# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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. 
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data_20221209-lqy-2
_database_code_depnum_ccdc_archive 'CCDC 2308124'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2023-11-15 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2023-10-13
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C51 H46 O, C2 H3 Cl3'
_chemical_formula_sum            'C53 H49 Cl3 O'
_chemical_formula_weight         808.27
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHOCl
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'
Cl Cl 0.3639 0.7018 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   18.7443(6)
_cell_length_b                   10.4995(3)
_cell_length_c                   24.1927(8)
_cell_angle_alpha                90
_cell_angle_beta                 110.663(4)
_cell_angle_gamma                90
_cell_volume                     4455.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13022
_cell_measurement_temperature    302.33(10)
_cell_measurement_theta_max      75.7010
_cell_measurement_theta_min      2.5150
_shelx_estimated_absorpt_T_max   0.882
_shelx_estimated_absorpt_T_min   0.279
_exptl_absorpt_coefficient_mu    2.139
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28798
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.590
_diffrn_reflns_theta_max         66.590
_diffrn_reflns_theta_min         2.586
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      302.33(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     54.00 102.00   0.50    0.30    --   62.89  15.00 150.00   96
  2  ω     55.00 104.00   0.50    0.30    --   62.89  15.00  90.00   98
  3  ω     82.00 108.00   0.50    0.30    --   72.93  15.00 -60.00   52
  4  ω     66.00 120.00   0.50    0.30    --   76.75  15.00   0.00  108
  5  ω     62.00 113.00   0.50    0.30    --   72.93  15.00-120.00  102
  6  ω     62.00  87.00   0.50    0.30    --   72.93  15.00-180.00   50
  7  ω   -122.00 -72.00   0.50    0.30    --  -81.49 -15.00  90.00  100
  8  ω   -103.00 -66.00   0.50    0.30    --  -63.72 -15.00 120.00   74
  9  ω   -100.00 -72.00   0.50    0.30    --  -63.72 -15.00-120.00   56
 10  ω    -98.00 -67.00   0.50    0.30    --  -63.72 -15.00-180.00   62
 11  ω   -115.00 -69.00   0.50    0.30    --  -76.43 -15.00-150.00   92
 12  ω   -123.00 -84.00   0.50    0.30    --  -81.49 -15.00-180.00   78
 13  ω   -115.00 -66.00   0.50    0.30    --  -76.43 -15.00 -30.00   98
 14  ω   -125.00 -81.00   0.50    0.30    --  -81.49 -15.00  30.00   88
 15  ω    -95.00 -36.00   0.50    0.30    --  -76.43 125.00 -60.00  118
 16  ω   -101.00 -44.00   0.50    0.30    --  -81.49 125.00   0.00  114
 17  ω     39.00  68.00   0.50    0.30    --   72.93-125.00-180.00   58
 18  ω     67.00  93.00   0.50    0.30    --   76.75-125.00-180.00   52
 19  ω     35.00  81.00   0.50    0.30    --   76.75-125.00 120.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0792509000
_diffrn_orient_matrix_UB_12      -0.0295315000
_diffrn_orient_matrix_UB_13      -0.0459095000
_diffrn_orient_matrix_UB_21      0.0377823000
_diffrn_orient_matrix_UB_22      -0.0585924000
_diffrn_orient_matrix_UB_23      -0.0412381000
_diffrn_orient_matrix_UB_31      0.0010325000
_diffrn_orient_matrix_UB_32      -0.1312673000
_diffrn_orient_matrix_UB_33      0.0287424000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6149
_reflns_number_total             7860
_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       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         7860
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0832
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1736P)²+1.7364P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2708
_refine_ls_wR_factor_ref         0.2840
_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. Restrained distances
 C4-C2
 1.54 with sigma of 0.01
 Cl3-C2 = Cl2-C4 = Cl1-C4
 1.78 with sigma of 0.01
 Cl1-C4 \\sim Cl1A-C4A
 with sigma of 0.02
 Cl2-C2 \\sim Cl2A-C2A
 with sigma of 0.04
 Cl3-C4 \\sim Cl3A-C4A
 with sigma of 0.04
 Cl3-C2 \\sim Cl3A-C2A
 with sigma of 0.02
 Cl2-C4 \\sim Cl2A-C4A
 with sigma of 0.02
 C4-C2 \\sim C4A-C2A
 with sigma of 0.02
 Cl1-Cl2 \\sim Cl1A-Cl2A
 with sigma of 0.04
 Cl1-C2 \\sim Cl1A-C2A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(Cl1)
\\sim Ueq, Uanis(Cl3) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(Cl3A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(Cl2A)
\\sim Ueq, Uanis(Cl1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Sof(C4A)=Sof(H4A)=Sof(Cl2A)=Sof(Cl1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(Cl3A)=
 1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=Sof(C4)=Sof(H4)=Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C4A(H4A)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C2A(H2AA,H2AB)
5.c Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00C(H00C), C00J(H00J), C00K(H00K), C00M(H00M), C00O(H00O),
 C00Q(H00Q), C00U(H00U), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010),
 C011(H011), C012(H012), C013(H013), C014(H014), C015(H015), C017(H017),
 C01A(H01G), C01B(H01H), C01C(H01I), C01D(H01J)
5.d Idealised Me refined as rotating group:
 C016(H01A,H01B,H01C), C018(H01D,H01E,H01F), C01E(H01K,H01L,H01M), C01F(H01N,
 H01O,H01P), C01G(H01Q,H01R,H01S), C01H(H01T,H01U,H01V), C01I(H01W,H01X,H01Y),
 C01J(H01Z,H,HA)
;
_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
O001 O 0.63940(9) 0.61768(17) 0.31149(7) 0.0514(5) Uani 1 1 d . . . . .
C002 C 0.71632(13) 0.6195(2) 0.32061(10) 0.0428(5) Uani 1 1 d . . . . .
C003 C 0.58818(13) 0.6206(2) 0.25459(10) 0.0442(5) Uani 1 1 d . . . . .
C004 C 0.73096(12) 0.6118(2) 0.42792(9) 0.0433(5) Uani 1 1 d . . . . .
C005 C 0.76358(13) 0.6170(2) 0.37964(10) 0.0444(5) Uani 1 1 d . . . . .
C006 C 0.74429(13) 0.6245(2) 0.27455(10) 0.0442(5) Uani 1 1 d . . . . .
C007 C 0.51213(13) 0.6186(2) 0.25048(10) 0.0474(6) Uani 1 1 d . . . . .
C008 C 0.73626(13) 0.4984(2) 0.46035(10) 0.0461(5) Uani 1 1 d . . . . .
C009 C 0.60868(14) 0.6253(2) 0.20519(10) 0.0462(5) Uani 1 1 d . . . . .
C00A C 0.69593(12) 0.7199(2) 0.44131(10) 0.0450(5) Uani 1 1 d . . . . .
C00B C 0.84190(14) 0.6178(2) 0.39265(11) 0.0499(6) Uani 1 1 d . . . . .
H00B H 0.874197 0.615235 0.431945 0.060 Uiso 1 1 calc R U . . .
C00C C 0.82316(14) 0.6257(2) 0.29028(11) 0.0490(6) Uani 1 1 d . . . . .
H00C H 0.843282 0.628968 0.260245 0.059 Uiso 1 1 calc R U . . .
C00D C 0.87357(14) 0.6223(2) 0.34826(11) 0.0497(6) Uani 1 1 d . . . . .
C00E C 0.49356(13) 0.6106(2) 0.30560(11) 0.0495(6) Uani 1 1 d . . . . .
C00F C 0.66705(14) 0.7147(2) 0.48861(11) 0.0515(6) Uani 1 1 d . . . . .
C00G C 0.69203(14) 0.6279(2) 0.20983(10) 0.0517(6) Uani 1 1 d . . . . .
C00H C 0.70763(15) 0.4951(2) 0.50796(11) 0.0531(6) Uani 1 1 d . . . . .
C00I C 0.46789(14) 0.7178(3) 0.32716(12) 0.0569(6) Uani 1 1 d . . . . .
C00J C 0.67405(15) 0.6030(3) 0.52086(11) 0.0561(6) Uani 1 1 d . . . . .
H00J H 0.655710 0.600614 0.551896 0.067 Uiso 1 1 calc R U . . .
C00K C 0.45625(14) 0.6218(2) 0.19487(12) 0.0548(6) Uani 1 1 d . . . . .
H00K H 0.405344 0.620341 0.191694 0.066 Uiso 1 1 calc R U . . .
C00L C 0.50455(14) 0.4938(3) 0.33648(11) 0.0544(6) Uani 1 1 d . . . . .
C00M C 0.54988(15) 0.6280(2) 0.15015(11) 0.0518(6) Uani 1 1 d . . . . .
H00M H 0.562789 0.630690 0.116413 0.062 Uiso 1 1 calc R U . . .
C00N C 0.47361(15) 0.6270(2) 0.14335(11) 0.0552(6) Uani 1 1 d . . . . .
C00O C 0.69024(16) 0.8376(3) 0.41102(12) 0.0604(7) Uani 1 1 d . . . . .
H00O H 0.709433 0.844246 0.380542 0.073 Uiso 1 1 calc R U . . .
C00Q C 0.76851(18) 0.3845(3) 0.44779(13) 0.0638(7) Uani 1 1 d . . . . .
H00Q H 0.787096 0.383940 0.416868 0.077 Uiso 1 1 calc R U . . .
C00S C 0.48707(15) 0.4845(3) 0.38937(12) 0.0637(7) Uani 1 1 d . . . . .
C00T C 0.44997(16) 0.7061(3) 0.38056(14) 0.0683(8) Uani 1 1 d . . . . .
C00U C 0.53171(18) 0.3828(3) 0.31733(15) 0.0691(8) Uani 1 1 d . . . . .
H00U H 0.542546 0.386171 0.282695 0.083 Uiso 1 1 calc R U . . .
C00V C 0.95986(15) 0.6258(3) 0.36184(13) 0.0634(7) Uani 1 1 d . . . . .
C00W C 0.40991(17) 0.6359(3) 0.08235(12) 0.0688(8) Uani 1 1 d . . . . .
C00X C 0.46002(18) 0.5902(4) 0.40969(13) 0.0733(8) Uani 1 1 d . . . . .
H00X H 0.448227 0.583391 0.443831 0.088 Uiso 1 1 calc R U . . .
C00Y C 0.7155(2) 0.3797(3) 0.54099(14) 0.0709(8) Uani 1 1 d . . . . .
H00Y H 0.698588 0.377260 0.572758 0.085 Uiso 1 1 calc R U . . .
C00Z C 0.63292(18) 0.8261(3) 0.50238(14) 0.0681(8) Uani 1 1 d . . . . .
H00Z H 0.613581 0.823244 0.532860 0.082 Uiso 1 1 calc R U . . .
C010 C 0.45995(19) 0.8392(3) 0.29986(16) 0.0747(8) Uani 1 1 d . . . . .
H010 H 0.471757 0.849089 0.265861 0.090 Uiso 1 1 calc R U . . .
C011 C 0.4985(2) 0.3646(4) 0.41944(15) 0.0848(10) Uani 1 1 d . . . . .
H011 H 0.487277 0.357322 0.453818 0.102 Uiso 1 1 calc R U . . .
C012 C 0.6571(2) 0.9405(3) 0.42606(15) 0.0774(9) Uani 1 1 d . . . . .
H012 H 0.653519 1.016243 0.405357 0.093 Uiso 1 1 calc R U . . .
C013 C 0.7730(2) 0.2770(3) 0.47941(16) 0.0816(10) Uani 1 1 d . . . . .
H013 H 0.793499 0.203584 0.469467 0.098 Uiso 1 1 calc R U . . .
C014 C 0.6282(2) 0.9349(3) 0.47212(16) 0.0800(9) Uani 1 1 d . . . . .
H014 H 0.605844 1.006485 0.481722 0.096 Uiso 1 1 calc R U . . .
C015 C 0.7469(2) 0.2747(3) 0.52730(16) 0.0842(10) Uani 1 1 d . . . . .
H015 H 0.751314 0.200784 0.549421 0.101 Uiso 1 1 calc R U . . .
C016 C 0.70847(19) 0.5114(4) 0.17793(15) 0.0905(12) Uani 1 1 d . . . . .
H01A H 0.677917 0.515622 0.136702 0.136 Uiso 1 1 calc R U . . .
H01B H 0.696315 0.435114 0.194649 0.136 Uiso 1 1 calc R U . . .
H01C H 0.761459 0.510474 0.182476 0.136 Uiso 1 1 calc R U . . .
C017 C 0.4232(2) 0.8163(4) 0.4017(2) 0.0938(12) Uani 1 1 d . . . . .
H017 H 0.410321 0.809810 0.435350 0.113 Uiso 1 1 calc R U . . .
C018 C 0.7064(2) 0.7516(4) 0.18147(15) 0.0920(12) Uani 1 1 d . . . . .
H01D H 0.758747 0.754599 0.184164 0.138 Uiso 1 1 calc R U . . .
H01E H 0.695715 0.823435 0.201837 0.138 Uiso 1 1 calc R U . . .
H01F H 0.673841 0.754112 0.140699 0.138 Uiso 1 1 calc R U . . .
C01A C 0.5425(3) 0.2715(4) 0.34765(18) 0.0944(11) Uani 1 1 d . . . . .
H01G H 0.561638 0.201025 0.334189 0.113 Uiso 1 1 calc R U . . .
C01B C 0.4161(3) 0.9273(5) 0.3746(2) 0.1054(14) Uani 1 1 d . . . . .
H01H H 0.398444 0.997415 0.389490 0.126 Uiso 1 1 calc R U . . .
C01C C 0.4353(2) 0.9409(4) 0.3227(2) 0.0987(12) Uani 1 1 d . . . . .
H01I H 0.430921 1.020072 0.304570 0.118 Uiso 1 1 calc R U . . .
C01D C 0.5249(3) 0.2626(4) 0.39937(19) 0.1012(13) Uani 1 1 d . . . . .
H01J H 0.531587 0.185785 0.419716 0.121 Uiso 1 1 calc R U . . .
C01E C 1.0050(2) 0.5948(6) 0.42585(17) 0.1155(17) Uani 1 1 d . . . . .
H01K H 0.997142 0.660415 0.450753 0.173 Uiso 1 1 calc R U . . .
H01L H 1.058197 0.589666 0.431432 0.173 Uiso 1 1 calc R U . . .
H01M H 0.988143 0.514624 0.435923 0.173 Uiso 1 1 calc R U . . .
C01F C 0.9821(2) 0.5286(5) 0.3242(2) 0.1159(16) Uani 1 1 d . . . . .
H01N H 0.969540 0.444619 0.333604 0.174 Uiso 1 1 calc R U . . .
H01O H 1.035979 0.533740 0.332195 0.174 Uiso 1 1 calc R U . . .
H01P H 0.954946 0.545937 0.283208 0.174 Uiso 1 1 calc R U . . .
C01G C 0.3468(3) 0.5454(6) 0.07773(19) 0.146(2) Uani 1 1 d . . . . .
H01Q H 0.325263 0.565651 0.107260 0.219 Uiso 1 1 calc R U . . .
H01R H 0.366320 0.459976 0.083704 0.219 Uiso 1 1 calc R U . . .
H01S H 0.308066 0.552173 0.039239 0.219 Uiso 1 1 calc R U . . .
C01H C 0.3773(3) 0.7682(5) 0.0757(2) 0.145(2) Uani 1 1 d . . . . .
H01T H 0.332618 0.772598 0.040702 0.217 Uiso 1 1 calc R U . . .
H01U H 0.414540 0.828009 0.072773 0.217 Uiso 1 1 calc R U . . .
H01V H 0.363971 0.788551 0.109560 0.217 Uiso 1 1 calc R U . . .
C01I C 0.4408(3) 0.6166(10) 0.03352(18) 0.211(4) Uani 1 1 d . . . . .
H01W H 0.458672 0.530572 0.034604 0.317 Uiso 1 1 calc R U . . .
H01X H 0.482289 0.674464 0.038605 0.317 Uiso 1 1 calc R U . . .
H01Y H 0.401249 0.632274 -0.003852 0.317 Uiso 1 1 calc R U . . .
C01J C 0.9812(2) 0.7567(5) 0.3468(3) 0.152(3) Uani 1 1 d . . . . .
H01Z H 0.947847 0.780262 0.307975 0.229 Uiso 1 1 calc R U . . .
H H 1.032941 0.755580 0.347935 0.229 Uiso 1 1 calc R U . . .
HA H 0.976533 0.817303 0.375047 0.229 Uiso 1 1 calc R U . . .
Cl1 Cl 0.2849(4) 0.1982(4) 0.3215(3) 0.233(3) Uani 0.634(7) 1 d D U P A 1
Cl2 Cl 0.2442(3) 0.4544(4) 0.31436(16) 0.273(4) Uani 0.634(7) 1 d D U P A 1
Cl3 Cl 0.3280(3) 0.2678(8) 0.1975(2) 0.229(3) Uani 0.634(7) 1 d D U P A 1
C4 C 0.2517(7) 0.3223(8) 0.2692(4) 0.163(4) Uani 0.634(7) 1 d D U P A 1
H4 H 0.206305 0.303540 0.234569 0.195 Uiso 0.634(7) 1 calc R U P A 1
C2 C 0.3228(10) 0.356(2) 0.2571(8) 0.265(9) Uani 0.634(7) 1 d D U P A 1
H2A H 0.367217 0.338464 0.291912 0.318 Uiso 0.634(7) 1 calc R U P A 1
H2B H 0.322551 0.446198 0.248381 0.318 Uiso 0.634(7) 1 calc R U P A 1
C4A C 0.264(2) 0.401(4) 0.2382(14) 0.46(4) Uani 0.366(7) 1 d D U P A 2
H4A H 0.211131 0.371226 0.221624 0.549 Uiso 0.366(7) 1 calc R U P A 2
Cl2A Cl 0.3167(8) 0.3737(14) 0.1923(5) 0.255(6) Uani 0.366(7) 1 d D U P A 2
Cl1A Cl 0.273(3) 0.564(4) 0.2625(18) 0.85(3) Uani 0.366(7) 1 d D U P A 2
C2A C 0.3125(16) 0.326(3) 0.2906(12) 0.227(13) Uani 0.366(7) 1 d D U P A 2
H2AA H 0.352440 0.380079 0.316450 0.272 Uiso 0.366(7) 1 calc R U P A 2
H2AB H 0.336184 0.255682 0.277767 0.272 Uiso 0.366(7) 1 calc R U P A 2
Cl3A Cl 0.2554(7) 0.2693(17) 0.3282(4) 0.291(7) Uani 0.366(7) 1 d D U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O001 C002 1.380(3) . ?
O001 C003 1.373(3) . ?
C002 C005 1.390(3) . ?
C002 C006 1.390(3) . ?
C003 C007 1.394(3) . ?
C003 C009 1.379(3) . ?
C004 C005 1.498(3) . ?
