3.00 0.0210
0.00 1.00 3.00 0.0150
0.00 3.00 -1.00 0.0090
0.00 0.00 -1.00 0.0160
0.00 0.00 1.00 0.0200
0.00 -2.00 3.00 0.0130
2.00 -1.00 2.00 0.1150

_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.026
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            26912
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         2.114
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.702
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                4620
_reflns_number_total             4722
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.129
_refine_diff_density_min         -0.160
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details 
;
 Flack x determined using 1857 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4722
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0285
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0299P)²+0.6971P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0704
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.57724(19) 0.76058(13) 0.71059(3) 0.0198(3) Uani 1 1 d . . . . .
O2 O 0.6510(2) 0.67258(14) 0.75864(3) 0.0279(3) Uani 1 1 d . . . . .
O3 O 0.6190(2) 0.74622(14) 0.64740(3) 0.0224(3) Uani 1 1 d . . . . .
O4 O 0.3218(3) 0.8574(2) 0.64010(4) 0.0559(6) Uani 1 1 d . . . . .
O5 O 0.4128(2) 0.58298(16) 0.59894(4) 0.0343(4) Uani 1 1 d . . . . .
O6 O 0.8595(2) 0.51622(14) 0.58210(3) 0.0266(3) Uani 1 1 d . . . . .
O7 O 0.8945(3) 0.55327(17) 0.52967(4) 0.0484(5) Uani 1 1 d . . . . .
C1 C 0.5268(3) 0.69036(19) 0.73757(5) 0.0206(4) Uani 1 1 d . . . . .
C2 C 0.3009(3) 0.65187(19) 0.73521(5) 0.0211(4) Uani 1 1 d . . . . .
C3 C 0.2885(3) 0.62753(19) 0.69836(5) 0.0217(4) Uani 1 1 d . . . . .
C4 C 0.3870(3) 0.7661(2) 0.69152(4) 0.0207(4) Uani 1 1 d . . . . .
C5 C 0.2454(3) 0.86669(19) 0.70838(5) 0.0231(4) Uani 1 1 d . . . . .
H5A H 0.121285 0.887019 0.695377 0.028 Uiso 1 1 calc R U . . .
H5B H 0.319136 0.951157 0.713324 0.028 Uiso 1 1 calc R U . . .
C6 C 0.1882(3) 0.78935(19) 0.73918(5) 0.0232(4) Uani 1 1 d . . . . .
H6A H 0.036730 0.776837 0.740861 0.028 Uiso 1 1 calc R U . . .
H6B H 0.238127 0.837260 0.758434 0.028 Uiso 1 1 calc R U . . .
C7 C 0.2322(3) 0.5424(2) 0.75751(5) 0.0290(5) Uani 1 1 d . . . . .
H7A H 0.297387 0.457684 0.751241 0.043 Uiso 1 1 calc R U . . .
H7B H 0.081445 0.533078 0.756392 0.043 Uiso 1 1 calc R U . . .
H7C H 0.272855 0.565021 0.779438 0.043 Uiso 1 1 calc R U . . .
C8 C 0.0689(3) 0.6119(2) 0.68506(5) 0.0314(5) Uani 1 1 d . . . . .
H8A H -0.019551 0.683039 0.693675 0.047 Uiso 1 1 calc R U . . .
H8B H 0.013316 0.524338 0.691326 0.047 Uiso 1 1 calc R U . . .
H8C H 0.072474 0.618278 0.661673 0.047 Uiso 1 1 calc R U . . .
C9 C 0.4209(3) 0.5091(2) 0.68725(5) 0.0267(5) Uani 1 1 d . . . . .
H9A H 0.417323 0.503528 0.663853 0.040 Uiso 1 1 calc R U . . .
H9B H 0.366263 0.425905 0.696412 0.040 Uiso 1 1 calc R U . . .
H9C H 0.563929 0.522097 0.694379 0.040 Uiso 1 1 calc R U . . .
C10 C 0.4360(3) 0.7975(2) 0.65732(5) 0.0258(4) Uani 1 1 d . . . . .
C11 C 0.6501(3) 0.75545(19) 0.61440(4) 0.0207(4) Uani 1 1 d . . . . .
C12 C 0.7737(3) 0.84278(19) 0.59983(4) 0.0203(4) Uani 1 1 d . . . . .
C13 C 0.7627(3) 0.82458(19) 0.56376(4) 0.0207(4) Uani 1 1 d . . . . .
H13 H 0.906616 0.815387 0.555266 0.025 Uiso 1 1 calc R U . . .