C004 C008 1.410(3) . ?
C004 C00A 1.405(3) . ?
C005 C00B 1.389(3) . ?
C006 C00C 1.391(3) . ?
C006 C00G 1.526(3) . ?
C007 C00E 1.494(3) . ?
C007 C00K 1.383(3) . ?
C008 C00H 1.432(3) . ?
C008 C00Q 1.421(4) . ?
C009 C00G 1.527(3) . ?
C009 C00M 1.397(3) . ?
C00A C00F 1.429(3) . ?
C00A C00O 1.422(4) . ?
C00B C00D 1.399(3) . ?
C00C C00D 1.388(3) . ?
C00D C00V 1.533(3) . ?
C00E C00I 1.396(4) . ?
C00E C00L 1.413(4) . ?
C00F C00J 1.389(4) . ?
C00F C00Z 1.427(4) . ?
C00G C016 1.535(4) . ?
C00G C018 1.537(4) . ?
C00H C00J 1.384(4) . ?
C00H C00Y 1.430(4) . ?
C00I C00T 1.450(4) . ?
C00I C010 1.418(4) . ?
C00K C00N 1.396(4) . ?
C00L C00S 1.432(4) . ?
C00L C00U 1.414(4) . ?
C00M C00N 1.380(4) . ?
C00N C00W 1.539(3) . ?
C00O C012 1.358(4) . ?
C00Q C013 1.349(4) . ?
C00S C00X 1.381(5) . ?
C00S C011 1.431(5) . ?
C00T C00X 1.386(5) . ?
C00T C017 1.426(5) . ?
C00U C01A 1.356(5) . ?
C00V C01E 1.515(5) . ?
C00V C01F 1.521(5) . ?
C00V C01J 1.511(5) . ?
C00W C01G 1.491(5) . ?
C00W C01H 1.503(6) . ?
C00W C01I 1.502(6) . ?
C00Y C015 1.344(4) . ?
C00Z C014 1.343(5) . ?
C010 C01C 1.357(5) . ?
C011 C01D 1.341(6) . ?
C012 C014 1.401(5) . ?
C013 C015 1.408(5) . ?
C017 C01B 1.320(6) . ?
C01A C01D 1.406(6) . ?
C01B C01C 1.430(6) . ?
Cl1 C4 1.770(8) . ?
Cl2 C4 1.802(8) . ?
Cl3 C2 1.745(9) . ?
C4 C2 1.504(9) . ?
C4A Cl2A 1.75(2) . ?
C4A Cl1A 1.80(2) . ?
C4A C2A 1.50(2) . ?
C2A Cl3A 1.738(18) . ?

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
C003 O001 C002 118.80(17) . . ?
O001 C002 C005 114.54(19) . . ?
O001 C002 C006 122.7(2) . . ?
C006 C002 C005 122.7(2) . . ?
O001 C003 C007 114.0(2) . . ?
O001 C003 C009 124.0(2) . . ?
C009 C003 C007 122.0(2) . . ?
C008 C004 C005 119.8(2) . . ?
C00A C004 C005 120.2(2) . . ?
C00A C004 C008 120.0(2) . . ?
C002 C005 C004 120.9(2) . . ?
C00B C005 C002 118.2(2) . . ?
C00B C005 C004 120.9(2) . . ?
C002 C006 C00C 116.5(2) . . ?
C002 C006 C00G 122.4(2) . . ?
C00C C006 C00G 121.1(2) . . ?
C003 C007 C00E 119.4(2) . . ?
C00K C007 C003 118.2(2) . . ?
C00K C007 C00E 122.3(2) . . ?
C004 C008 C00H 119.7(2) . . ?
C004 C008 C00Q 122.9(2) . . ?
C00Q C008 C00H 117.4(2) . . ?
C003 C009 C00G 121.9(2) . . ?
C003 C009 C00M 117.3(2) . . ?
C00M C009 C00G 120.8(2) . . ?
C004 C00A C00F 119.6(2) . . ?
C004 C00A C00O 122.6(2) . . ?
C00O C00A C00F 117.7(2) . . ?
C005 C00B C00D 121.8(2) . . ?
C00D C00C C006 123.7(2) . . ?
C00B C00D C00V 122.5(2) . . ?
C00C C00D C00B 117.0(2) . . ?
C00C C00D C00V 120.4(2) . . ?
C00I C00E C007 120.5(2) . . ?
C00I C00E C00L 120.5(2) . . ?
C00L C00E C007 119.0(2) . . ?
C00J C00F C00A 119.6(2) . . ?
C00J C00F C00Z 121.5(2) . . ?
C00Z C00F C00A 118.9(2) . . ?
C006 C00G C009 110.16(19) . . ?
C006 C00G C016 109.1(2) . . ?
C006 C00G C018 109.1(2) . . ?
C009 C00G C016 109.3(2) . . ?
C009 C00G C018 108.6(2) . . ?
C016 C00G C018 110.6(3) . . ?
C00J C00H C008 119.4(2) . . ?
C00J C00H C00Y 122.2(2) . . ?
C00Y C00H C008 118.4(2) . . ?
C00E C00I C00T 118.9(3) . . ?
C00E C00I C010 122.9(3) . . ?
C010 C00I C00T 118.1(3) . . ?
C00H C00J C00F 121.7(2) . . ?
C007 C00K C00N 122.3(2) . . ?
C00E C00L C00S 119.7(2) . . ?
C00E C00L C00U 123.0(2) . . ?
C00U C00L C00S 117.3(3) . . ?
C00N C00M C009 123.3(2) . . ?
C00K C00N C00W 120.8(2) . . ?
C00M C00N C00K 116.9(2) . . ?
C00M C00N C00W 122.3(2) . . ?
C012 C00O C00A 120.8(3) . . ?
C013 C00Q C008 121.9(3) . . ?
C00X C00S C00L 119.4(3) . . ?
C00X C00S C011 122.2(3) . . ?
C011 C00S C00L 118.3(3) . . ?
C00X C00T C00I 119.7(3) . . ?
C00X C00T C017 122.2(3) . . ?
C017 C00T C00I 118.2(3) . . ?
C01A C00U C00L 122.4(3) . . ?
C01E C00V C00D 112.3(3) . . ?
C01E C00V C01F 107.1(3) . . ?
C01F C00V C00D 110.3(3) . . ?
C01J C00V C00D 108.7(3) . . ?
C01J C00V C01E 110.0(4) . . ?
C01J C00V C01F 108.3(4) . . ?
C01G C00W C00N 111.1(3) . . ?
C01G C00W C01H 107.4(4) . . ?
C01G C00W C01I 111.8(5) . . ?
C01H C00W C00N 107.8(3) . . ?
C01I C00W C00N 111.2(3) . . ?
C01I C00W C01H 107.3(5) . . ?
C00S C00X C00T 121.7(3) . . ?
C015 C00Y C00H 121.7(3) . . ?
C014 C00Z C00F 121.2(3) . . ?
C01C C010 C00I 120.8(3) . . ?
C01D C011 C00S 121.8(3) . . ?
C00O C012 C014 121.4(3) . . ?
C00Q C013 C015 120.7(3) . . ?
C00Z C014 C012 120.0(3) . . ?
C00Y C015 C013 119.9(3) . . ?
C01B C017 C00T 121.7(4) . . ?
C00U C01A C01D 120.1(4) . . ?
C017 C01B C01C 120.7(3) . . ?
C010 C01C C01B 120.4(4) . . ?
C011 C01D C01A 120.1(3) . . ?
Cl1 C4 Cl2 102.5(5) . . ?
C2 C4 Cl1 101.5(12) . . ?
C2 C4 Cl2 101.6(7) . . ?
C4 C2 Cl3 110.3(9) . . ?
Cl2A C4A Cl1A 111(2) . . ?
C2A C4A Cl2A 98.1(17) . . ?
C2A C4A Cl1A 105(2) . . ?
C4A C2A Cl3A 108.8(19) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.538
_oxdiff_exptl_absorpt_empirical_full_min 0.353
####################################################################### 
# 
# 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_20221124-etbr_auto
_database_code_depnum_ccdc_archive 'CCDC 2308125'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2023-11-15 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2023-11-15
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C51 H46 O, C2 H5 Br1'
_chemical_formula_sum            'C53 H51 Br O'
_chemical_formula_weight         783.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHOBr
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'
Br Br -0.6763 1.2805 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.8123(5)
_cell_length_b                   13.0931(5)
_cell_length_c                   14.9329(5)
_cell_angle_alpha                93.704(3)
_cell_angle_beta                 113.887(4)
_cell_angle_gamma                108.240(4)
_cell_volume                     2121.91(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8465
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      72.3650
_cell_measurement_theta_min      3.2950
_shelx_estimated_absorpt_T_max   0.857
_shelx_estimated_absorpt_T_min   0.796
_exptl_absorpt_coefficient_mu    1.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24328
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         3.318
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      273(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     57.00  89.00   0.50    0.50    --   62.87  15.00 -90.00   64
  2  ω     76.00 116.00   0.50    0.50    --   72.70  15.00-150.00   80
  3  ω     67.00 111.00   0.50    0.50    --   76.90  15.00 -90.00   88
  4  ω     79.00 121.00   0.50    0.50    --   76.90  15.00 -60.00   84
  5  ω     61.00 101.00   0.50    0.50    --   72.70  15.00   0.00   80
  6  ω   -105.00 -54.00   0.50    0.50    --  -63.75 -15.00  30.00  102
  7  ω   -103.00 -58.00   0.50    0.50    --  -63.75 -15.00 -30.00   90
  8  ω   -103.00 -59.00   0.50    0.50    --  -63.75 -15.00 -90.00   88
  9  ω   -119.00 -88.00   0.50    0.50    --  -76.53 -15.00 -30.00   62
 10  ω   -114.00 -74.00   0.50    0.50    --  -81.41 -15.00   0.00   80
 11  ω    -96.00 -70.00   0.50    0.50    --  -76.53 -15.00  30.00   52
 12  ω   -125.00 -86.00   0.50    0.50    --  -81.41 -15.00  90.00   78
 13  ω   -113.00 -77.00   0.50    0.50    --  -81.41 -15.00 120.00   72
 14  ω    -82.00 -32.00   0.50    0.50    --  -63.75 125.00  30.00  100
 15  ω    -70.00 -29.00   0.50    0.50    --  -63.75 125.00 150.00   82
 16  ω    -97.00 -38.00   0.50    0.50    --  -76.53 125.00 120.00  118
 17  ω   -102.00 -76.00   0.50    0.50    --  -81.41 125.00 120.00   52
 18  ω    -97.00 -34.00   0.50    0.50    --  -76.53 125.00  60.00  126
 19  ω   -102.00 -48.00   0.50    0.50    --  -81.41 125.00   0.00  108
 20  ω   -102.00 -74.00   0.50    0.50    --  -81.41 125.00  30.00   56
 21  ω   -102.00 -54.00   0.50    0.50    --  -81.41 125.00  90.00   96
 22  ω    -99.00 -42.00   0.50    0.50    --  -81.41 125.00 -60.00  114
 23  ω   -102.00 -76.00   0.50    0.50    --  -81.41 125.00 -30.00   52
 24  ω   -102.00 -45.00   0.50    0.50    --  -81.41 125.00 -90.00  114
 25  ω    -68.00 -43.00   0.50    0.50    --  -81.41 125.00  30.00   50
 26  ω   -102.00 -76.00   0.50    0.50    --  -81.41 125.00-120.00   52
 27  ω    -64.00 -22.00   0.50    0.50    --  -63.75 125.00-150.00   84
 28  ω    -82.00 -39.00   0.50    0.50    --  -81.41 125.00-150.00   86
 29  ω   -102.00 -50.00   0.50    0.50    --  -81.41 125.00-180.00  104
 30  ω     37.00  98.00   0.50    0.50    --   76.90-125.00 -30.00  122
 31  ω     31.00  68.00   0.50    0.50    --   72.70-125.00  30.00   74
 32  ω     47.00  98.00   0.50    0.50    --   76.90-125.00  60.00  102
 33  ω     55.00  97.00   0.50    0.50    --   76.90-125.00-120.00   84
 34  ω     22.00  63.00   0.50    0.50    --   62.87-125.00-180.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0326678000
_diffrn_orient_matrix_UB_12      0.1000385000
_diffrn_orient_matrix_UB_13      -0.0461702000
_diffrn_orient_matrix_UB_21      0.0575698000
_diffrn_orient_matrix_UB_22      -0.0570716000
_diffrn_orient_matrix_UB_23      -0.0498136000
_diffrn_orient_matrix_UB_31      -0.1252371000
_diffrn_orient_matrix_UB_32      -0.0535378000
_diffrn_orient_matrix_UB_33      -0.0936327000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5231
_reflns_number_total             7420
_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       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         7420
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.1320
_refine_ls_R_factor_gt           0.0998
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1470P)²+2.1766P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2730
_refine_ls_wR_factor_ref         0.2954
_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. Restrained distances
 C15-C1
 1.54 with sigma of 0.01
 C1-Br1
 1.94 with sigma of 0.01
 C1A-C15A
 1.54 with sigma of 0.01
 Br1A-C1A
 1.94 with sigma of 0.01
 Br1-C15 \\sim Br1A-C15A
 with sigma of 0.04
 Br1-C1 \\sim Br1A-C1A
 with sigma of 0.02
 C15-C1 \\sim C15A-C1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C15A) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(Br1A) \\sim Ueq, Uanis(Br1) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=
 Sof(Br1A)=1-FVAR(1)
 Sof(Br1)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C1)=Sof(H1A)=Sof(H1B)=
 FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1A(H1AA,H1AB)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C6(H6), C4(H4), C18(H18), C40(H40), C23(H23), C43(H43),
 C26(H26), C37(H37), C32(H32), C21(H21), C19(H19), C20(H20), C41(H41), C42(H42),
  C29(H29), C35(H35), C28(H28), C27(H27), C34(H34), C33(H33)
5.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C52(H52A,H52B,H52C), C45(H45A,H45B,H45C), C49(H49A,H49B,
 H49C), C46(H46A,H46B,H46C), C50(H50A,H50B,H50C), C47(H47A,H47B,H47C), C51(H51A,
 H51B,H51C), C15(H15A,H15B,H15C), C15A(H15D,H15E,H15F)
;
_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
O15 O 0.7672(2) 0.50304(18) 0.74799(19) 0.0498(6) Uani 1 1 d . . . . .
C7 C 0.8485(3) 0.4384(3) 0.6438(2) 0.0395(7) Uani 1 1 d . . . . .
C9 C 0.9316(3) 0.6375(3) 0.7274(2) 0.0396(7) Uani 1 1 d . . . . .
C2 C 0.7686(3) 0.4204(3) 0.6866(2) 0.0405(8) Uani 1 1 d . . . . .
C14 C 0.8482(3) 0.6092(3) 0.7665(2) 0.0409(8) Uani 1 1 d . . . . .
C16 C 0.5936(3) 0.2947(3) 0.7147(3) 0.0446(8) Uani 1 1 d . . . . .
C3 C 0.6831(3) 0.3157(3) 0.6712(3) 0.0436(8) Uani 1 1 d . . . . .
C13 C 0.8399(3) 0.6879(3) 0.8285(3) 0.0424(8) Uani 1 1 d . . . . .
C10 C 1.0077(3) 0.7484(3) 0.7513(2) 0.0428(8) Uani 1 1 d . . . . .
H10 H 1.063715 0.768543 0.724901 0.051 Uiso 1 1 calc R U . . .
C12 C 0.9183(3) 0.7972(3) 0.8504(3) 0.0457(8) Uani 1 1 d . . . . .
H12 H 0.913447 0.850058 0.891618 0.055 Uiso 1 1 calc R U . . .
C11 C 1.0035(3) 0.8299(3) 0.8125(3) 0.0447(8) Uani 1 1 d . . . . .
C8 C 0.9412(3) 0.5529(3) 0.6590(2) 0.0401(8) Uani 1 1 d . . . . .
C30 C 0.7507(3) 0.6569(3) 0.8721(3) 0.0444(8) Uani 1 1 d . . . . .
C6 C 0.8412(3) 0.3479(3) 0.5840(2) 0.0423(8) Uani 1 1 d . . . . .
H6 H 0.894556 0.359204 0.554831 0.051 Uiso 1 1 calc R U . . .
C39 C 0.7931(4) 0.6628(3) 0.9755(3) 0.0484(9) Uani 1 1 d . . . . .
C31 C 0.6232(3) 0.6268(3) 0.8087(3) 0.0497(9) Uani 1 1 d . . . . .
C25 C 0.6336(3) 0.2968(3) 0.8180(3) 0.0489(9) Uani 1 1 d . . . . .
C17 C 0.4679(3) 0.2663(3) 0.6501(3) 0.0469(8) Uani 1 1 d . . . . .
C5 C 0.7578(3) 0.2410(3) 0.5654(3) 0.0431(8) Uani 1 1 d . . . . .
C4 C 0.6793(3) 0.2276(3) 0.6105(3) 0.0461(8) Uani 1 1 d . . . . .
H4 H 0.622509 0.157553 0.599645 0.055 Uiso 1 1 calc R U . . .
C53 C 0.9119(4) 0.5842(3) 0.5558(3) 0.0521(9) Uani 1 1 d . . . . .
H53A H 0.918750 0.531764 0.512543 0.078 Uiso 1 1 calc R U . . .
H53B H 0.968953 0.656484 0.564557 0.078 Uiso 1 1 calc R U . . .
H53C H 0.829702 0.583581 0.526142 0.078 Uiso 1 1 calc R U . . .
C44 C 0.7549(4) 0.1458(3) 0.4979(3) 0.0528(9) Uani 1 1 d . . . . .
C24 C 0.5439(4) 0.2632(3) 0.8554(3) 0.0543(10) Uani 1 1 d . . . . .
C52 C 1.0718(3) 0.5525(3) 0.7061(3) 0.0522(9) Uani 1 1 d . . . . .
H52A H 1.090073 0.533950 0.770526 0.078 Uiso 1 1 calc R U . . .
H52B H 1.129474 0.624217 0.714211 0.078 Uiso 1 1 calc R U . . .
H52C H 1.077661 0.498979 0.663182 0.078 Uiso 1 1 calc R U . . .
C22 C 0.3798(4) 0.2343(3) 0.6893(3) 0.0535(9) Uani 1 1 d . . . . .
C36 C 0.5393(4) 0.6045(3) 0.8518(3) 0.0591(10) Uani 1 1 d . . . . .
C38 C 0.7073(4) 0.6393(3) 1.0169(3) 0.0562(10) Uani 1 1 d . . . . .
C48 C 1.0904(4) 0.9513(3) 0.8361(3) 0.0539(9) Uani 1 1 d . . . . .
C18 C 0.4212(4) 0.2668(3) 0.5452(3) 0.0566(10) Uani 1 1 d . . . . .
H18 H 0.475991 0.288045 0.517678 0.068 Uiso 1 1 calc R U . . .
C40 C 0.9204(4) 0.6915(3) 1.0435(3) 0.0582(10) Uani 1 1 d . . . . .
H40 H 0.977944 0.705666 1.018452 0.070 Uiso 1 1 calc R U . . .
C23 C 0.4206(4) 0.2322(3) 0.7904(3) 0.0592(10) Uani 1 1 d . . . . .
H23 H 0.363085 0.209298 0.815159 0.071 Uiso 1 1 calc R U . . .
C43 C 0.7529(5) 0.6477(4) 1.1237(4) 0.0701(13) Uani 1 1 d . . . . .
H43 H 0.697960 0.633053 1.151384 0.084 Uiso 1 1 calc R U . . .
C26 C 0.7595(4) 0.3281(4) 0.8879(3) 0.0622(11) Uani 1 1 d . . . . .
H26 H 0.819161 0.349878 0.865315 0.075 Uiso 1 1 calc R U . . .
C37 C 0.5834(4) 0.6113(3) 0.9548(3) 0.0629(11) Uani 1 1 d . . . . .
H37 H 0.528428 0.596707 0.982392 0.075 Uiso 1 1 calc R U . . .
C32 C 0.5735(4) 0.6191(4) 0.7026(3) 0.0627(11) Uani 1 1 d . . . . .
H32 H 0.626220 0.632163 0.672835 0.075 Uiso 1 1 calc R U . . .
C21 C 0.2524(4) 0.2044(4) 0.6230(4) 0.0656(11) Uani 1 1 d . . . . .
H21 H 0.195135 0.183734 0.648164 0.079 Uiso 1 1 calc R U . . .
C19 C 0.2984(4) 0.2370(4) 0.4847(4) 0.0709(12) Uani 1 1 d . . . . .
H19 H 0.270683 0.237440 0.416751 0.085 Uiso 1 1 calc R U . . .
C20 C 0.2133(4) 0.2054(4) 0.5245(4) 0.0722(12) Uani 1 1 d . . . . .
H20 H 0.129754 0.185212 0.482729 0.087 Uiso 1 1 calc R U . . .
C41 C 0.9588(5) 0.6985(4) 1.1438(3) 0.0707(12) Uani 1 1 d . . . . .
H41 H 1.041985 0.717981 1.186277 0.085 Uiso 1 1 calc R U . . .
C42 C 0.8733(6) 0.6763(4) 1.1838(4) 0.0741(13) Uani 1 1 d . . . . .
H42 H 0.900717 0.681545 1.252505 0.089 Uiso 1 1 calc R U . . .
C29 C 0.5849(5) 0.2602(4) 0.9594(3) 0.0706(12) Uani 1 1 d . . . . .
H29 H 0.527359 0.236846 0.984010 0.085 Uiso 1 1 calc R U . . .
C35 C 0.4113(4) 0.5787(4) 0.7877(4) 0.0772(14) Uani 1 1 d . . . . .
H35 H 0.356310 0.565682 0.815322 0.093 Uiso 1 1 calc R U . . .
C28 C 0.7061(5) 0.2910(5) 1.0225(4) 0.0842(15) Uani 1 1 d . . . . .
H28 H 0.730810 0.288149 1.089728 0.101 Uiso 1 1 calc R U . . .
C27 C 0.7950(5) 0.3271(5) 0.9870(3) 0.0797(14) Uani 1 1 d . . . . .
H27 H 0.878105 0.350322 1.031311 0.096 Uiso 1 1 calc R U . . .
C34 C 0.3692(5) 0.5729(5) 0.6876(5) 0.0939(17) Uani 1 1 d . . . . .
H34 H 0.285847 0.555548 0.647313 0.113 Uiso 1 1 calc R U . . .
C45 C 0.7377(6) 0.1746(4) 0.3958(4) 0.0908(17) Uani 1 1 d . . . . .
H45A H 0.660333 0.183540 0.363454 0.136 Uiso 1 1 calc R U . . .
H45B H 0.738807 0.116218 0.354264 0.136 Uiso 1 1 calc R U . . .
H45C H 0.803173 0.241985 0.405953 0.136 Uiso 1 1 calc R U . . .
C49 C 1.2223(4) 0.9578(4) 0.8665(5) 0.0912(17) Uani 1 1 d . . . . .
H49A H 1.247280 0.923502 0.922349 0.137 Uiso 1 1 calc R U . . .
H49B H 1.276467 1.033662 0.885371 0.137 Uiso 1 1 calc R U . . .
H49C H 1.225631 0.920329 0.810918 0.137 Uiso 1 1 calc R U . . .
C46 C 0.6496(6) 0.0397(4) 0.4769(5) 0.0981(19) Uani 1 1 d . . . . .
H46A H 0.657844 0.018186 0.538937 0.147 Uiso 1 1 calc R U . . .
H46B H 0.650769 -0.016987 0.433640 0.147 Uiso 1 1 calc R U . . .
H46C H 0.573294 0.050475 0.444832 0.147 Uiso 1 1 calc R U . . .
C50 C 1.0927(5) 1.0225(4) 0.9210(4) 0.0905(17) Uani 1 1 d . . . . .
H50A H 1.122731 0.995896 0.981141 0.136 Uiso 1 1 calc R U . . .
H50B H 1.011016 1.019659 0.904263 0.136 Uiso 1 1 calc R U . . .
H50C H 1.145737 1.097239 0.931453 0.136 Uiso 1 1 calc R U . . .
C33 C 0.4514(5) 0.5932(5) 0.6441(4) 0.0854(15) Uani 1 1 d . . . . .
H33 H 0.421876 0.588718 0.575343 0.102 Uiso 1 1 calc R U . . .
C47 C 0.8772(5) 0.1314(5) 0.5449(5) 0.108(2) Uani 1 1 d . . . . .
H47A H 0.941650 0.197978 0.551726 0.163 Uiso 1 1 calc R U . . .
H47B H 0.875264 0.071523 0.502776 0.163 Uiso 1 1 calc R U . . .
H47C H 0.892212 0.115558 0.609853 0.163 Uiso 1 1 calc R U . . .
C51 C 1.0496(7) 0.9951(4) 0.7411(4) 0.117(2) Uani 1 1 d . . . . .
H51A H 1.102827 1.070378 0.754228 0.175 Uiso 1 1 calc R U . . .
H51B H 0.966689 0.991016 0.719933 0.175 Uiso 1 1 calc R U . . .
H51C H 1.053440 0.951497 0.689147 0.175 Uiso 1 1 calc R U . . .
Br1 Br 0.7030(3) 0.9797(4) 0.7667(2) 0.252(2) Uani 0.621(7) 1 d D U P A 1
C15 C 0.5267(9) 0.9111(10) 0.8632(7) 0.074(3) Uani 0.621(7) 1 d D U P A 1
H15A H 0.473663 0.847369 0.809297 0.111 Uiso 0.621(7) 1 calc R U P A 1
H15B H 0.478381 0.936824 0.887394 0.111 Uiso 0.621(7) 1 calc R U P A 1
H15C H 0.585166 0.892035 0.916774 0.111 Uiso 0.621(7) 1 calc R U P A 1
C1 C 0.5954(10) 1.0029(9) 0.8249(8) 0.147(5) Uani 0.621(7) 1 d D U P A 1
H1A H 0.645564 1.066462 0.880696 0.176 Uiso 0.621(7) 1 calc R U P A 1
H1B H 0.533771 1.023533 0.774496 0.176 Uiso 0.621(7) 1 calc R U P A 1
C15A C 0.5032(14) 0.9451(13) 0.8703(12) 0.060(4) Uani 0.379(7) 1 d D U P A 2
H15D H 0.416851 0.901135 0.837922 0.090 Uiso 0.379(7) 1 calc R U P A 2
H15E H 0.517185 1.012816 0.847564 0.090 Uiso 0.379(7) 1 calc R U P A 2
H15F H 0.531816 0.961125 0.941686 0.090 Uiso 0.379(7) 1 calc R U P A 2
C1A C 0.5724(14) 0.8823(11) 0.8445(11) 0.085(5) Uani 0.379(7) 1 d D U P A 2
H1AA H 0.513714 0.812740 0.798331 0.103 Uiso 0.379(7) 1 calc R U P A 2
H1AB H 0.624874 0.865946 0.905205 0.103 Uiso 0.379(7) 1 calc R U P A 2
Br1A Br 0.6729(19) 0.962(2) 0.7843(16) 0.744(19) Uani 0.379(7) 1 d D U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O15 C2 1.382(4) . ?
O15 C14 1.379(4) . ?
C7 C2 1.381(4) . ?
C7 C8 1.528(4) . ?
C7 C6 1.391(4) . ?
C9 C14 1.381(4) . ?
C9 C10 1.397(4) . ?
C9 C8 1.524(4) . ?
C2 C3 1.397(4) . ?
C14 C13 1.398(4) . ?
C16 C3 1.495(4) . ?
C16 C25 1.410(5) . ?
C16 C17 1.409(5) . ?
C3 C4 1.397(4) . ?
C13 C12 1.392(5) . ?
C13 C30 1.497(4) . ?
C10 C11 1.388(5) . ?
C12 C11 1.391(5) . ?
C11 C48 1.547(5) . ?
C8 C53 1.547(5) . ?
C8 C52 1.532(5) . ?
C30 C39 1.401(5) . ?
C30 C31 1.420(5) . ?
C6 C5 1.397(5) . ?
C39 C38 1.431(5) . ?
C39 C40 1.435(6) . ?
C31 C36 1.430(5) . ?
C31 C32 1.430(6) . ?
C25 C24 1.436(5) . ?
C25 C26 1.423(6) . ?
C17 C22 1.437(5) . ?
C17 C18 1.434(5) . ?
C5 C4 1.395(5) . ?
C5 C44 1.533(4) . ?
C44 C45 1.540(6) . ?
C44 C46 1.508(6) . ?
C44 C47 1.514(6) . ?
C24 C23 1.382(6) . ?
C24 C29 1.430(6) . ?
C22 C23 1.389(6) . ?
C22 C21 1.428(6) . ?
C36 C37 1.392(6) . ?
C36 C35 1.435(6) . ?
C38 C43 1.443(6) . ?
C38 C37 1.383(6) . ?
C48 C49 1.533(6) . ?
C48 C50 1.509(6) . ?
C48 C51 1.518(6) . ?
C18 C19 1.365(6) . ?
C40 C41 1.360(6) . ?
C43 C42 1.341(7) . ?
C26 C27 1.363(6) . ?
C32 C33 1.359(6) . ?
C21 C20 1.351(6) . ?
C19 C20 1.410(6) . ?
C41 C42 1.413(7) . ?
C29 C28 1.355(7) . ?
C35 C34 1.356(7) . ?
C28 C27 1.409(7) . ?
C34 C33 1.416(7) . ?
Br1 C1 1.987(8) . ?
C15 C1 1.543(8) . ?
C15A C1A 1.518(8) . ?
C1A Br1A 1.944(9) . ?

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
C14 O15 C2 118.6(2) . . ?
C2 C7 C8 122.3(3) . . ?
C2 C7 C6 117.7(3) . . ?
C6 C7 C8 120.0(3) . . ?
C14 C9 C10 117.6(3) . . ?
C14 C9 C8 122.4(3) . . ?
C10 C9 C8 120.0(3) . . ?
O15 C2 C3 114.7(3) . . ?
C7 C2 O15 123.3(3) . . ?
C7 C2 C3 121.9(3) . . ?
O15 C14 C9 123.4(3) . . ?
O15 C14 C13 114.9(3) . . ?
C9 C14 C13 121.7(3) . . ?
C25 C16 C3 120.4(3) . . ?
C17 C16 C3 119.1(3) . . ?
C17 C16 C25 120.4(3) . . ?
C2 C3 C16 122.9(3) . . ?
C2 C3 C4 118.2(3) . . ?
C4 C3 C16 118.9(3) . . ?
C14 C13 C30 121.7(3) . . ?
C12 C13 C14 118.3(3) . . ?
C12 C13 C30 120.0(3) . . ?
C11 C10 C9 123.1(3) . . ?
C11 C12 C13 122.1(3) . . ?
C10 C11 C12 117.1(3) . . ?
C10 C11 C48 120.5(3) . . ?
C12 C11 C48 122.4(3) . . ?
C7 C8 C53 108.8(3) . . ?
C7 C8 C52 109.9(3) . . ?
C9 C8 C7 110.0(2) . . ?
C9 C8 C53 109.0(3) . . ?
C9 C8 C52 109.5(3) . . ?
C52 C8 C53 109.7(3) . . ?
C39 C30 C13 120.3(3) . . ?
C39 C30 C31 120.2(3) . . ?
C31 C30 C13 119.5(3) . . ?
C7 C6 C5 123.4(3) . . ?
C30 C39 C38 119.6(4) . . ?
C30 C39 C40 123.0(3) . . ?
C38 C39 C40 117.4(3) . . ?
C30 C31 C36 119.2(3) . . ?
C30 C31 C32 123.2(3) . . ?
C32 C31 C36 117.6(4) . . ?
C16 C25 C24 119.2(3) . . ?
C16 C25 C26 123.3(3) . . ?
C26 C25 C24 117.5(3) . . ?
C16 C17 C22 119.5(3) . . ?
C16 C17 C18 123.4(3) . . ?
C18 C17 C22 117.1(3) . . ?
C6 C5 C44 120.2(3) . . ?
C4 C5 C6 116.5(3) . . ?
C4 C5 C44 123.3(3) . . ?
C5 C4 C3 122.4(3) . . ?
C5 C44 C45 109.4(3) . . ?
C46 C44 C5 112.4(3) . . ?
C46 C44 C45 106.9(4) . . ?
C46 C44 C47 111.3(4) . . ?
C47 C44 C5 109.5(3) . . ?
C47 C44 C45 107.2(4) . . ?
C23 C24 C25 119.6(4) . . ?
C23 C24 C29 121.5(4) . . ?
C29 C24 C25 118.8(4) . . ?
C23 C22 C17 119.2(4) . . ?
C23 C22 C21 121.7(4) . . ?
C21 C22 C17 119.1(4) . . ?
C31 C36 C35 118.8(4) . . ?
C37 C36 C31 119.7(4) . . ?
C37 C36 C35 121.5(4) . . ?
C39 C38 C43 118.8(4) . . ?
C37 C38 C39 119.9(4) . . ?
C37 C38 C43 121.3(4) . . ?
C49 C48 C11 110.0(3) . . ?
C50 C48 C11 112.5(3) . . ?
C50 C48 C49 107.5(4) . . ?
C50 C48 C51 110.6(4) . . ?
C51 C48 C11 108.3(3) . . ?
C51 C48 C49 107.8(5) . . ?
C19 C18 C17 121.7(4) . . ?
C41 C40 C39 121.5(4) . . ?
C24 C23 C22 122.0(3) . . ?
C42 C43 C38 121.1(4) . . ?
C27 C26 C25 121.9(4) . . ?
C38 C37 C36 121.4(3) . . ?
C33 C32 C31 122.0(4) . . ?
C20 C21 C22 121.4(4) . . ?
C18 C19 C20 120.4(4) . . ?
C21 C20 C19 120.4(4) . . ?
C40 C41 C42 120.5(5) . . ?
C43 C42 C41 120.7(4) . . ?
C28 C29 C24 121.0(4) . . ?
C34 C35 C36 121.1(4) . . ?
C29 C28 C27 120.5(4) . . ?
C26 C27 C28 120.2(5) . . ?
C35 C34 C33 120.4(5) . . ?
C32 C33 C34 120.1(5) . . ?
C15 C1 Br1 121.4(8) . . ?
C15A C1A Br1A 113.3(12) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.723
_oxdiff_exptl_absorpt_empirical_full_min 0.506
####################################################################### 
# 
# 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_20221124-3cbr_auto
_database_code_depnum_ccdc_archive 'CCDC 2308126'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2023-11-15 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2023-11-15
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C51 H46 O, C3 H7 Br'
_chemical_formula_sum            'C54 H53 Br O'
_chemical_formula_weight         797.87
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHOBr
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'
Br Br -0.6763 1.2805 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.8327(4)
_cell_length_b                   13.0654(3)
_cell_length_c                   15.2440(5)
_cell_angle_alpha                94.104(2)
_cell_angle_beta                 114.041(3)
_cell_angle_gamma                108.338(2)
_cell_volume                     2156.01(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12435
_cell_measurement_temperature    283(1)
_cell_measurement_theta_max      75.7200
_cell_measurement_theta_min      3.2230
_shelx_estimated_absorpt_T_max   0.858
_shelx_estimated_absorpt_T_min   0.798
_exptl_absorpt_coefficient_mu    1.576
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25029
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        66.581
_diffrn_reflns_theta_max         66.581
_diffrn_reflns_theta_min         3.262
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      283(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     52.00  95.00   0.50    0.30    --   62.89  15.00 -90.00   86
  2  ω     60.00 106.00   0.50    0.30    --   62.89  15.00-150.00   92
  3  ω     62.00 113.00   0.50    0.30    --   72.93  15.00-180.00  102
  4  ω    -71.00 -29.00   0.50    0.30    --  -71.74 125.00 -30.00   84
  5  ω    -97.00 -37.00   0.50    0.30    --  -76.43 125.00 -60.00  120
  6  ω   -102.00 -77.00   0.50    0.30    --  -81.49 125.00 -60.00   50
  7  ω    -56.00 -30.00   0.50    0.30    --  -71.74 125.00   0.00   52
  8  ω    -72.00 -30.00   0.50    0.30    --  -71.74 125.00  30.00   84
  9  ω   -102.00 -76.00   0.50    0.30    --  -81.49 125.00  60.00   52
 10  ω   -101.00 -75.00   0.50    0.30    --  -81.49 125.00 120.00   52
 11  ω   -101.00 -52.00   0.50    0.30    --  -81.49 125.00 150.00   98
 12  ω    -65.00 -30.00   0.50    0.30    --  -63.72 125.00 150.00   70
 13  ω   -102.00 -47.00   0.50    0.30    --  -81.49 125.00  90.00  110
 14  ω   -100.00 -74.00   0.50    0.30    --  -81.49 125.00  30.00   52
 15  ω   -102.00 -40.00   0.50    0.30    --  -81.49 125.00   0.00  124
 16  ω   -102.00 -75.00   0.50    0.30    --  -81.49 125.00 -30.00   54
 17  ω   -102.00 -61.00   0.50    0.30    --  -81.49 125.00 -90.00   82
 18  ω   -102.00 -49.00   0.50    0.30    --  -81.49 125.00-150.00  106
 19  ω   -107.00 -54.00   0.50    0.30    --  -63.72 -15.00-120.00  106
 20  ω   -103.00 -54.00   0.50    0.30    --  -63.72 -15.00-180.00   98
 21  ω   -101.00 -73.00   0.50    0.30    --  -71.74 -15.00-150.00   56
 22  ω   -112.00 -74.00   0.50    0.30    --  -81.49 -15.00 -90.00   76
 23  ω   -104.00 -65.00   0.50    0.30    --  -63.72 -15.00 -60.00   78
 24  ω   -124.00 -81.00   0.50    0.30    --  -81.49 -15.00 -30.00   86
 25  ω   -116.00 -67.00   0.50    0.30    --  -76.43 -15.00   0.00   98
 26  ω   -124.00 -72.00   0.50    0.30    --  -81.49 -15.00  60.00  104
 27  ω   -106.00 -81.00   0.50    0.30    --  -63.72 -15.00  90.00   50
 28  ω   -120.00 -94.00   0.50    0.30    --  -76.43 -15.00 120.00   52
 29  ω     33.00  74.00   0.50    0.30    --   62.89-125.00 150.00   82
 30  ω     34.00  74.00   0.50    0.30    --   62.89-125.00   0.00   80
 31  ω     40.00  98.00   0.50    0.30    --   76.75-125.00 -30.00  116
 32  ω     31.00  58.00   0.50    0.30    --   72.93-125.00 -60.00   54
 33  ω     37.00  96.00   0.50    0.30    --   76.75-125.00 -90.00  118
 34  ω     40.00  98.00   0.50    0.30    --   76.75-125.00-150.00  116
 35  ω     69.00  98.00   0.50    0.30    --   76.75-125.00  90.00   58
 36  ω     69.00  98.00   0.50    0.30    --   76.75-125.00 120.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1345623000
_diffrn_orient_matrix_UB_12      0.0528908000
_diffrn_orient_matrix_UB_13      0.0178131000
_diffrn_orient_matrix_UB_21      -0.0392335000
_diffrn_orient_matrix_UB_22      0.0629415000
_diffrn_orient_matrix_UB_23      -0.0815878000
_diffrn_orient_matrix_UB_31      0.0224344000
_diffrn_orient_matrix_UB_32      0.0976550000
_diffrn_orient_matrix_UB_33      0.0771888000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5406
_reflns_number_total             7518
_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       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.031
_refine_diff_density_min         -1.594
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       0.0037(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.831
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7518
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.1686
_refine_ls_R_factor_gt           0.1461
_refine_ls_restrained_S_all      1.899
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4206
_refine_ls_wR_factor_ref         0.4423
_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. Restrained distances
 C15-C1 = C54-C15
 1.54 with sigma of 0.01
 Br1-C54
 1.94 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(Br1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C54(H54A,H54B)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C6(H6), C4(H4), C12(H12), C26(H26), C40(H40), C23(H23), C37(H37),
 C29(H29), C18(H18), C43(H43), C32(H32), C28(H28), C27(H27), C21(H21), C41(H41),
  C42(H42), C35(H35), C19(H19), C33(H33), C20(H20), C34(H34)
4.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C52(H52A,H52B,H52C), C45(H45A,H45B,H45C), C49(H49A,H49B,
 H49C), C50(H50A,H50B,H50C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C51(H51A,
 H51B,H51C), C1(H1A,H1B,H1C)
;
_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
O15 O 0.2660(2) 0.50429(16) 0.2445(2) 0.0504(8) Uani 1 1 d . . . . .