C14 C 0.6478(3) 0.68598(19) 0.55975(4) 0.0229(4) Uani 1 1 d . . . . .
C15 C 0.5480(3) 0.6633(2) 0.59250(5) 0.0237(4) Uani 1 1 d . . . . .
C16 C 0.8982(3) 0.9482(2) 0.61609(5) 0.0266(4) Uani 1 1 d . . . . .
H16A H 0.832711 1.035798 0.612878 0.040 Uiso 1 1 calc R U . . .
H16B H 1.038101 0.949637 0.607063 0.040 Uiso 1 1 calc R U . . .
H16C H 0.905859 0.928684 0.639036 0.040 Uiso 1 1 calc R U . . .
C17 C 0.4654(3) 0.9973(2) 0.56474(5) 0.0211(4) Uani 1 1 d . . . . .
H17A H 0.361924 0.924514 0.566451 0.025 Uiso 1 1 calc R U . . .
H17B H 0.505928 1.023871 0.586682 0.025 Uiso 1 1 calc R U . . .
C18 C 0.3678(3) 1.1176(2) 0.54771(5) 0.0239(4) Uani 1 1 d . . . . .
H18A H 0.314783 1.089206 0.526556 0.029 Uiso 1 1 calc R U . . .
H18B H 0.249623 1.151274 0.560449 0.029 Uiso 1 1 calc R U . . .
C19 C 0.5259(3) 1.2296(2) 0.54331(5) 0.0252(4) Uani 1 1 d . . . . .
H19A H 0.574161 1.261297 0.564468 0.030 Uiso 1 1 calc R U . . .
H19B H 0.460925 1.306039 0.532043 0.030 Uiso 1 1 calc R U . . .
C20 C 0.7094(3) 1.1779(2) 0.52392(5) 0.0248(4) Uani 1 1 d . . . . .
H20A H 0.661493 1.149735 0.502447 0.030 Uiso 1 1 calc R U . . .
H20B H 0.811773 1.250719 0.521128 0.030 Uiso 1 1 calc R U . . .
C21 C 0.8115(3) 1.0593(2) 0.54077(5) 0.0224(4) Uani 1 1 d . . . . .
H21A H 0.869684 1.089583 0.561447 0.027 Uiso 1 1 calc R U . . .
H21B H 0.926824 1.025408 0.527459 0.027 Uiso 1 1 calc R U . . .
C22 C 0.6563(3) 0.94531(19) 0.54679(4) 0.0200(4) Uani 1 1 d . . . . .
H22 H 0.608108 0.912989 0.525404 0.024 Uiso 1 1 calc R U . . .
C23 C 0.8135(3) 0.57837(19) 0.55486(5) 0.0256(4) Uani 1 1 d . . . . .
C24 C 1.0133(3) 0.4106(2) 0.58093(5) 0.0247(4) Uani 1 1 d . . . . .
H24A H 1.151353 0.449012 0.576352 0.030 Uiso 1 1 calc R U . . .
H24B H 0.978691 0.345834 0.563807 0.030 Uiso 1 1 calc R U . . .
C25 C 0.8393(3) 0.3349(2) 0.63220(5) 0.0254(4) Uani 1 1 d . . . . .
H25 H 0.713942 0.375521 0.625387 0.030 Uiso 1 1 calc R U . . .
C26 C 0.8478(3) 0.2688(2) 0.66152(5) 0.0277(4) Uani 1 1 d . . . . .
H26 H 0.728341 0.265420 0.674722 0.033 Uiso 1 1 calc R U . . .
C27 C 1.0292(3) 0.2078(2) 0.67160(5) 0.0285(5) Uani 1 1 d . . . . .
H27 H 1.034315 0.162819 0.691620 0.034 Uiso 1 1 calc R U . . .
C28 C 1.2030(3) 0.2129(2) 0.65224(5) 0.0291(5) Uani 1 1 d . . . . .
H28 H 1.327042 0.169974 0.658823 0.035 Uiso 1 1 calc R U . . .
C29 C 1.1964(3) 0.2804(2) 0.62337(5) 0.0261(4) Uani 1 1 d . . . . .
H29 H 1.317369 0.285242 0.610514 0.031 Uiso 1 1 calc R U . . .
C30 C 1.0145(3) 0.34156(19) 0.61287(5) 0.0228(4) Uani 1 1 d . . . . .
C31 C 0.4908(4) 0.6736(2) 0.53236(5) 0.0298(5) Uani 1 1 d . . . . .
H31A H 0.561647 0.685920 0.511850 0.045 Uiso 1 1 calc R U . . .