C7 C 0.4336(3) 0.6404(2) 0.2292(3) 0.0399(9) Uani 1 1 d . . . . .
C2 C 0.3481(3) 0.6105(2) 0.2652(3) 0.0427(9) Uani 1 1 d . . . . .
C8 C 0.4451(3) 0.5561(2) 0.1611(3) 0.0404(9) Uani 1 1 d . . . . .
C9 C 0.3509(3) 0.4411(2) 0.1449(3) 0.0404(9) Uani 1 1 d . . . . .
C5 C 0.5054(4) 0.8326(2) 0.3152(3) 0.0443(9) Uani 1 1 d . . . . .
C3 C 0.3394(4) 0.6891(2) 0.3271(3) 0.0440(10) Uani 1 1 d . . . . .
C14 C 0.2689(3) 0.4221(2) 0.1844(3) 0.0419(9) Uani 1 1 d . . . . .
C13 C 0.1804(3) 0.3165(2) 0.1660(3) 0.0441(10) Uani 1 1 d . . . . .
C25 C 0.2875(4) 0.6605(2) 0.4669(3) 0.0468(10) Uani 1 1 d . . . . .
C10 C 0.3442(3) 0.3502(2) 0.0862(3) 0.0426(9) Uani 1 1 d . . . . .
H10 H 0.398921 0.361413 0.059069 0.051 Uiso 1 1 calc R U . . .
C6 C 0.5105(3) 0.7512(2) 0.2548(3) 0.0441(9) Uani 1 1 d . . . . .
H6 H 0.567846 0.772010 0.230461 0.053 Uiso 1 1 calc R U . . .
C30 C 0.0920(4) 0.2955(2) 0.2093(3) 0.0452(10) Uani 1 1 d . . . . .
C16 C 0.2467(4) 0.6562(2) 0.3661(3) 0.0460(10) Uani 1 1 d . . . . .
C11 C 0.2588(3) 0.2428(2) 0.0661(3) 0.0434(9) Uani 1 1 d . . . . .
C39 C -0.0353(4) 0.2654(2) 0.1440(3) 0.0478(10) Uani 1 1 d . . . . .
C4 C 0.4179(4) 0.7985(2) 0.3499(3) 0.0453(10) Uani 1 1 d . . . . .
H4 H 0.411952 0.851371 0.389923 0.054 Uiso 1 1 calc R U . . .
C12 C 0.1793(4) 0.2290(2) 0.1078(3) 0.0462(10) Uani 1 1 d . . . . .
H12 H 0.122675 0.158246 0.096436 0.055 Uiso 1 1 calc R U . . .
C17 C 0.1205(4) 0.6248(3) 0.3011(3) 0.0499(11) Uani 1 1 d . . . . .
C24 C 0.1978(4) 0.6348(3) 0.5046(3) 0.0550(12) Uani 1 1 d . . . . .
C53 C 0.4180(4) 0.5874(3) 0.0627(3) 0.0546(11) Uani 1 1 d . . . . .
H53A H 0.335049 0.584579 0.031916 0.082 Uiso 1 1 calc R U . . .
H53B H 0.427694 0.536341 0.020916 0.082 Uiso 1 1 calc R U . . .
H53C H 0.474236 0.661072 0.072903 0.082 Uiso 1 1 calc R U . . .
C48 C 0.2582(4) 0.1471(3) -0.0003(3) 0.0530(11) Uani 1 1 d . . . . .
C38 C -0.1229(4) 0.2346(3) 0.1819(4) 0.0542(11) Uani 1 1 d . . . . .
C31 C 0.1311(4) 0.3004(3) 0.3092(3) 0.0514(11) Uani 1 1 d . . . . .
C52 C 0.5739(4) 0.5553(3) 0.2089(3) 0.0537(11) Uani 1 1 d . . . . .
H52A H 0.633193 0.629603 0.227638 0.081 Uiso 1 1 calc R U . . .
H52B H 0.584275 0.510292 0.162883 0.081 Uiso 1 1 calc R U . . .
H52C H 0.585847 0.525463 0.266421 0.081 Uiso 1 1 calc R U . . .
C44 C 0.5919(4) 0.9542(3) 0.3397(3) 0.0538(11) Uani 1 1 d . . . . .
C22 C 0.0334(4) 0.5992(3) 0.3409(4) 0.0575(12) Uani 1 1 d . . . . .
C26 C 0.4136(4) 0.6886(3) 0.5371(3) 0.0583(11) Uani 1 1 d . . . . .
H26 H 0.472707 0.703525 0.514240 0.070 Uiso 1 1 calc R U . . .
C36 C 0.0413(4) 0.2689(3) 0.3462(3) 0.0587(12) Uani 1 1 d . . . . .
C40 C -0.0805(4) 0.2636(3) 0.0412(3) 0.0578(11) Uani 1 1 d . . . . .
H40 H -0.025268 0.283261 0.014763 0.069 Uiso 1 1 calc R U . . .
C23 C 0.0749(4) 0.6060(3) 0.4414(4) 0.0584(12) Uani 1 1 d . . . . .
H23 H 0.018312 0.590711 0.466675 0.070 Uiso 1 1 calc R U . . .
C37 C -0.0826(4) 0.2356(3) 0.2821(4) 0.0597(12) Uani 1 1 d . . . . .
H37 H -0.140179 0.213358 0.306188 0.072 Uiso 1 1 calc R U . . .
C29 C 0.2409(5) 0.6413(3) 0.6086(4) 0.0638(13) Uani 1 1 d . . . . .
H29 H 0.184530 0.625111 0.634178 0.077 Uiso 1 1 calc R U . . .
C18 C 0.0732(5) 0.6193(3) 0.1984(3) 0.0627(12) Uani 1 1 d . . . . .
H18 H 0.127611 0.635663 0.170996 0.075 Uiso 1 1 calc R U . . .
C43 C -0.2516(4) 0.2025(3) 0.1165(5) 0.0688(14) Uani 1 1 d . . . . .
H43 H -0.308625 0.182354 0.141252 0.083 Uiso 1 1 calc R U . . .
C32 C 0.2573(5) 0.3331(4) 0.3795(4) 0.0655(13) Uani 1 1 d . . . . .
H32 H 0.317575 0.354219 0.358080 0.079 Uiso 1 1 calc R U . . .
C28 C 0.3635(6) 0.6710(4) 0.6707(4) 0.0720(15) Uani 1 1 d . . . . .
H28 H 0.389908 0.675760 0.737957 0.086 Uiso 1 1 calc R U . . .
C27 C 0.4503(5) 0.6944(4) 0.6328(4) 0.0701(14) Uani 1 1 d . . . . .
H27 H 0.533418 0.713980 0.675274 0.084 Uiso 1 1 calc R U . . .
C21 C -0.0935(5) 0.5734(4) 0.2769(4) 0.0763(16) Uani 1 1 d . . . . .
H21 H -0.149790 0.559928 0.302466 0.092 Uiso 1 1 calc R U . . .
C41 C -0.2044(5) 0.2335(4) -0.0195(4) 0.0739(14) Uani 1 1 d . . . . .
H41 H -0.231679 0.234352 -0.085953 0.089 Uiso 1 1 calc R U . . .
C42 C -0.2911(5) 0.2010(4) 0.0189(5) 0.0767(16) Uani 1 1 d . . . . .
H42 H -0.374850 0.178807 -0.022851 0.092 Uiso 1 1 calc R U . . .
C35 C 0.0825(6) 0.2719(4) 0.4488(4) 0.0769(16) Uani 1 1 d . . . . .
H35 H 0.025516 0.254730 0.473689 0.092 Uiso 1 1 calc R U . . .
C45 C 0.5933(5) 1.0264(3) 0.4225(4) 0.0817(18) Uani 1 1 d . . . . .
H45A H 0.510265 1.016149 0.408817 0.122 Uiso 1 1 calc R U . . .
H45B H 0.638284 1.102725 0.427872 0.122 Uiso 1 1 calc R U . . .
H45C H 0.632204 1.006261 0.483464 0.122 Uiso 1 1 calc R U . . .
C49 C 0.2454(6) 0.1784(4) -0.0993(4) 0.0806(17) Uani 1 1 d . . . . .
H49A H 0.165607 0.181518 -0.135101 0.121 Uiso 1 1 calc R U . . .
H49B H 0.254554 0.123536 -0.137891 0.121 Uiso 1 1 calc R U . . .
H49C H 0.308007 0.249399 -0.086400 0.121 Uiso 1 1 calc R U . . .
C50 C 0.1505(6) 0.0400(3) -0.0235(5) 0.087(2) Uani 1 1 d . . . . .
H50A H 0.164413 0.011159 0.034648 0.131 Uiso 1 1 calc R U . . .
H50B H 0.143089 -0.013060 -0.074821 0.131 Uiso 1 1 calc R U . . .
H50C H 0.076016 0.054265 -0.045073 0.131 Uiso 1 1 calc R U . . .
C19 C -0.0463(5) 0.5915(5) 0.1398(4) 0.0837(17) Uani 1 1 d . . . . .
H19 H -0.073454 0.587233 0.072535 0.100 Uiso 1 1 calc R U . . .
C46 C 0.5516(7) 1.0004(3) 0.2482(4) 0.095(2) Uani 1 1 d . . . . .
H46A H 0.549342 0.954693 0.194726 0.142 Uiso 1 1 calc R U . . .
H46B H 0.608841 1.074522 0.261550 0.142 Uiso 1 1 calc R U . . .
H46C H 0.470964 1.001158 0.230367 0.142 Uiso 1 1 calc R U . . .
C33 C 0.2925(6) 0.3344(5) 0.4772(4) 0.0890(19) Uani 1 1 d . . . . .
H33 H 0.375833 0.358754 0.521104 0.107 Uiso 1 1 calc R U . . .
C47 C 0.7249(5) 0.9615(4) 0.3724(5) 0.091(2) Uani 1 1 d . . . . .
H47A H 0.749601 0.929493 0.428507 0.136 Uiso 1 1 calc R U . . .
H47B H 0.778916 1.037818 0.389821 0.136 Uiso 1 1 calc R U . . .
H47C H 0.729171 0.921908 0.319232 0.136 Uiso 1 1 calc R U . . .
C20 C -0.1333(6) 0.5683(5) 0.1780(5) 0.0907(19) Uani 1 1 d . . . . .
H20 H -0.216425 0.549856 0.136231 0.109 Uiso 1 1 calc R U . . .
C34 C 0.2055(7) 0.2997(6) 0.5117(5) 0.097(2) Uani 1 1 d . . . . .
H34 H 0.230106 0.295328 0.577239 0.117 Uiso 1 1 calc R U . . .
C51 C 0.3774(6) 0.1311(5) 0.0514(5) 0.097(2) Uani 1 1 d . . . . .
H51A H 0.444690 0.197870 0.062257 0.146 Uiso 1 1 calc R U . . .
H51B H 0.377723 0.071224 0.011260 0.146 Uiso 1 1 calc R U . . .
H51C H 0.386240 0.114109 0.113611 0.146 Uiso 1 1 calc R U . . .
Br1 Br 0.2344(3) 0.0021(3) 0.2591(2) 0.3285(19) Uani 1 1 d D U . . .
C1 C -0.0187(4) -0.0982(5) 0.3746(3) 0.0700(15) Uani 1 1 d D U . . .
H1A H -0.091289 -0.164922 0.346500 0.105 Uiso 1 1 calc R U . . .
H1B H -0.041109 -0.036363 0.357140 0.105 Uiso 1 1 calc R U . . .
H1C H 0.020336 -0.087126 0.445197 0.105 Uiso 1 1 calc R U . . .
C15 C 0.0699(9) -0.1081(8) 0.3353(8) 0.205(5) Uani 1 1 d D U . . .
H15A H 0.027625 -0.166584 0.275766 0.246 Uiso 1 1 calc R U . . .
H15B H 0.136721 -0.123506 0.384104 0.246 Uiso 1 1 calc R U . . .
C54 C 0.1192(12) 0.0072(10) 0.3129(11) 0.233(7) Uani 1 1 d D U . . .
H54A H 0.161362 0.065056 0.372921 0.280 Uiso 1 1 calc R U . . .
H54B H 0.051408 0.022667 0.265392 0.280 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
O15 C2 1.371(4) . ?
O15 C14 1.380(3) . ?
C7 C2 1.383(5) . ?
C7 C8 1.541(4) . ?
C7 C6 1.389(4) . ?
C2 C3 1.406(4) . ?
C8 C9 1.530(4) . ?
C8 C53 1.513(6) . ?
C8 C52 1.515(5) . ?
C9 C14 1.381(5) . ?
C9 C10 1.393(4) . ?
C5 C6 1.390(4) . ?
C5 C4 1.394(5) . ?
C5 C44 1.538(4) . ?
C3 C16 1.498(5) . ?
C3 C4 1.384(4) . ?
C14 C13 1.404(4) . ?
C13 C30 1.496(5) . ?
C13 C12 1.388(4) . ?
C25 C16 1.398(6) . ?
C25 C24 1.444(5) . ?
C25 C26 1.435(6) . ?
C10 C11 1.400(4) . ?
C30 C39 1.424(6) . ?
C30 C31 1.385(6) . ?
C16 C17 1.410(6) . ?
C11 C12 1.382(5) . ?
C11 C48 1.547(4) . ?
C39 C38 1.428(5) . ?
C39 C40 1.427(6) . ?
C17 C22 1.442(6) . ?
C17 C18 1.416(7) . ?
C24 C23 1.376(7) . ?
C24 C29 1.437(7) . ?
C48 C49 1.550(7) . ?
C48 C50 1.518(6) . ?
C48 C51 1.499(7) . ?
C38 C37 1.397(7) . ?
C38 C43 1.435(7) . ?
C31 C36 1.443(5) . ?
C31 C32 1.428(7) . ?
C44 C45 1.512(6) . ?
C44 C46 1.519(7) . ?
C44 C47 1.538(7) . ?
C22 C23 1.386(7) . ?
C22 C21 1.425(7) . ?
C26 C27 1.327(7) . ?
C36 C37 1.382(7) . ?
C36 C35 1.426(7) . ?
C40 C41 1.376(7) . ?
C29 C28 1.368(8) . ?
C18 C19 1.330(7) . ?
C43 C42 1.359(8) . ?
C32 C33 1.366(8) . ?
C28 C27 1.414(8) . ?
C21 C20 1.369(8) . ?
C41 C42 1.425(8) . ?
C35 C34 1.377(9) . ?
C19 C20 1.420(8) . ?
C33 C34 1.387(9) . ?
Br1 C54 1.976(9) . ?
C1 C15 1.518(9) . ?
C15 C54 1.560(9) . ?

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
C2 O15 C14 118.3(3) . . ?
C2 C7 C8 122.6(3) . . ?
C2 C7 C6 118.1(3) . . ?
C6 C7 C8 119.4(3) . . ?
O15 C2 C7 123.8(2) . . ?
O15 C2 C3 114.8(3) . . ?
C7 C2 C3 121.4(3) . . ?
C9 C8 C7 108.7(3) . . ?
C53 C8 C7 109.3(3) . . ?
C53 C8 C9 109.2(3) . . ?
C53 C8 C52 110.3(3) . . ?
C52 C8 C7 109.6(3) . . ?
C52 C8 C9 109.7(3) . . ?
C14 C9 C8 123.1(2) . . ?
C14 C9 C10 117.3(3) . . ?
C10 C9 C8 119.5(3) . . ?
C6 C5 C4 117.0(3) . . ?
C6 C5 C44 120.4(3) . . ?
C4 C5 C44 122.7(3) . . ?
C2 C3 C16 121.2(3) . . ?
C4 C3 C2 118.1(3) . . ?
C4 C3 C16 120.7(3) . . ?
O15 C14 C9 123.4(3) . . ?
O15 C14 C13 114.3(3) . . ?
C9 C14 C13 122.2(3) . . ?
C14 C13 C30 122.4(3) . . ?
C12 C13 C14 117.7(3) . . ?
C12 C13 C30 119.9(3) . . ?
C16 C25 C24 118.7(4) . . ?
C16 C25 C26 124.5(4) . . ?
C26 C25 C24 116.8(4) . . ?
C9 C10 C11 122.9(3) . . ?
C7 C6 C5 122.9(3) . . ?
C39 C30 C13 118.0(4) . . ?
C31 C30 C13 121.4(4) . . ?
C31 C30 C39 120.5(3) . . ?
C25 C16 C3 119.2(4) . . ?
C25 C16 C17 121.3(3) . . ?
C17 C16 C3 119.5(4) . . ?
C10 C11 C48 119.3(3) . . ?
C12 C11 C10 117.1(3) . . ?
C12 C11 C48 123.7(3) . . ?
C30 C39 C38 119.1(4) . . ?
C30 C39 C40 123.1(4) . . ?
C40 C39 C38 117.8(4) . . ?
C3 C4 C5 122.5(3) . . ?
C11 C12 C13 122.7(3) . . ?
C16 C17 C22 118.7(4) . . ?
C16 C17 C18 124.1(4) . . ?
C18 C17 C22 117.2(4) . . ?
C23 C24 C25 120.0(4) . . ?
C23 C24 C29 121.7(4) . . ?
C29 C24 C25 118.3(4) . . ?
C11 C48 C49 108.9(3) . . ?
C50 C48 C11 111.7(3) . . ?
C50 C48 C49 107.8(4) . . ?
C51 C48 C11 108.7(3) . . ?
C51 C48 C49 109.7(5) . . ?
C51 C48 C50 110.1(4) . . ?
C39 C38 C43 119.6(5) . . ?
C37 C38 C39 119.7(4) . . ?
C37 C38 C43 120.7(4) . . ?
C30 C31 C36 119.5(4) . . ?
C30 C31 C32 123.7(4) . . ?
C32 C31 C36 116.8(4) . . ?
C5 C44 C47 109.8(3) . . ?
C45 C44 C5 113.0(3) . . ?
C45 C44 C46 108.6(4) . . ?
C45 C44 C47 107.0(4) . . ?
C46 C44 C5 109.1(3) . . ?
C46 C44 C47 109.2(5) . . ?
C23 C22 C17 119.7(4) . . ?
C23 C22 C21 121.1(4) . . ?
C21 C22 C17 119.1(5) . . ?
C27 C26 C25 123.3(5) . . ?
C37 C36 C31 119.9(4) . . ?
C37 C36 C35 121.1(4) . . ?
C35 C36 C31 119.0(5) . . ?
C41 C40 C39 121.3(5) . . ?
C24 C23 C22 121.7(4) . . ?
C36 C37 C38 121.1(4) . . ?
C28 C29 C24 121.0(5) . . ?
C19 C18 C17 122.4(5) . . ?
C42 C43 C38 120.8(5) . . ?
C33 C32 C31 122.2(5) . . ?
C29 C28 C27 120.2(5) . . ?
C26 C27 C28 120.4(5) . . ?
C20 C21 C22 120.6(5) . . ?
C40 C41 C42 120.4(5) . . ?
C43 C42 C41 120.1(5) . . ?
C34 C35 C36 121.1(5) . . ?
C18 C19 C20 121.3(6) . . ?
C32 C33 C34 120.8(6) . . ?
C21 C20 C19 119.4(6) . . ?
C35 C34 C33 120.0(6) . . ?
C1 C15 C54 104.5(7) . . ?
C15 C54 Br1 107.6(7) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.417
_oxdiff_exptl_absorpt_empirical_full_min 0.131
####################################################################### 
# 
# 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_20221209-lqy-1_auto
_database_code_depnum_ccdc_archive 'CCDC 2308248'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2023-11-15 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2023-11-15
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H5 I1, C51 H46 O'
_chemical_formula_sum            'C53 H51 I O'
_chemical_formula_weight         830.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHOI
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'
I I -0.3257 6.8362 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.8029(2)
_cell_length_b                   13.1018(2)
_cell_length_c                   15.0559(3)
_cell_angle_alpha                93.947(2)
_cell_angle_beta                 113.886(2)
_cell_angle_gamma                108.270(2)
_cell_volume                     2136.31(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13256
_cell_measurement_temperature    302.47(10)
_cell_measurement_theta_max      75.1660
_cell_measurement_theta_min      3.2650
_shelx_estimated_absorpt_T_max   0.578
_shelx_estimated_absorpt_T_min   0.458
_exptl_absorpt_coefficient_mu    6.160
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26596
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.295
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      302.47(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00  61.00   0.50    0.20    --   76.75-125.00  30.00   52
  2  ω     71.00  97.00   0.50    0.20    --   76.75-125.00  30.00   52
  3  ω     41.00  96.00   0.50    0.20    --   77.87-120.00  -8.23  110
  4  ω     49.00  75.00   0.50    0.20    --   76.75-125.00 -30.00   52
  5  ω     28.00  65.00   0.50    0.20    --   62.89-125.00 -30.00   74
  6  ω     47.00  96.00   0.50    0.20    --   76.75-125.00 -90.00   98
  7  ω     52.00  98.00   0.50    0.20    --   76.75-125.00-150.00   92
  8  ω     52.00 102.00   0.50    0.20    --   62.89  15.00-180.00  100
  9  ω     63.00 110.00   0.50    0.20    --   72.93  15.00 120.00   94
 10  ω   -106.00 -61.00   0.50    0.20    --  -63.72 -15.00 -90.00   90
 11  ω    -88.00 -63.00   0.50    0.20    --  -71.74 -15.00-120.00   50
 12  ω    -99.00 -57.00   0.50    0.20    --  -63.72 -15.00 -30.00   84
 13  ω    -98.00 -72.00   0.50    0.20    --  -76.43 -15.00-150.00   52
 14  ω    -91.00 -54.00   0.50    0.20    --  -63.72 -15.00   0.00   74
 15  ω   -114.00 -64.00   0.50    0.20    --  -71.74 -15.00  60.00  100
 16  ω   -119.00 -83.00   0.50    0.20    --  -76.43 -15.00 120.00   72
 17  ω    -85.00 -59.00   0.50    0.20    --  -63.72 -15.00 120.00   52
 18  ω   -125.00 -79.00   0.50    0.20    --  -81.49 -15.00 150.00   92
 19  ω   -124.00 -74.00   0.50    0.20    --  -81.49 -15.00 -60.00  100
 20  ω   -125.00 -77.00   0.50    0.20    --  -81.49 -15.00-120.00   96
 21  ω   -118.00 -66.00   0.50    0.20    --  -76.43 -15.00-180.00  104
 22  ω   -102.00 -43.00   0.50    0.20    --  -81.49 125.00-150.00  118
 23  ω    -53.00 -26.00   0.50    0.20    --  -63.72 125.00-180.00   54
 24  ω    -72.00 -29.00   0.50    0.20    --  -71.74 125.00 -30.00   86
 25  ω    -94.00 -52.00   0.50    0.20    --  -76.43 125.00   0.00   84
 26  ω   -102.00 -41.00   0.50    0.20    --  -81.49 125.00  60.00  122
 27  ω    -97.00 -34.00   0.50    0.20    --  -76.43 125.00  90.00  126
 28  ω   -101.00 -75.00   0.50    0.20    --  -81.49 125.00 120.00   52
 29  ω    -68.00 -40.00   0.50    0.20    --  -81.49 125.00 120.00   56
 30  ω   -102.00 -47.00   0.50    0.20    --  -81.49 125.00 150.00  110
 31  ω   -100.00 -74.00   0.50    0.20    --  -81.49 125.00  90.00   52
 32  ω   -102.00 -40.00   0.50    0.20    --  -81.49 125.00  30.00  124
 33  ω    -68.00 -42.00   0.50    0.20    --  -81.49 125.00   0.00   52
 34  ω   -102.00 -77.00   0.50    0.20    --  -81.49 125.00   0.00   50
 35  ω   -101.00 -43.00   0.50    0.20    --  -81.49 125.00 -60.00  116
 36  ω   -102.00 -77.00   0.50    0.20    --  -81.49 125.00 -90.00   50
 37  ω   -102.00 -76.00   0.50    0.20    --  -81.49 125.00-180.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0399536000
_diffrn_orient_matrix_UB_12      -0.0015498000
_diffrn_orient_matrix_UB_13      0.0837946000
_diffrn_orient_matrix_UB_21      -0.0819452000
_diffrn_orient_matrix_UB_22      -0.1231714000
_diffrn_orient_matrix_UB_23      -0.0442770000
_diffrn_orient_matrix_UB_31      0.1087549000
_diffrn_orient_matrix_UB_32      -0.0313132000
_diffrn_orient_matrix_UB_33      0.0648990000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5762
_reflns_number_total             7478
_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       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.279
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.0019(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         7478
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0890
_refine_ls_restrained_S_all      1.126
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2625
_refine_ls_wR_factor_ref         0.2771
_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. Restrained distances
 C52-C53
 1.54 with sigma of 0.02
 C52-I1'
 2.13 with sigma of 0.02
 C52'-I1
 2.13 with sigma of 0.02
 C52'-C53'
 1.54 with sigma of 0.02
 C53'-C52'
 1.54 with sigma of 0.01
 I1'-C52 \\sim I1-C52'
 with sigma of 0.02
 I1'-C53 \\sim I1-C53'
 with sigma of 0.04
 C53-C52 \\sim C53'-C52'
 with sigma of 0.02
3. Others
 Sof(I1)=Sof(C52')=Sof(H52A)=Sof(H52B)=Sof(C53')=Sof(H53A)=Sof(H53B)=Sof(H53C)=
 1-FVAR(1)
 Sof(I1')=Sof(C52)=Sof(H52C)=Sof(H52D)=Sof(C53)=Sof(H53D)=Sof(H53E)=Sof(H53F)=
 FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C52(H52C,H52D), C52'(H52A,H52B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C10(H10), C15(H15), C16(H16), C17(H17), C18(H18),
 C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C29(H29), C30(H30), C31(H31),
  C32(H32), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39)
4.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C), C53(H53D,H53E,H53F), C53'(H53A,H53B,H53C)
;
_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
I1 I 0.2899(2) -0.0154(5) 0.2117(4) 0.1855(15) Uani 0.493(7) 1 d D . P A 2
I1' I 0.3165(3) 0.0472(4) 0.24216(14) 0.1446(11) Uani 0.507(7) 1 d D . P A 1
O1 O 0.23109(17) 0.49667(13) 0.25225(14) 0.0454(5) Uani 1 1 d . . . . .
C1 C 0.2303(2) 0.57948(19) 0.31328(19) 0.0387(5) Uani 1 1 d . . . . .
C2 C 0.3165(2) 0.68418(19) 0.3297(2) 0.0414(6) Uani 1 1 d . . . . .
C3 C 0.3200(2) 0.77216(19) 0.3899(2) 0.0424(6) Uani 1 1 d . . . . .
H3 H 0.377017 0.842394 0.401327 0.051 Uiso 1 1 calc R U . . .
C4 C 0.2403(2) 0.75783(19) 0.43364(19) 0.0414(6) Uani 1 1 d . . . . .
C5 C 0.1572(2) 0.65231(19) 0.41485(19) 0.0400(5) Uani 1 1 d . . . . .
H5 H 0.103361 0.641456 0.443333 0.048 Uiso 1 1 calc R U . . .
C6 C 0.1494(2) 0.56103(19) 0.35551(18) 0.0377(5) Uani 1 1 d . . . . .
C7 C 0.0661(2) 0.36161(19) 0.27197(18) 0.0378(5) Uani 1 1 d . . . . .
C8 C -0.0100(2) 0.25080(19) 0.24735(19) 0.0399(5) Uani 1 1 d . . . . .
H8 H -0.066168 0.230364 0.273377 0.048 Uiso 1 1 calc R U . . .
C9 C -0.0063(2) 0.16939(19) 0.18607(19) 0.0410(6) Uani 1 1 d . . . . .
C10 C 0.0797(2) 0.2024(2) 0.1486(2) 0.0419(6) Uani 1 1 d . . . . .
H10 H 0.084373 0.149708 0.107286 0.050 Uiso 1 1 calc R U . . .
C11 C 0.1583(2) 0.3116(2) 0.1713(2) 0.0401(6) Uani 1 1 d . . . . .
C12 C 0.1505(2) 0.39068(19) 0.23345(19) 0.0378(5) Uani 1 1 d . . . . .
C13 C 0.4068(2) 0.70465(19) 0.2871(2) 0.0419(6) Uani 1 1 d . . . . .
C14 C 0.5326(2) 0.73352(19) 0.3516(2) 0.0439(6) Uani 1 1 d . . . . .
C15 C 0.5782(3) 0.7341(2) 0.4558(2) 0.0558(7) Uani 1 1 d . . . . .
H15 H 0.523071 0.713849 0.482799 0.067 Uiso 1 1 calc R U . . .
C16 C 0.7006(3) 0.7635(3) 0.5157(3) 0.0686(9) Uani 1 1 d . . . . .
H16 H 0.727800 0.762721 0.583003 0.082 Uiso 1 1 calc R U . . .
C17 C 0.7873(3) 0.7955(3) 0.4772(3) 0.0701(9) Uani 1 1 d . . . . .
H17 H 0.870840 0.816395 0.519380 0.084 Uiso 1 1 calc R U . . .
C18 C 0.7488(3) 0.7956(3) 0.3794(3) 0.0658(9) Uani 1 1 d . . . . .
H18 H 0.806565 0.816369 0.354977 0.079 Uiso 1 1 calc R U . . .
C19 C 0.6213(3) 0.7646(2) 0.3129(2) 0.0503(7) Uani 1 1 d . . . . .
C20 C 0.5810(3) 0.7660(2) 0.2126(3) 0.0564(7) Uani 1 1 d . . . . .
H20 H 0.638971 0.789055 0.188544 0.068 Uiso 1 1 calc R U . . .
C21 C 0.4569(3) 0.7341(2) 0.1470(2) 0.0525(7) Uani 1 1 d . . . . .
C22 C 0.4172(4) 0.7362(3) 0.0440(3) 0.0702(9) Uani 1 1 d . . . . .
H22 H 0.475207 0.759195 0.020039 0.084 Uiso 1 1 calc R U . . .
C23 C 0.2963(4) 0.7052(4) -0.0190(3) 0.0801(11) Uani 1 1 d . . . . .
H23 H 0.271763 0.706195 -0.086045 0.096 Uiso 1 1 calc R U . . .
C24 C 0.2064(4) 0.6712(4) 0.0163(3) 0.0794(11) Uani 1 1 d . . . . .
H24 H 0.123402 0.649823 -0.027768 0.095 Uiso 1 1 calc R U . . .
C25 C 0.2409(3) 0.6695(3) 0.1143(2) 0.0616(8) Uani 1 1 d . . . . .
H25 H 0.180674 0.646774 0.136131 0.074 Uiso 1 1 calc R U . . .
C26 C 0.3669(3) 0.7018(2) 0.1840(2) 0.0473(6) Uani 1 1 d . . . . .
C27 C 0.2490(2) 0.34307(19) 0.1296(2) 0.0413(6) Uani 1 1 d . . . . .
C28 C 0.3760(3) 0.3746(2) 0.1934(2) 0.0481(6) Uani 1 1 d . . . . .
C29 C 0.4243(3) 0.3827(3) 0.2978(3) 0.0627(8) Uani 1 1 d . . . . .
H29 H 0.370865 0.369171 0.326691 0.075 Uiso 1 1 calc R U . . .
C30 C 0.5468(4) 0.4098(4) 0.3568(3) 0.0842(12) Uani 1 1 d . . . . .
H30 H 0.575709 0.415574 0.425109 0.101 Uiso 1 1 calc R U . . .
C31 C 0.6299(4) 0.4291(4) 0.3153(4) 0.0879(12) Uani 1 1 d . . . . .
H31 H 0.712821 0.444425 0.355859 0.105 Uiso 1 1 calc R U . . .
C32 C 0.5889(3) 0.4253(3) 0.2151(4) 0.0775(11) Uani 1 1 d . . . . .
H32 H 0.644836 0.440828 0.188570 0.093 Uiso 1 1 calc R U . . .
C33 C 0.4624(3) 0.3979(2) 0.1519(3) 0.0542(7) Uani 1 1 d . . . . .
C34 C 0.4181(3) 0.3914(3) 0.0498(3) 0.0609(8) Uani 1 1 d . . . . .
H34 H 0.473953 0.407390 0.023270 0.073 Uiso 1 1 calc R U . . .
C35 C 0.2942(3) 0.3621(2) -0.0139(2) 0.0529(7) Uani 1 1 d . . . . .
C36 C 0.2496(4) 0.3541(3) -0.1187(3) 0.0669(9) Uani 1 1 d . . . . .
H36 H 0.305347 0.369810 -0.145350 0.080 Uiso 1 1 calc R U . . .
C37 C 0.1290(4) 0.3245(3) -0.1798(3) 0.0726(10) Uani 1 1 d . . . . .
H37 H 0.102296 0.319399 -0.247869 0.087 Uiso 1 1 calc R U . . .
C38 C 0.0423(4) 0.3009(3) -0.1407(3) 0.0682(9) Uani 1 1 d . . . . .
H38 H -0.040963 0.280664 -0.183382 0.082 Uiso 1 1 calc R U . . .
C39 C 0.0799(3) 0.3076(3) -0.0411(2) 0.0574(7) Uani 1 1 d . . . . .
H39 H 0.021642 0.292523 -0.016931 0.069 Uiso 1 1 calc R U . . .
C40 C 0.2061(3) 0.33707(19) 0.0265(2) 0.0444(6) Uani 1 1 d . . . . .
C41 C 0.0570(2) 0.44646(19) 0.34027(19) 0.0379(5) Uani 1 1 d . . . . .
C42 C -0.0739(2) 0.4472(2) 0.2936(2) 0.0492(7) Uani 1 1 d . . . . .
H42A H -0.079061 0.501530 0.336156 0.074 Uiso 1 1 calc R U . . .
H42B H -0.131897 0.375781 0.286078 0.074 Uiso 1 1 calc R U . . .
H42C H -0.092597 0.464845 0.229460 0.074 Uiso 1 1 calc R U . . .
C43 C 0.0857(3) 0.4156(2) 0.4420(2) 0.0507(7) Uani 1 1 d . . . . .
H43A H 0.167619 0.415498 0.471370 0.076 Uiso 1 1 calc R U . . .
H43B H 0.027747 0.343590 0.432993 0.076 Uiso 1 1 calc R U . . .
H43C H 0.079563 0.468582 0.485081 0.076 Uiso 1 1 calc R U . . .
C44 C 0.2437(3) 0.8543(2) 0.5011(2) 0.0484(6) Uani 1 1 d . . . . .
C45 C 0.3504(5) 0.9610(3) 0.5228(4) 0.0881(14) Uani 1 1 d . . . . .