H31B H 0.383751 0.742476 0.534795 0.045 Uiso 1 1 calc R U . . .
H31C H 0.426640 0.584663 0.532963 0.045 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
O1 C1 1.367(2) . ?
O1 C4 1.467(2) . ?
O2 C1 1.205(2) . ?
O3 C10 1.353(2) . ?
O3 C11 1.397(2) . ?
O4 C10 1.192(3) . ?
O5 C15 1.216(3) . ?
O6 C23 1.330(2) . ?
O6 C24 1.449(2) . ?
O7 C23 1.202(3) . ?
C1 C2 1.513(3) . ?
C2 C3 1.561(3) . ?
C2 C6 1.562(3) . ?
C2 C7 1.503(3) . ?
C3 C4 1.548(3) . ?
C3 C8 1.533(3) . ?
C3 C9 1.531(3) . ?
C4 C5 1.530(3) . ?
C4 C10 1.498(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.546(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C11 C12 1.329(3) . ?
C11 C15 1.456(3) . ?
C12 C13 1.520(3) . ?
C12 C16 1.489(3) . ?
C13 H13 1.0000 . ?
C13 C14 1.579(3) . ?
C13 C22 1.558(3) . ?
C14 C15 1.530(3) . ?
C14 C23 1.530(3) . ?
C14 C31 1.535(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.531(3) . ?
C17 C22 1.535(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.525(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.527(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.527(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.537(3) . ?
C22 H22 1.0000 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C30 1.503(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.393(3) . ?
C25 C30 1.393(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.387(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.386(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.382(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.396(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 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
C1 O1 C4 105.52(14) . . ?
C10 O3 C11 113.80(15) . . ?
C23 O6 C24 117.59(15) . . ?
O1 C1 C2 107.84(16) . . ?
O2 C1 O1 121.33(18) . . ?
O2 C1 C2 130.77(18) . . ?
C1 C2 C3 98.82(15) . . ?
C1 C2 C6 102.74(15) . . ?
C3 C2 C6 102.56(15) . . ?
C7 C2 C1 115.43(17) . . ?
C7 C2 C3 118.92(17) . . ?
C7 C2 C6 115.73(16) . . ?
C4 C3 C2 91.28(14) . . ?
C8 C3 C2 114.93(16) . . ?
C8 C3 C4 113.87(17) . . ?
C9 C3 C2 112.98(16) . . ?
C9 C3 C4 113.75(16) . . ?
C9 C3 C8 109.23(16) . . ?
O1 C4 C3 102.18(14) . . ?
O1 C4 C5 106.01(15) . . ?
O1 C4 C10 110.43(15) . . ?
C5 C4 C3 104.74(15) . . ?
C10 C4 C3 116.75(16) . . ?
C10 C4 C5 115.43(16) . . ?
C4 C5 H5A 111.5 . . ?
C4 C5 H5B 111.5 . . ?
C4 C5 C6 101.49(15) . . ?
H5A C5 H5B 109.3 . . ?
C6 C5 H5A 111.5 . . ?
C6 C5 H5B 111.5 . . ?
C2 C6 H6A 111.0 . . ?
C2 C6 H6B 111.0 . . ?
C5 C6 C2 103.79(15) . . ?
C5 C6 H6A 111.0 . . ?
C5 C6 H6B 111.0 . . ?
H6A C6 H6B 109.0 . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C9 H9A 109.5 . . ?
C3 C9 H9B 109.5 . . ?
C3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 C4 113.48(16) . . ?
O4 C10 O3 123.10(19) . . ?
O4 C10 C4 123.36(18) . . ?
O3 C11 C15 120.92(17) . . ?
C12 C11 O3 125.59(17) . . ?
C12 C11 C15 113.47(17) . . ?
C11 C12 C13 110.37(17) . . ?
C11 C12 C16 125.37(18) . . ?
C16 C12 C13 124.21(17) . . ?
C12 C13 H13 108.7 . . ?
C12 C13 C14 103.41(15) . . ?
C12 C13 C22 112.33(15) . . ?
C14 C13 H13 108.7 . . ?
C22 C13 H13 108.7 . . ?
C22 C13 C14 114.87(15) . . ?
C15 C14 C13 103.46(15) . . ?
C15 C14 C23 108.10(16) . . ?
C15 C14 C31 112.14(17) . . ?
C23 C14 C13 107.39(16) . . ?
C23 C14 C31 107.89(16) . . ?
C31 C14 C13 117.45(16) . . ?
O5 C15 C11 127.08(19) . . ?
O5 C15 C14 126.76(18) . . ?