H45A H 0.341146 0.983801 0.461719 0.132 Uiso 1 1 calc R U . . .
H45B H 0.426491 0.949399 0.552787 0.132 Uiso 1 1 calc R U . . .
H45C H 0.351060 1.017193 0.567677 0.132 Uiso 1 1 calc R U . . .
C46 C 0.1206(5) 0.8681(4) 0.4536(4) 0.0985(17) Uani 1 1 d . . . . .
H46A H 0.118160 0.921471 0.498969 0.148 Uiso 1 1 calc R U . . .
H46B H 0.055139 0.798603 0.438688 0.148 Uiso 1 1 calc R U . . .
H46C H 0.110643 0.892785 0.393192 0.148 Uiso 1 1 calc R U . . .
C47 C 0.2617(5) 0.8258(3) 0.6017(3) 0.0827(12) Uani 1 1 d . . . . .
H47A H 0.336960 0.812819 0.631629 0.124 Uiso 1 1 calc R U . . .
H47B H 0.193738 0.760572 0.591991 0.124 Uiso 1 1 calc R U . . .
H47C H 0.265709 0.885973 0.644732 0.124 Uiso 1 1 calc R U . . .
C48 C -0.0921(3) 0.04824(19) 0.1637(2) 0.0481(6) Uani 1 1 d . . . . .
C49 C -0.2247(3) 0.0411(3) 0.1324(4) 0.0797(11) Uani 1 1 d . . . . .
H49A H -0.279296 -0.034905 0.110881 0.119 Uiso 1 1 calc R U . . .
H49B H -0.248208 0.077736 0.078694 0.119 Uiso 1 1 calc R U . . .
H49C H -0.229392 0.076100 0.188080 0.119 Uiso 1 1 calc R U . . .
C50 C -0.0488(5) 0.0042(3) 0.2566(3) 0.0961(15) Uani 1 1 d . . . . .
H50A H -0.052900 0.046310 0.309037 0.144 Uiso 1 1 calc R U . . .
H50B H 0.034646 0.010192 0.276789 0.144 Uiso 1 1 calc R U . . .
H50C H -0.100660 -0.071754 0.243024 0.144 Uiso 1 1 calc R U . . .
C51 C -0.0933(4) -0.0239(3) 0.0796(3) 0.0793(11) Uani 1 1 d . . . . .
H51A H -0.148795 -0.098158 0.067361 0.119 Uiso 1 1 calc R U . . .
H51B H -0.011837 -0.022946 0.097985 0.119 Uiso 1 1 calc R U . . .
H51C H -0.119957 0.003853 0.020297 0.119 Uiso 1 1 calc R U . . .
C52 C 0.4235(10) -0.0019(8) 0.1694(7) 0.156(9) Uani 0.507(7) 1 d D . P A 1
H52C H 0.487413 -0.022871 0.216058 0.187 Uiso 0.507(7) 1 calc R U P A 1
H52D H 0.369417 -0.062508 0.111559 0.187 Uiso 0.507(7) 1 calc R U P A 1
C52' C 0.4122(11) 0.1119(9) 0.1687(10) 0.26(2) Uani 0.493(7) 1 d D . P A 2
H52A H 0.362771 0.139212 0.115428 0.310 Uiso 0.493(7) 1 calc R U P A 2
H52B H 0.468166 0.173580 0.225335 0.310 Uiso 0.493(7) 1 calc R U P A 2
C53 C 0.4795(14) 0.1046(12) 0.1391(12) 0.086(5) Uani 0.507(7) 1 d D . P A 1
H53D H 0.497640 0.086098 0.085663 0.129 Uiso 0.507(7) 1 calc R U P A 1
H53E H 0.553892 0.153187 0.195324 0.129 Uiso 0.507(7) 1 calc R U P A 1
H53F H 0.421585 0.140560 0.117660 0.129 Uiso 0.507(7) 1 calc R U P A 1
C53' C 0.4858(15) 0.0613(13) 0.1339(13) 0.074(5) Uani 0.493(7) 1 d D . P A 2
H53A H 0.430459 0.005233 0.073857 0.112 Uiso 0.493(7) 1 calc R U P A 2
H53B H 0.529390 0.029181 0.184785 0.112 Uiso 0.493(7) 1 calc R U P A 2
H53C H 0.543531 0.117712 0.121159 0.112 Uiso 0.493(7) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C52' 2.233(12) . ?
I1' C52 2.271(11) . ?
O1 C1 1.378(3) . ?
O1 C12 1.373(3) . ?
C1 C2 1.394(3) . ?
C1 C6 1.390(4) . ?
C2 C3 1.394(3) . ?
C2 C13 1.500(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.397(4) . ?
C4 C5 1.380(3) . ?
C4 C44 1.544(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.394(3) . ?
C6 C41 1.524(3) . ?
C7 C8 1.393(3) . ?
C7 C12 1.389(4) . ?
C7 C41 1.526(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.387(3) . ?
C9 C10 1.398(4) . ?
C9 C48 1.541(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.388(3) . ?
C11 C12 1.402(3) . ?
C11 C27 1.496(4) . ?
C13 C14 1.407(4) . ?
C13 C26 1.417(4) . ?
C14 C15 1.434(4) . ?
C14 C19 1.440(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.358(5) . ?
C16 H16 0.9300 . ?
C16 C17 1.416(6) . ?
C17 H17 0.9300 . ?
C17 C18 1.351(6) . ?
C18 H18 0.9300 . ?
C18 C19 1.427(5) . ?
C19 C20 1.387(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.389(5) . ?
C21 C22 1.429(5) . ?
C21 C26 1.437(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.351(6) . ?
C23 H23 0.9300 . ?
C23 C24 1.418(6) . ?
C24 H24 0.9300 . ?
C24 C25 1.363(5) . ?
C25 H25 0.9300 . ?
C25 C26 1.423(4) . ?
C27 C28 1.413(4) . ?
C27 C40 1.408(4) . ?
C28 C29 1.418(5) . ?
C28 C33 1.443(4) . ?
C29 H29 0.9300 . ?
C29 C30 1.361(5) . ?
C30 H30 0.9300 . ?
C30 C31 1.406(7) . ?
C31 H31 0.9300 . ?
C31 C32 1.374(7) . ?
C32 H32 0.9300 . ?
C32 C33 1.414(5) . ?
C33 C34 1.392(5) . ?
C34 H34 0.9300 . ?
C34 C35 1.385(5) . ?
C35 C36 1.427(5) . ?
C35 C40 1.449(4) . ?
C36 H36 0.9300 . ?
C36 C37 1.343(6) . ?
C37 H37 0.9300 . ?
C37 C38 1.419(6) . ?
C38 H38 0.9300 . ?
C38 C39 1.362(5) . ?
C39 H39 0.9300 . ?
C39 C40 1.421(5) . ?
C41 C42 1.537(3) . ?
C41 C43 1.538(4) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 C45 1.518(5) . ?
C44 C46 1.521(5) . ?
C44 C47 1.528(5) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 C49 1.536(5) . ?
C48 C50 1.509(5) . ?
C48 C51 1.519(4) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52C 0.9700 . ?
C52 H52D 0.9700 . ?
C52 C53 1.547(13) . ?
C52' H52A 0.9700 . ?
C52' H52B 0.9700 . ?
C52' C53' 1.532(8) . ?
C53 H53D 0.9600 . ?
C53 H53E 0.9600 . ?
C53 H53F 0.9600 . ?
C53' H53A 0.9600 . ?
C53' H53B 0.9600 . ?
C53' H53C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 O1 C1 119.05(19) . . ?
O1 C1 C2 115.2(2) . . ?
O1 C1 C6 122.9(2) . . ?
C6 C1 C2 121.9(2) . . ?
C1 C2 C3 118.3(2) . . ?
C1 C2 C13 122.5(2) . . ?
C3 C2 C13 119.2(2) . . ?
C2 C3 H3 119.1 . . ?
C2 C3 C4 121.9(2) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C44 122.5(2) . . ?
C5 C4 C3 117.2(2) . . ?
C5 C4 C44 120.3(2) . . ?
C4 C5 H5 118.2 . . ?
C4 C5 C6 123.6(2) . . ?
C6 C5 H5 118.2 . . ?
C1 C6 C5 117.1(2) . . ?
C1 C6 C41 122.4(2) . . ?
C5 C6 C41 120.5(2) . . ?
C8 C7 C41 120.4(2) . . ?
C12 C7 C8 117.6(2) . . ?
C12 C7 C41 121.9(2) . . ?
C7 C8 H8 118.3 . . ?
C9 C8 C7 123.4(2) . . ?
C9 C8 H8 118.3 . . ?
C8 C9 C10 117.0(2) . . ?
C8 C9 C48 120.3(2) . . ?
C10 C9 C48 122.7(2) . . ?
C9 C10 H10 119.0 . . ?
C11 C10 C9 121.9(2) . . ?
C11 C10 H10 119.0 . . ?
C10 C11 C12 118.8(2) . . ?
C10 C11 C27 120.1(2) . . ?
C12 C11 C27 121.2(2) . . ?
O1 C12 C7 123.5(2) . . ?
O1 C12 C11 115.3(2) . . ?
C7 C12 C11 121.2(2) . . ?
C14 C13 C2 119.3(2) . . ?
C14 C13 C26 120.3(2) . . ?
C26 C13 C2 120.3(2) . . ?
C13 C14 C15 123.0(3) . . ?
C13 C14 C19 119.5(3) . . ?
C15 C14 C19 117.4(3) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 C14 121.2(3) . . ?
C16 C15 H15 119.4 . . ?
C15 C16 H16 119.6 . . ?
C15 C16 C17 120.9(4) . . ?
C17 C16 H16 119.6 . . ?
C16 C17 H17 119.9 . . ?
C18 C17 C16 120.1(3) . . ?
C18 C17 H17 119.9 . . ?
C17 C18 H18 119.3 . . ?
C17 C18 C19 121.3(3) . . ?
C19 C18 H18 119.3 . . ?
C18 C19 C14 119.0(3) . . ?
C20 C19 C14 119.3(3) . . ?
C20 C19 C18 121.8(3) . . ?
C19 C20 H20 119.0 . . ?
C19 C20 C21 122.1(3) . . ?
C21 C20 H20 119.0 . . ?
C20 C21 C22 121.3(3) . . ?
C20 C21 C26 119.4(3) . . ?
C22 C21 C26 119.2(3) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.8(3) . . ?
C23 C22 H22 119.6 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.5(4) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.5(4) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 119.3 . . ?
C24 C25 C26 121.4(3) . . ?
C26 C25 H25 119.3 . . ?
C13 C26 C21 119.3(3) . . ?
C13 C26 C25 123.2(3) . . ?
C25 C26 C21 117.6(3) . . ?
C28 C27 C11 119.7(2) . . ?
C40 C27 C11 119.4(2) . . ?
C40 C27 C28 120.8(2) . . ?
C27 C28 C29 123.2(3) . . ?
C27 C28 C33 119.5(3) . . ?
C29 C28 C33 117.3(3) . . ?
C28 C29 H29 119.1 . . ?
C30 C29 C28 121.8(3) . . ?
C30 C29 H29 119.1 . . ?
C29 C30 H30 119.7 . . ?
C29 C30 C31 120.6(4) . . ?
C31 C30 H30 119.7 . . ?
C30 C31 H31 119.9 . . ?
C32 C31 C30 120.2(4) . . ?
C32 C31 H31 119.9 . . ?
C31 C32 H32 119.7 . . ?
C31 C32 C33 120.5(3) . . ?
C33 C32 H32 119.7 . . ?
C32 C33 C28 119.6(3) . . ?
C34 C33 C28 118.7(3) . . ?
C34 C33 C32 121.7(3) . . ?
C33 C34 H34 118.6 . . ?
C35 C34 C33 122.7(3) . . ?
C35 C34 H34 118.6 . . ?
C34 C35 C36 122.3(3) . . ?
C34 C35 C40 119.2(3) . . ?
C36 C35 C40 118.5(3) . . ?
C35 C36 H36 119.2 . . ?
C37 C36 C35 121.6(3) . . ?
C37 C36 H36 119.2 . . ?
C36 C37 H37 119.9 . . ?
C36 C37 C38 120.2(3) . . ?
C38 C37 H37 119.9 . . ?
C37 C38 H38 119.7 . . ?
C39 C38 C37 120.7(4) . . ?
C39 C38 H38 119.7 . . ?
C38 C39 H39 119.3 . . ?
C38 C39 C40 121.4(3) . . ?
C40 C39 H39 119.3 . . ?
C27 C40 C35 119.0(3) . . ?
C27 C40 C39 123.4(3) . . ?
C39 C40 C35 117.6(3) . . ?
C6 C41 C7 110.24(19) . . ?
C6 C41 C42 109.41(19) . . ?
C6 C41 C43 109.0(2) . . ?
C7 C41 C42 109.6(2) . . ?
C7 C41 C43 109.19(19) . . ?
C42 C41 C43 109.4(2) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C45 C44 C4 112.7(2) . . ?
C45 C44 C46 111.7(3) . . ?
C45 C44 C47 106.5(3) . . ?
C46 C44 C4 109.0(2) . . ?
C46 C44 C47 107.9(4) . . ?
C47 C44 C4 108.9(2) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C49 C48 C9 109.8(2) . . ?
C50 C48 C9 108.8(2) . . ?
C50 C48 C49 109.6(4) . . ?
C50 C48 C51 108.8(3) . . ?
C51 C48 C9 112.2(2) . . ?
C51 C48 C49 107.6(3) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C48 C51 H51A 109.5 . . ?
C48 C51 H51B 109.5 . . ?
C48 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
I1' C52 H52C 111.2 . . ?
I1' C52 H52D 111.2 . . ?
H52C C52 H52D 109.1 . . ?
C53 C52 I1' 102.9(7) . . ?
C53 C52 H52C 111.2 . . ?
C53 C52 H52D 111.2 . . ?
I1 C52' H52A 109.7 . . ?
I1 C52' H52B 109.7 . . ?
H52A C52' H52B 108.2 . . ?
C53' C52' I1 109.6(8) . . ?
C53' C52' H52A 109.7 . . ?
C53' C52' H52B 109.7 . . ?
C52 C53 H53D 109.5 . . ?
C52 C53 H53E 109.5 . . ?
C52 C53 H53F 109.5 . . ?
H53D C53 H53E 109.5 . . ?
H53D C53 H53F 109.5 . . ?
H53E C53 H53F 109.5 . . ?
C52' C53' H53A 109.5 . . ?
C52' C53' H53B 109.5 . . ?
C52' C53' H53C 109.5 . . ?
H53A C53' H53B 109.5 . . ?
H53A C53' H53C 109.5 . . ?
H53B C53' H53C 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 179.4(2) . . . . ?
O1 C1 C2 C13 -2.2(4) . . . . ?
O1 C1 C6 C5 -179.2(2) . . . . ?
O1 C1 C6 C41 1.9(4) . . . . ?
C1 O1 C12 C7 0.7(3) . . . . ?
C1 O1 C12 C11 -179.5(2) . . . . ?
C1 C2 C3 C4 0.1(4) . . . . ?
C1 C2 C13 C14 -110.4(3) . . . . ?
C1 C2 C13 C26 73.5(3) . . . . ?
C1 C6 C41 C7 -1.7(3) . . . . ?
C1 C6 C41 C42 -122.3(3) . . . . ?
C1 C6 C41 C43 118.2(3) . . . . ?
C2 C1 C6 C5 0.5(4) . . . . ?
C2 C1 C6 C41 -178.4(2) . . . . ?
C2 C3 C4 C5 0.0(4) . . . . ?
C2 C3 C4 C44 179.6(2) . . . . ?
C2 C13 C14 C15 6.3(3) . . . . ?
C2 C13 C14 C19 -173.5(2) . . . . ?
C2 C13 C26 C21 172.8(2) . . . . ?
C2 C13 C26 C25 -6.4(4) . . . . ?
C3 C2 C13 C14 68.0(3) . . . . ?
C3 C2 C13 C26 -108.0(3) . . . . ?
C3 C4 C5 C6 0.1(4) . . . . ?
C3 C4 C44 C45 -6.2(4) . . . . ?
C3 C4 C44 C46 118.3(4) . . . . ?
C3 C4 C44 C47 -124.1(3) . . . . ?
C4 C5 C6 C1 -0.4(4) . . . . ?
C4 C5 C6 C41 178.5(2) . . . . ?
C5 C4 C44 C45 173.3(3) . . . . ?
C5 C4 C44 C46 -62.2(4) . . . . ?
C5 C4 C44 C47 55.4(4) . . . . ?
C5 C6 C41 C7 179.5(2) . . . . ?
C5 C6 C41 C42 58.9(3) . . . . ?
C5 C6 C41 C43 -60.7(3) . . . . ?
C6 C1 C2 C3 -0.3(4) . . . . ?
C6 C1 C2 C13 178.1(2) . . . . ?
C7 C8 C9 C10 0.4(4) . . . . ?
C7 C8 C9 C48 179.0(2) . . . . ?
C8 C7 C12 O1 -179.7(2) . . . . ?
C8 C7 C12 C11 0.5(4) . . . . ?
C8 C7 C41 C6 -179.9(2) . . . . ?
C8 C7 C41 C42 -59.4(3) . . . . ?
C8 C7 C41 C43 60.4(3) . . . . ?
C8 C9 C10 C11 0.0(4) . . . . ?
C8 C9 C48 C49 48.7(4) . . . . ?
C8 C9 C48 C50 -71.2(4) . . . . ?
C8 C9 C48 C51 168.3(3) . . . . ?
C9 C10 C11 C12 -0.2(4) . . . . ?
C9 C10 C11 C27 179.9(2) . . . . ?
C10 C9 C48 C49 -132.8(3) . . . . ?
C10 C9 C48 C50 107.2(4) . . . . ?
C10 C9 C48 C51 -13.3(4) . . . . ?
C10 C11 C12 O1 -179.9(2) . . . . ?
C10 C11 C12 C7 -0.1(4) . . . . ?
C10 C11 C27 C28 -109.3(3) . . . . ?
C10 C11 C27 C40 68.4(3) . . . . ?
C11 C27 C28 C29 -2.8(4) . . . . ?
C11 C27 C28 C33 176.0(2) . . . . ?
C11 C27 C40 C35 -176.8(2) . . . . ?
C11 C27 C40 C39 3.3(3) . . . . ?
C12 O1 C1 C2 179.0(2) . . . . ?
C12 O1 C1 C6 -1.3(3) . . . . ?
C12 C7 C8 C9 -0.7(4) . . . . ?
C12 C7 C41 C6 1.0(3) . . . . ?
C12 C7 C41 C42 121.5(3) . . . . ?
C12 C7 C41 C43 -118.7(3) . . . . ?
C12 C11 C27 C28 70.8(3) . . . . ?
C12 C11 C27 C40 -111.5(3) . . . . ?
C13 C2 C3 C4 -178.4(2) . . . . ?
C13 C14 C15 C16 -179.3(3) . . . . ?
C13 C14 C19 C18 178.9(2) . . . . ?
C13 C14 C19 C20 0.3(4) . . . . ?
C14 C13 C26 C21 -3.1(3) . . . . ?
C14 C13 C26 C25 177.7(2) . . . . ?
C14 C15 C16 C17 0.4(5) . . . . ?
C14 C19 C20 C21 -2.6(4) . . . . ?
C15 C14 C19 C18 -0.9(4) . . . . ?
C15 C14 C19 C20 -179.5(2) . . . . ?
C15 C16 C17 C18 -0.9(5) . . . . ?
C16 C17 C18 C19 0.4(5) . . . . ?
C17 C18 C19 C14 0.5(4) . . . . ?
C17 C18 C19 C20 179.1(3) . . . . ?
C18 C19 C20 C21 178.9(3) . . . . ?
C19 C14 C15 C16 0.5(4) . . . . ?
C19 C20 C21 C22 179.9(3) . . . . ?
C19 C20 C21 C26 2.0(4) . . . . ?
C20 C21 C22 C23 -179.9(3) . . . . ?
C20 C21 C26 C13 0.9(4) . . . . ?
C20 C21 C26 C25 -179.9(3) . . . . ?
C21 C22 C23 C24 0.8(6) . . . . ?
C22 C21 C26 C13 -177.1(2) . . . . ?
C22 C21 C26 C25 2.2(4) . . . . ?
C22 C23 C24 C25 0.1(7) . . . . ?
C23 C24 C25 C26 0.2(6) . . . . ?
C24 C25 C26 C13 177.9(3) . . . . ?
C24 C25 C26 C21 -1.3(5) . . . . ?
C26 C13 C14 C15 -177.7(2) . . . . ?
C26 C13 C14 C19 2.5(3) . . . . ?
C26 C21 C22 C23 -1.9(5) . . . . ?
C27 C11 C12 O1 0.0(4) . . . . ?
C27 C11 C12 C7 179.8(2) . . . . ?
C27 C28 C29 C30 177.8(3) . . . . ?
C27 C28 C33 C32 -177.6(3) . . . . ?
C27 C28 C33 C34 1.6(4) . . . . ?
C28 C27 C40 C35 0.9(3) . . . . ?
C28 C27 C40 C39 -179.0(2) . . . . ?
C28 C29 C30 C31 -1.0(7) . . . . ?
C28 C33 C34 C35 -0.8(4) . . . . ?
C29 C28 C33 C32 1.3(4) . . . . ?
C29 C28 C33 C34 -179.6(3) . . . . ?
C29 C30 C31 C32 2.7(8) . . . . ?
C30 C31 C32 C33 -2.4(7) . . . . ?
C31 C32 C33 C28 0.4(5) . . . . ?
C31 C32 C33 C34 -178.7(4) . . . . ?
C32 C33 C34 C35 178.4(3) . . . . ?
C33 C28 C29 C30 -1.0(5) . . . . ?
C33 C34 C35 C36 -179.0(3) . . . . ?
C33 C34 C35 C40 0.0(4) . . . . ?
C34 C35 C36 C37 179.3(3) . . . . ?
C34 C35 C40 C27 -0.1(4) . . . . ?
C34 C35 C40 C39 179.9(2) . . . . ?
C35 C36 C37 C38 0.4(5) . . . . ?
C36 C35 C40 C27 179.0(2) . . . . ?
C36 C35 C40 C39 -1.0(4) . . . . ?
C36 C37 C38 C39 -0.2(5) . . . . ?
C37 C38 C39 C40 -0.7(5) . . . . ?
C38 C39 C40 C27 -178.8(2) . . . . ?
C38 C39 C40 C35 1.3(4) . . . . ?
C40 C27 C28 C29 179.6(2) . . . . ?
C40 C27 C28 C33 -1.7(4) . . . . ?
C40 C35 C36 C37 0.2(4) . . . . ?
C41 C7 C8 C9 -179.8(2) . . . . ?
C41 C7 C12 O1 -0.7(4) . . . . ?
C41 C7 C12 C11 179.6(2) . . . . ?
C44 C4 C5 C6 -179.4(2) . . . . ?
C48 C9 C10 C11 -178.5(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.606
_oxdiff_exptl_absorpt_empirical_full_min 0.336
####################################################################### 
# 
# 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_20221124-meoh_auto
_database_code_depnum_ccdc_archive 'CCDC 2308129'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2023-11-15 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2023-11-15
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C51 H46 O'
_chemical_formula_sum            'C51 H46 O'
_chemical_formula_weight         674.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHO
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3897(3)
_cell_length_b                   18.1370(4)
_cell_length_c                   19.2706(5)
_cell_angle_alpha                83.875(2)
_cell_angle_beta                 81.204(2)
_cell_angle_gamma                81.729(2)
_cell_volume                     3878.46(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21104
_cell_measurement_temperature    292.5(9)
_cell_measurement_theta_max      75.5350
_cell_measurement_theta_min      2.3510
_shelx_estimated_absorpt_T_max   0.970
_shelx_estimated_absorpt_T_min   0.928
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            48581
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         2.329
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.5(9)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     60.00 100.00   0.50    0.50    --   62.89  15.00   0.00   80
  2  ω     67.00 121.00   0.50    0.50    --   76.75  15.00  30.00  108
  3  ω     62.00 117.00   0.50    0.50    --   72.93  15.00  90.00  110
  4  ω     58.00  98.00   0.50    0.50    --   62.89  15.00 150.00   80
  5  ω     48.00  98.00   0.50    0.50    --   76.75-125.00  30.00  100
  6  ω     24.00  62.00   0.50    0.50    --   62.89-125.00-120.00   76
  7  ω     36.00  96.00   0.50    0.50    --   76.75-125.00-150.00  120
  8  ω     39.00  98.00   0.50    0.50    --   76.75-125.00 -90.00  118
  9  ω     39.00  98.00   0.50    0.50    --   76.75-125.00 120.00  118
 10  ω     50.00  98.00   0.50    0.50    --   76.75-125.00 150.00   96
 11  ω    -99.00 -54.00   0.50    0.50    --  -63.72 -15.00 -30.00   90
 12  ω   -100.00 -61.00   0.50    0.50    --  -63.72 -15.00 -60.00   78
 13  ω   -107.00 -64.00   0.50    0.50    --  -63.72 -15.00  30.00   86
 14  ω   -117.00 -78.00   0.50    0.50    --  -76.43 -15.00  60.00   78
 15  ω    -82.00 -54.00   0.50    0.50    --  -63.72 -15.00  90.00   56
 16  ω   -108.00 -62.00   0.50    0.50    --  -71.74 -15.00  90.00   92
 17  ω   -121.00 -86.00   0.50    0.50    --  -81.49 -15.00 150.00   70
 18  ω   -117.00 -86.00   0.50    0.50    --  -76.43 -15.00-180.00   62
 19  ω   -123.00 -78.00   0.50    0.50    --  -81.49 -15.00-150.00   90
 20  ω   -124.00 -72.00   0.50    0.50    --  -81.49 -15.00 -90.00  104
 21  ω   -102.00 -42.00   0.50    0.50    --  -81.49 125.00 -90.00  120
 22  ω    -96.00 -34.00   0.50    0.50    --  -76.43 125.00-120.00  124
 23  ω    -60.00 -24.00   0.50    0.50    --  -63.72 125.00-150.00   72
 24  ω   -101.00 -58.00   0.50    0.50    --  -81.49 125.00-150.00   86
 25  ω   -102.00 -77.00   0.50    0.50    --  -81.49 125.00-120.00   50
 26  ω   -102.00 -76.00   0.50    0.50    --  -81.49 125.00 -60.00   52
 27  ω    -76.00 -50.00   0.50    0.50    --  -76.43 125.00 -30.00   52
 28  ω   -102.00 -43.00   0.50    0.50    --  -81.49 125.00   0.00  118
 29  ω    -53.00 -28.00   0.50    0.50    --  -63.72 125.00  90.00   50
 30  ω   -102.00 -57.00   0.50    0.50    --  -81.49 125.00 150.00   90
 31  ω   -102.00 -44.00   0.50    0.50    --  -81.49 125.00  90.00  116
 32  ω   -102.00 -50.00   0.50    0.50    --  -81.49 125.00  60.00  104
 33  ω   -102.00 -74.00   0.50    0.50    --  -81.49 125.00 -30.00   56
 34  ω   -100.00 -74.00   0.50    0.50    --  -81.49 125.00  30.00   52
 35  ω    -67.00 -40.00   0.50    0.50    --  -81.49 125.00 -30.00   54
 36  ω    -74.00 -49.00   0.50    0.50    --  -81.49 125.00-120.00   50
 37  ω    -65.00 -40.00   0.50    0.50    --  -81.49 125.00-180.00   50
 38  ω   -102.00 -77.00   0.50    0.50    --  -81.49 125.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0781793000
_diffrn_orient_matrix_UB_12      -0.0155235000
_diffrn_orient_matrix_UB_13      -0.0540060000
_diffrn_orient_matrix_UB_21      -0.1094137000
_diffrn_orient_matrix_UB_22      0.0455508000
_diffrn_orient_matrix_UB_23      0.0399123000
_diffrn_orient_matrix_UB_31      0.0311561000
_diffrn_orient_matrix_UB_32      0.0714645000
_diffrn_orient_matrix_UB_33      -0.0456487000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9986
_reflns_number_total             13560
_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       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1034
_refine_ls_number_reflns         13560
_refine_ls_number_restraints     117
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0563
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0918P)²+0.3757P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.1670
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C47-C48 \\sim C47-C48A
 with sigma of 0.02
 C47-C49 \\sim C47-C49A
 with sigma of 0.02
 C47-C50 \\sim C47-C50A
 with sigma of 0.02
 C99-C55 \\sim C99-C55A
 with sigma of 0.02
 C43-C45 \\sim C43-C45A
 with sigma of 0.02
 C43-C44 \\sim C43-C44A
 with sigma of 0.02
 C99-C102 \\sim C99-C103
 with sigma of 0.02
 C43-C46 \\sim C43-C46A
 with sigma of 0.02
 C99-C1 \\sim C99-C1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C49A) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C50A) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C48A) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C44) \\sim Ueq,
Uanis(C45A) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46A) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C44A) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C102) \\sim Ueq,
Uanis(C103) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C55A) \\sim Ueq, Uanis(C1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C50A)=Sof(H50D)=Sof(H50E)=Sof(H50F)=Sof(C49A)=Sof(H49D)=Sof(H49E)=
 Sof(H49F)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(1)
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(1)
 Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C44A)=Sof(H44D)=Sof(H44E)=
 Sof(H44F)=Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(2)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(2)
 Sof(C103)=Sof(H10J)=Sof(H10K)=Sof(H10L)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=
 Sof(H1AC)=Sof(C55A)=Sof(H55D)=Sof(H55E)=Sof(H55F)=1-FVAR(3)
 Sof(C102)=Sof(H10G)=Sof(H10H)=Sof(H10I)=Sof(C55)=Sof(H55A)=Sof(H55B)=
 Sof(H55C)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C66(H66), C64(H64), C4(H4), C6(H6), C58(H58), C77(H77), C74(H74), C12(H12),
 C39(H39), C22(H22), C10(H10), C60(H60), C42(H42), C69(H69), C30(H30), C35(H35),
  C25(H25), C80(H80), C78(H78), C40(H40), C94(H94), C72(H72), C17(H17),
 C20(H20), C70(H70), C71(H71), C79(H79), C41(H41), C34(H34), C32(H32), C88(H88),
  C19(H19), C33(H33), C18(H18), C28(H28), C26(H26), C93(H93), C91(H91),
 C27(H27), C92(H92), C84(H84), C83(H83), C86(H86), C85(H85)
5.b Fitted hexagon refined as free rotating group:
 C88(C87,C82,C81,C90,C89)
5.c Idealised Me refined as rotating group:
 C101(H10A,H10B,H10C), C100(H10D,H10E,H10F), C51(H51A,H51B,H51C), C52(H52A,
 H52B,H52C), C45(H45A,H45B,H45C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C44(H44A,H44B,H44C), C50(H50A,H50B,H50C), C46(H46A,H46B,H46C), C102(H10G,H10H,
 H10I), C55(H55A,H55B,H55C), C1(H1A,H1B,H1C), C50A(H50D,H50E,H50F), C49A(H49D,
 H49E,H49F), C48A(H48D,H48E,H48F), C45A(H45D,H45E,H45F), C44A(H44D,H44E,H44F),
 C46A(H46D,H46E,H46F), C103(H10J,H10K,H10L), C1A(H1AA,H1AB,H1AC), C55A(H55D,
 H55E,H55F), C97(H97A,H97B,H97C), C98(H98A,H98B,H98C), C96(H96A,H96B,H96C)
;
_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 0.86039(11) 0.16339(6) 0.87679(6) 0.0456(3) Uani 1 1 d . . . . .
O55 O 0.58259(12) 0.67864(6) 0.58080(6) 0.0484(3) Uani 1 1 d . . . . .
C67 C 0.64487(15) 0.58660(9) 0.69358(8) 0.0382(4) Uani 1 1 d . . . . .
C54 C 0.64453(15) 0.61122(9) 0.56281(8) 0.0380(4) Uani 1 1 d . . . . .
C53 C 0.67803(14) 0.56343(9) 0.62038(8) 0.0379(4) Uani 1 1 d . . . . .
C2 C 0.80977(15) 0.11608(9) 0.92958(9) 0.0392(4) Uani 1 1 d . . . . .
C56 C 0.53849(15) 0.72816(9) 0.52904(9) 0.0412(4) Uani 1 1 d . . . . .
C14 C 0.92435(15) 0.13394(9) 0.81722(9) 0.0405(4) Uani 1 1 d . . . . .
C3 C 0.74290(15) 0.15200(9) 0.98655(9) 0.0408(4) Uani 1 1 d . . . . .
C63 C 0.67243(15) 0.59191(9) 0.49442(8) 0.0390(4) Uani 1 1 d . . . . .
C15 C 0.72702(16) 0.23560(9) 0.98511(8) 0.0405(4) Uani 1 1 d . . . . .
C37 C 0.94033(15) 0.26818(9) 0.77806(8) 0.0411(4) Uani 1 1 d . . . . .
C7 C 0.82358(15) 0.03930(9) 0.92726(9) 0.0416(4) Uani 1 1 d . . . . .
C38 C 0.82194(15) 0.30453(10) 0.77878(8) 0.0414(4) Uani 1 1 d . . . . .
C65 C 0.77122(15) 0.47104(9) 0.53908(9) 0.0415(4) Uani 1 1 d . . . . .
C29 C 0.79634(16) 0.38193(10) 0.79131(9) 0.0448(4) Uani 1 1 d . . . . .
C66 C 0.74117(15) 0.49392(9) 0.60688(8) 0.0418(4) Uani 1 1 d . . . . .
H66 H 0.764226 0.461450 0.644533 0.050 Uiso 1 1 calc R U . . .
C64 C 0.73560(16) 0.52136(9) 0.48411(9) 0.0430(4) Uani 1 1 d . . . . .
H64 H 0.754900 0.507196 0.438347 0.052 Uiso 1 1 calc R U . . .
C76 C 0.52573(15) 0.58801(9) 0.72692(9) 0.0408(4) Uani 1 1 d . . . . .
C68 C 0.73376(15) 0.60440(9) 0.73044(9) 0.0417(4) Uani 1 1 d . . . . .
C36 C 1.03189(16) 0.30755(10) 0.79024(9) 0.0452(4) Uani 1 1 d . . . . .
C9 C 0.94491(15) 0.05841(10) 0.80851(9) 0.0437(4) Uani 1 1 d . . . . .
C13 C 0.96707(15) 0.18764(10) 0.76570(9) 0.0438(4) Uani 1 1 d . . . . .
C24 C 0.82496(16) 0.27311(10) 0.99035(8) 0.0430(4) Uani 1 1 d . . . . .
C57 C 0.47137(16) 0.79297(10) 0.55445(9) 0.0448(4) Uani 1 1 d . . . . .
C61 C 0.55986(16) 0.71614(10) 0.45866(9) 0.0430(4) Uani 1 1 d . . . . .
C73 C 0.70250(17) 0.62072(10) 0.80278(9) 0.0483(4) Uani 1 1 d . . . . .
C5 C 0.70224(16) 0.02934(10) 1.04312(10) 0.0470(4) Uani 1 1 d . . . . .
C4 C 0.69051(17) 0.10691(10) 1.04234(9) 0.0475(4) Uani 1 1 d . . . . .
H4 H 0.645775 0.129550 1.080738 0.057 Uiso 1 1 calc R U . . .
C21 C 0.60204(18) 0.35740(10) 0.97138(9) 0.0497(5) Uani 1 1 d . . . . .
C75 C 0.49559(17) 0.60525(10) 0.79898(9) 0.0470(4) Uani 1 1 d . . . . .
C23 C 0.81074(19) 0.35342(10) 0.98575(9) 0.0499(5) Uani 1 1 d . . . . .
C16 C 0.61489(16) 0.27691(10) 0.97650(9) 0.0446(4) Uani 1 1 d . . . . .
C6 C 0.76864(16) -0.00229(10) 0.98493(10) 0.0473(4) Uani 1 1 d . . . . .
H6 H 0.777055 -0.053987 0.984266 0.057 Uiso 1 1 calc R U . . .
C8 C 0.89645(17) 0.00086(9) 0.86513(10) 0.0488(4) Uani 1 1 d . . . . .
C62 C 0.63960(17) 0.64670(10) 0.43195(8) 0.0475(4) Uani 1 1 d . . . . .
C58 C 0.42326(17) 0.84629(10) 0.50565(10) 0.0511(5) Uani 1 1 d . . . . .
H58 H 0.377702 0.889581 0.521533 0.061 Uiso 1 1 calc R U . . .
C77 C 0.43169(17) 0.57191(10) 0.69234(10) 0.0494(4) Uani 1 1 d . . . . .
H77 H 0.448754 0.560397 0.645676 0.059 Uiso 1 1 calc R U . . .
C59 C 0.44085(17) 0.83717(10) 0.43388(10) 0.0492(4) Uani 1 1 d . . . . .
C99 C 0.84067(17) 0.39382(10) 0.52521(10) 0.0499(5) Uani 1 1 d D . . . .
C74 C 0.58538(18) 0.62022(11) 0.83484(9) 0.0540(5) Uani 1 1 d . . . . .
H74 H 0.566052 0.630195 0.881864 0.065 Uiso 1 1 calc R U . . .
C12 C 1.03245(17) 0.16274(11) 0.70381(10) 0.0524(5) Uani 1 1 d . . . . .
H12 H 1.061104 0.197818 0.668916 0.063 Uiso 1 1 calc R U . . .
C39 C 0.67533(18) 0.41710(11) 0.79326(10) 0.0535(5) Uani 1 1 d . . . . .