C11 C15 C14 106.15(16) . . ?
C12 C16 H16A 109.5 . . ?
C12 C16 H16B 109.5 . . ?
C12 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
H17A C17 H17B 108.0 . . ?
C18 C17 H17A 109.3 . . ?
C18 C17 H17B 109.3 . . ?
C18 C17 C22 111.65(16) . . ?
C22 C17 H17A 109.3 . . ?
C22 C17 H17B 109.3 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C19 C18 C17 110.73(16) . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
C18 C19 H19A 109.7 . . ?
C18 C19 H19B 109.7 . . ?
C18 C19 C20 109.72(17) . . ?
H19A C19 H19B 108.2 . . ?
C20 C19 H19A 109.7 . . ?
C20 C19 H19B 109.7 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
C21 C20 C19 110.65(16) . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
C20 C21 H21A 109.3 . . ?
C20 C21 H21B 109.3 . . ?
C20 C21 C22 111.50(16) . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 H21A 109.3 . . ?
C22 C21 H21B 109.3 . . ?
C13 C22 H22 107.2 . . ?
C17 C22 C13 113.19(15) . . ?
C17 C22 C21 110.77(16) . . ?
C17 C22 H22 107.2 . . ?
C21 C22 C13 110.99(15) . . ?
C21 C22 H22 107.2 . . ?
O6 C23 C14 111.66(16) . . ?
O7 C23 O6 123.7(2) . . ?
O7 C23 C14 124.62(19) . . ?
O6 C24 H24A 110.1 . . ?
O6 C24 H24B 110.1 . . ?
O6 C24 C30 107.88(15) . . ?
H24A C24 H24B 108.4 . . ?
C30 C24 H24A 110.1 . . ?
C30 C24 H24B 110.1 . . ?
C26 C25 H25 120.0 . . ?
C30 C25 H25 120.0 . . ?
C30 C25 C26 120.06(19) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 C25 120.57(19) . . ?
C27 C26 H26 119.7 . . ?
C26 C27 H27 120.3 . . ?
C28 C27 C26 119.46(19) . . ?
C28 C27 H27 120.3 . . ?
C27 C28 H28 119.9 . . ?
C29 C28 C27 120.2(2) . . ?
C29 C28 H28 119.9 . . ?
C28 C29 H29 119.6 . . ?
C28 C29 C30 120.89(19) . . ?
C30 C29 H29 119.6 . . ?
C25 C30 C24 122.21(19) . . ?
C25 C30 C29 118.80(18) . . ?
C29 C30 C24 118.99(18) . . ?
C14 C31 H31A 109.5 . . ?
C14 C31 H31B 109.5 . . ?
C14 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 35.18(18) . . . . ?
O1 C1 C2 C6 -69.93(18) . . . . ?
O1 C1 C2 C7 163.18(16) . . . . ?
O1 C4 C5 C6 -69.75(17) . . . . ?
O1 C4 C10 O3 33.2(2) . . . . ?
O1 C4 C10 O4 -149.6(2) . . . . ?
O2 C1 C2 C3 -147.7(2) . . . . ?
O2 C1 C2 C6 107.2(2) . . . . ?
O2 C1 C2 C7 -19.7(3) . . . . ?
O3 C11 C12 C13 -178.48(17) . . . . ?
O3 C11 C12 C16 -1.2(3) . . . . ?
O3 C11 C15 O5 9.2(3) . . . . ?
O3 C11 C15 C14 -169.82(16) . . . . ?
O6 C24 C30 C25 28.7(2) . . . . ?
O6 C24 C30 C29 -152.17(17) . . . . ?
C1 O1 C4 C3 -35.76(17) . . . . ?
C1 O1 C4 C5 73.67(17) . . . . ?
C1 O1 C4 C10 -160.63(16) . . . . ?
C1 C2 C3 C4 -51.52(15) . . . . ?
C1 C2 C3 C8 -168.70(17) . . . . ?
C1 C2 C3 C9 65.03(19) . . . . ?
C1 C2 C6 C5 67.96(18) . . . . ?
C2 C3 C4 O1 53.72(15) . . . . ?
C2 C3 C4 C5 -56.67(16) . . . . ?
C2 C3 C4 C10 174.30(16) . . . . ?
C3 C2 C6 C5 -34.25(19) . . . . ?
C3 C4 C5 C6 37.85(18) . . . . ?
C3 C4 C10 O3 -82.9(2) . . . . ?
C3 C4 C10 O4 94.4(3) . . . . ?
C4 O1 C1 O2 -177.57(18) . . . . ?
C4 O1 C1 C2 -0.12(18) . . . . ?
C4 C5 C6 C2 -1.64(19) . . . . ?
C5 C4 C10 O3 153.35(17) . . . . ?
C5 C4 C10 O4 -29.4(3) . . . . ?
C6 C2 C3 C4 53.73(16) . . . . ?
C6 C2 C3 C8 -63.4(2) . . . . ?
C6 C2 C3 C9 170.29(16) . . . . ?
C7 C2 C3 C4 -177.13(17) . . . . ?
C7 C2 C3 C8 65.7(2) . . . . ?
C7 C2 C3 C9 -60.6(2) . . . . ?
C7 C2 C6 C5 -165.34(17) . . . . ?
C8 C3 C4 O1 171.81(15) . . . . ?
C8 C3 C4 C5 61.4(2) . . . . ?
C8 C3 C4 C10 -67.6(2) . . . . ?
C9 C3 C4 O1 -62.15(19) . . . . ?
C9 C3 C4 C5 -172.55(16) . . . . ?
C9 C3 C4 C10 58.4(2) . . . . ?
C10 O3 C11 C12 104.2(2) . . . . ?
C10 O3 C11 C15 -77.3(2) . . . . ?
C10 C4 C5 C6 167.67(17) . . . . ?
C11 O3 C10 O4 -7.4(3) . . . . ?
C11 O3 C10 C4 169.88(17) . . . . ?
C11 C12 C13 C14 -12.9(2) . . . . ?
C11 C12 C13 C22 111.49(18) . . . . ?
C12 C11 C15 O5 -172.1(2) . . . . ?
C12 C11 C15 C14 8.8(2) . . . . ?
C12 C13 C14 C15 17.11(18) . . . . ?
C12 C13 C14 C23 -97.08(17) . . . . ?
C12 C13 C14 C31 141.23(17) . . . . ?
C12 C13 C22 C17 -41.4(2) . . . . ?
C12 C13 C22 C21 83.85(19) . . . . ?
C13 C14 C15 O5 165.0(2) . . . . ?
C13 C14 C15 C11 -15.93(19) . . . . ?
C13 C14 C23 O6 96.57(19) . . . . ?
C13 C14 C23 O7 -82.7(3) . . . . ?
C14 C13 C22 C17 76.4(2) . . . . ?
C14 C13 C22 C21 -158.32(15) . . . . ?
C15 C11 C12 C13 2.9(2) . . . . ?
C15 C11 C12 C16 -179.75(18) . . . . ?
C15 C14 C23 O6 -14.5(2) . . . . ?
C15 C14 C23 O7 166.2(2) . . . . ?
C16 C12 C13 C14 169.72(17) . . . . ?
C16 C12 C13 C22 -65.9(2) . . . . ?
C17 C18 C19 C20 58.7(2) . . . . ?
C18 C17 C22 C13 178.82(15) . . . . ?
C18 C17 C22 C21 53.4(2) . . . . ?
C18 C19 C20 C21 -59.1(2) . . . . ?
C19 C20 C21 C22 57.1(2) . . . . ?
C20 C21 C22 C13 179.58(15) . . . . ?
C20 C21 C22 C17 -53.8(2) . . . . ?
C22 C13 C14 C15 -105.65(18) . . . . ?
C22 C13 C14 C23 140.16(16) . . . . ?
C22 C13 C14 C31 18.5(2) . . . . ?
C22 C17 C18 C19 -56.4(2) . . . . ?
C23 O6 C24 C30 -171.16(17) . . . . ?
C23 C14 C15 O5 -81.3(3) . . . . ?
C23 C14 C15 C11 97.75(18) . . . . ?
C24 O6 C23 O7 -1.3(3) . . . . ?
C24 O6 C23 C14 179.42(16) . . . . ?
C25 C26 C27 C28 0.0(3) . . . . ?
C26 C25 C30 C24 179.49(18) . . . . ?
C26 C25 C30 C29 0.3(3) . . . . ?
C26 C27 C28 C29 1.1(3) . . . . ?
C27 C28 C29 C30 -1.5(3) . . . . ?
C28 C29 C30 C24 -178.40(18) . . . . ?
C28 C29 C30 C25 0.8(3) . . . . ?
C30 C25 C26 C27 -0.7(3) . . . . ?
C31 C14 C15 O5 37.5(3) . . . . ?
C31 C14 C15 C11 -143.45(17) . . . . ?
C31 C14 C23 O6 -135.94(18) . . . . ?
C31 C14 C23 O7 44.8(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