H39 H 0.657252 0.467208 0.801981 0.064 Uiso 1 1 calc R U . . .
C22 C 0.6998(2) 0.39280(11) 0.97530(10) 0.0554(5) Uani 1 1 d . . . . .
H22 H 0.691366 0.444786 0.970806 0.066 Uiso 1 1 calc R U . . .
C10 C 1.01168(17) 0.03717(11) 0.74526(10) 0.0534(5) Uani 1 1 d . . . . .
H10 H 1.026832 -0.013498 0.738427 0.064 Uiso 1 1 calc R U . . .
C60 C 0.50902(17) 0.77207(10) 0.41228(9) 0.0492(4) Uani 1 1 d . . . . .
H60 H 0.521747 0.765095 0.364461 0.059 Uiso 1 1 calc R U . . .
C42 C 0.72521(17) 0.26738(11) 0.76841(10) 0.0536(5) Uani 1 1 d . . . . .
H42 H 0.739815 0.217057 0.760184 0.064 Uiso 1 1 calc R U . . .
C31 C 1.00548(18) 0.38608(10) 0.80016(10) 0.0507(5) Uani 1 1 d . . . . .
C69 C 0.85469(17) 0.60757(11) 0.69887(10) 0.0511(5) Uani 1 1 d . . . . .
H69 H 0.876544 0.598616 0.651711 0.061 Uiso 1 1 calc R U . . .
C30 C 0.88838(18) 0.42047(11) 0.80050(10) 0.0519(5) Uani 1 1 d . . . . .
H30 H 0.871229 0.471143 0.807129 0.062 Uiso 1 1 calc R U . . .
C35 C 1.15120(17) 0.27273(12) 0.79584(10) 0.0554(5) Uani 1 1 d . . . . .
H35 H 1.170232 0.221638 0.791660 0.066 Uiso 1 1 calc R U . . .
C11 C 1.05676(18) 0.08754(12) 0.69195(10) 0.0561(5) Uani 1 1 d . . . . .
C25 C 0.94038(18) 0.23486(12) 1.00027(11) 0.0601(5) Uani 1 1 d . . . . .
H25 H 0.952738 0.182890 1.002754 0.072 Uiso 1 1 calc R U . . .
C80 C 0.37493(19) 0.60537(12) 0.83163(11) 0.0610(5) Uani 1 1 d . . . . .
H80 H 0.354753 0.616161 0.878406 0.073 Uiso 1 1 calc R U . . .
C78 C 0.31796(18) 0.57298(12) 0.72580(12) 0.0620(5) Uani 1 1 d . . . . .
H78 H 0.258406 0.562205 0.701822 0.074 Uiso 1 1 calc R U . . .
C47 C 0.64216(19) -0.01826(11) 1.10568(10) 0.0571(5) Uani 1 1 d D . . . .
C40 C 0.58689(18) 0.37936(12) 0.78277(11) 0.0597(5) Uani 1 1 d . . . . .
H40 H 0.508994 0.403596 0.783836 0.072 Uiso 1 1 calc R U . . .
C94 C 0.24000(19) 0.78598(11) 0.64547(13) 0.0638(6) Uani 1 1 d . . . . .
H94 H 0.243969 0.783416 0.597206 0.077 Uiso 1 1 calc R U . . .
C72 C 0.7949(2) 0.63621(12) 0.83970(11) 0.0617(5) Uani 1 1 d . . . . .
H72 H 0.776086 0.645837 0.886835 0.074 Uiso 1 1 calc R U . . .
C17 C 0.51225(18) 0.24328(13) 0.97103(11) 0.0620(5) Uani 1 1 d . . . . .
H17 H 0.518042 0.191420 0.973434 0.074 Uiso 1 1 calc R U . . .
C20 C 0.4880(2) 0.39819(13) 0.96158(11) 0.0650(6) Uani 1 1 d . . . . .
H20 H 0.479343 0.450187 0.957511 0.078 Uiso 1 1 calc R U . . .
C70 C 0.93881(19) 0.62336(12) 0.73600(12) 0.0617(5) Uani 1 1 d . . . . .
H70 H 1.017082 0.625111 0.714021 0.074 Uiso 1 1 calc R U . . .
C71 C 0.9084(2) 0.63713(13) 0.80765(12) 0.0663(6) Uani 1 1 d . . . . .
H71 H 0.967060 0.646886 0.832855 0.080 Uiso 1 1 calc R U . . .
C79 C 0.28881(19) 0.59012(13) 0.79619(12) 0.0673(6) Uani 1 1 d . . . . .
H79 H 0.210257 0.591003 0.818459 0.081 Uiso 1 1 calc R U . . .
C41 C 0.61215(18) 0.30346(13) 0.77022(11) 0.0610(5) Uani 1 1 d . . . . .
H41 H 0.550670 0.277699 0.763080 0.073 Uiso 1 1 calc R U . . .
C34 C 1.23708(19) 0.31272(15) 0.80712(12) 0.0693(6) Uani 1 1 d . . . . .
H34 H 1.313868 0.288568 0.810965 0.083 Uiso 1 1 calc R U . . .
C43 C 1.1316(2) 0.06074(15) 0.62395(12) 0.0770(7) Uani 1 1 d D . . . .
C32 C 1.1001(2) 0.42531(13) 0.81006(12) 0.0680(6) Uani 1 1 d . . . . .
H32 H 1.084163 0.476464 0.814531 0.082 Uiso 1 1 calc R U . . .
C88 C 0.43860(15) 0.80127(8) 0.77765(5) 0.0787(7) Uani 1 1 d G . . . .
H88 H 0.432876 0.800990 0.826339 0.094 Uiso 1 1 calc R U . . .
C87 C 0.54771(12) 0.80797(8) 0.73552(7) 0.0675(6) Uani 1 1 d G . . . .
C82 C 0.55626(9) 0.80840(7) 0.66276(7) 0.0550(5) Uani 1 1 d G . . . .
C81 C 0.45570(11) 0.80212(7) 0.63212(5) 0.0469(4) Uani 1 1 d G . . . .
C90 C 0.34659(9) 0.79543(7) 0.67424(6) 0.0516(5) Uani 1 1 d G . . . .
C89 C 0.33804(11) 0.79500(8) 0.74701(6) 0.0654(6) Uani 1 1 d G . . . .
C19 C 0.3934(2) 0.36343(15) 0.95811(12) 0.0753(7) Uani 1 1 d . . . . .
H19 H 0.319573 0.391232 0.952878 0.090 Uiso 1 1 calc R U . . .
C101 C 0.7565(2) 0.67177(13) 0.39069(12) 0.0787(8) Uani 1 1 d . . . . .
H10A H 0.806785 0.629287 0.371914 0.118 Uiso 1 1 calc R U . . .
H10B H 0.797757 0.693376 0.421749 0.118 Uiso 1 1 calc R U . . .
H10C H 0.737662 0.708222 0.352755 0.118 Uiso 1 1 calc R U . . .
C33 C 1.2119(2) 0.39064(15) 0.81316(13) 0.0733(7) Uani 1 1 d . . . . .
H33 H 1.272453 0.417735 0.819236 0.088 Uiso 1 1 calc R U . . .
C18 C 0.4056(2) 0.28490(16) 0.96238(13) 0.0754(7) Uani 1 1 d . . . . .
H18 H 0.339689 0.261127 0.959231 0.091 Uiso 1 1 calc R U . . .
C100 C 0.5758(3) 0.60840(13) 0.38422(12) 0.0818(8) Uani 1 1 d . . . . .
H10D H 0.548419 0.644309 0.347931 0.123 Uiso 1 1 calc R U . . .
H10E H 0.508496 0.587915 0.411697 0.123 Uiso 1 1 calc R U . . .
H10F H 0.630433 0.568940 0.363107 0.123 Uiso 1 1 calc R U . . .
C28 C 0.9113(2) 0.38953(14) 0.99155(12) 0.0732(7) Uani 1 1 d . . . . .
H28 H 0.902958 0.441494 0.988464 0.088 Uiso 1 1 calc R U . . .
C26 C 1.0325(2) 0.27239(16) 1.00615(14) 0.0794(7) Uani 1 1 d . . . . .
H26 H 1.106357 0.245819 1.013474 0.095 Uiso 1 1 calc R U . . .
C93 C 0.1342(2) 0.78082(14) 0.68806(16) 0.0814(7) Uani 1 1 d . . . . .
H93 H 0.066373 0.775281 0.668667 0.098 Uiso 1 1 calc R U . . .
C51 C 1.0014(2) -0.05185(14) 0.89129(14) 0.0910(9) Uani 1 1 d . . . . .
H51A H 0.971078 -0.091495 0.922955 0.136 Uiso 1 1 calc R U . . .
H51B H 1.046305 -0.024462 0.915483 0.136 Uiso 1 1 calc R U . . .
H51C H 1.052452 -0.072625 0.851826 0.136 Uiso 1 1 calc R U . . .
C91 C 0.2237(3) 0.79044(14) 0.79023(14) 0.0871(8) Uani 1 1 d . . . . .
H91 H 0.217380 0.792123 0.838742 0.104 Uiso 1 1 calc R U . . .
C27 C 1.0179(3) 0.35056(16) 1.00135(14) 0.0841(8) Uani 1 1 d . . . . .
H27 H 1.082185 0.375628 1.004957 0.101 Uiso 1 1 calc R U . . .
C92 C 0.1266(3) 0.78382(14) 0.76129(17) 0.0917(9) Uani 1 1 d . . . . .
H92 H 0.053449 0.781167 0.789825 0.110 Uiso 1 1 calc R U . . .
C84 C 0.7688(2) 0.82126(14) 0.65218(18) 0.0875(8) Uani 1 1 d . . . . .
H84 H 0.841762 0.826267 0.624081 0.105 Uiso 1 1 calc R U . . .
C83 C 0.6707(2) 0.81741(12) 0.62170(14) 0.0665(6) Uani 1 1 d . . . . .
H83 H 0.677404 0.820689 0.572791 0.080 Uiso 1 1 calc R U . . .
C86 C 0.6558(3) 0.81206(15) 0.76656(16) 0.0915(9) Uani 1 1 d . . . . .
H86 H 0.651769 0.810700 0.815237 0.110 Uiso 1 1 calc R U . . .
C85 C 0.7617(3) 0.81781(16) 0.7250(2) 0.0996(10) Uani 1 1 d . . . . .
H85 H 0.830139 0.819452 0.745292 0.120 Uiso 1 1 calc R U . . .
C52 C 0.8163(3) -0.04306(16) 0.83230(15) 0.0949(9) Uani 1 1 d . . . . .
H52A H 0.862133 -0.066594 0.792680 0.142 Uiso 1 1 calc R U . . .
H52B H 0.750271 -0.009451 0.816962 0.142 Uiso 1 1 calc R U . . .
H52C H 0.786287 -0.080577 0.866769 0.142 Uiso 1 1 calc R U . . .
C45 C 1.2416(6) 0.0026(5) 0.6475(4) 0.094(2) Uani 0.506(9) 1 d D U P A 1
H45A H 1.211405 -0.039552 0.675317 0.141 Uiso 0.506(9) 1 calc R U P A 1
H45B H 1.286119 0.026683 0.674927 0.141 Uiso 0.506(9) 1 calc R U P A 1
H45C H 1.293103 -0.014116 0.606393 0.141 Uiso 0.506(9) 1 calc R U P A 1
C48 C 0.6911(5) -0.0069(3) 1.1716(2) 0.096(2) Uani 0.672(7) 1 d D U P B 1
H48A H 0.676513 0.045214 1.179664 0.143 Uiso 0.672(7) 1 calc R U P B 1
H48B H 0.775784 -0.023101 1.166104 0.143 Uiso 0.672(7) 1 calc R U P B 1
H48C H 0.652227 -0.035411 1.211081 0.143 Uiso 0.672(7) 1 calc R U P B 1
C49 C 0.5089(4) 0.0075(4) 1.1143(3) 0.103(2) Uani 0.672(7) 1 d D U P B 1
H49A H 0.468996 -0.024001 1.150843 0.154 Uiso 0.672(7) 1 calc R U P B 1
H49B H 0.479148 0.004752 1.070766 0.154 Uiso 0.672(7) 1 calc R U P B 1
H49C H 0.494047 0.058256 1.126674 0.154 Uiso 0.672(7) 1 calc R U P B 1
C44 C 1.0613(8) 0.0065(7) 0.5952(5) 0.131(5) Uani 0.506(9) 1 d D U P A 1
H44A H 1.110921 -0.017214 0.556778 0.197 Uiso 0.506(9) 1 calc R U P A 1
H44B H 0.990685 0.033945 0.578838 0.197 Uiso 0.506(9) 1 calc R U P A 1
H44C H 1.038564 -0.030872 0.631981 0.197 Uiso 0.506(9) 1 calc R U P A 1
C50 C 0.6649(6) -0.1013(2) 1.0933(3) 0.112(3) Uani 0.672(7) 1 d D U P B 1
H50A H 0.749533 -0.117652 1.087434 0.167 Uiso 0.672(7) 1 calc R U P B 1
H50B H 0.633059 -0.108770 1.051602 0.167 Uiso 0.672(7) 1 calc R U P B 1
H50C H 0.626368 -0.129623 1.133053 0.167 Uiso 0.672(7) 1 calc R U P B 1
C46 C 1.1793(14) 0.1176(4) 0.5750(5) 0.176(7) Uani 0.506(9) 1 d D U P A 1
H46A H 1.206898 0.153102 0.600233 0.264 Uiso 0.506(9) 1 calc R U P A 1
H46B H 1.117907 0.142621 0.548603 0.264 Uiso 0.506(9) 1 calc R U P A 1
H46C H 1.244936 0.095262 0.543385 0.264 Uiso 0.506(9) 1 calc R U P A 1
C102 C 0.8695(6) 0.3464(3) 0.5916(2) 0.087(2) Uani 0.596(7) 1 d D U P C 1
H10G H 0.908937 0.298048 0.579554 0.131 Uiso 0.596(7) 1 calc R U P C 1
H10H H 0.796687 0.340657 0.622944 0.131 Uiso 0.596(7) 1 calc R U P C 1
H10I H 0.921224 0.370315 0.614395 0.131 Uiso 0.596(7) 1 calc R U P C 1
C55 C 0.9579(5) 0.4038(3) 0.4779(4) 0.100(3) Uani 0.596(7) 1 d D U P C 1
H55A H 1.007114 0.428155 0.502133 0.149 Uiso 0.596(7) 1 calc R U P C 1
H55B H 0.941597 0.433908 0.435518 0.149 Uiso 0.596(7) 1 calc R U P C 1
H55C H 0.999008 0.355800 0.466228 0.149 Uiso 0.596(7) 1 calc R U P C 1
C1 C 0.7652(5) 0.3505(3) 0.4888(4) 0.105(3) Uani 0.596(7) 1 d D U P C 1
H1A H 0.809811 0.303082 0.477902 0.157 Uiso 0.596(7) 1 calc R U P C 1
H1B H 0.745904 0.378692 0.446020 0.157 Uiso 0.596(7) 1 calc R U P C 1
H1C H 0.692644 0.342568 0.519534 0.157 Uiso 0.596(7) 1 calc R U P C 1
C50A C 0.7361(8) -0.0779(7) 1.1347(6) 0.109(5) Uani 0.328(7) 1 d D U P B 2
H50D H 0.784783 -0.054839 1.160290 0.164 Uiso 0.328(7) 1 calc R U P B 2
H50E H 0.785752 -0.101633 1.096298 0.164 Uiso 0.328(7) 1 calc R U P B 2
H50F H 0.696537 -0.114682 1.165573 0.164 Uiso 0.328(7) 1 calc R U P B 2
C49A C 0.5457(10) -0.0562(7) 1.0824(5) 0.100(4) Uani 0.328(7) 1 d D U P B 2
H49D H 0.516116 -0.090792 1.119994 0.149 Uiso 0.328(7) 1 calc R U P B 2
H49E H 0.579045 -0.082630 1.041823 0.149 Uiso 0.328(7) 1 calc R U P B 2
H49F H 0.481068 -0.019112 1.070622 0.149 Uiso 0.328(7) 1 calc R U P B 2
C48A C 0.5851(14) 0.0266(5) 1.1681(5) 0.110(5) Uani 0.328(7) 1 d D U P B 2
H48D H 0.551257 -0.006466 1.205755 0.165 Uiso 0.328(7) 1 calc R U P B 2
H48E H 0.523220 0.064135 1.153601 0.165 Uiso 0.328(7) 1 calc R U P B 2
H48F H 0.645202 0.050058 1.184135 0.165 Uiso 0.328(7) 1 calc R U P B 2
C45A C 1.1121(13) -0.0127(6) 0.6055(6) 0.161(6) Uani 0.494(9) 1 d D U P A 2
H45D H 1.153333 -0.021198 0.559181 0.241 Uiso 0.494(9) 1 calc R U P A 2
H45E H 1.027900 -0.013866 0.606301 0.241 Uiso 0.494(9) 1 calc R U P A 2
H45F H 1.142316 -0.051033 0.639004 0.241 Uiso 0.494(9) 1 calc R U P A 2
C44A C 1.0866(7) 0.1147(5) 0.5595(3) 0.102(3) Uani 0.494(9) 1 d D U P A 2
H44D H 1.100094 0.164937 0.564071 0.153 Uiso 0.494(9) 1 calc R U P A 2
H44E H 1.002629 0.113355 0.559790 0.153 Uiso 0.494(9) 1 calc R U P A 2
H44F H 1.130188 0.098338 0.515989 0.153 Uiso 0.494(9) 1 calc R U P A 2
C46A C 1.2579(5) 0.0735(9) 0.6223(5) 0.150(5) Uani 0.494(9) 1 d D U P A 2
H46D H 1.286279 0.051338 0.665132 0.225 Uiso 0.494(9) 1 calc R U P A 2
H46E H 1.262576 0.126225 0.617719 0.225 Uiso 0.494(9) 1 calc R U P A 2
H46F H 1.306548 0.051053 0.582839 0.225 Uiso 0.494(9) 1 calc R U P A 2
C103 C 0.9524(8) 0.3842(5) 0.5613(6) 0.117(4) Uani 0.404(7) 1 d D U P C 2
H10J H 0.930062 0.394049 0.609873 0.176 Uiso 0.404(7) 1 calc R U P C 2
H10K H 1.005698 0.418531 0.538301 0.176 Uiso 0.404(7) 1 calc R U P C 2
H10L H 0.991786 0.333892 0.558607 0.176 Uiso 0.404(7) 1 calc R U P C 2
C1A C 0.7632(8) 0.3344(3) 0.5580(6) 0.106(4) Uani 0.404(7) 1 d D U P C 2
H1AA H 0.803023 0.286015 0.546321 0.159 Uiso 0.404(7) 1 calc R U P C 2
H1AB H 0.687757 0.343665 0.540105 0.159 Uiso 0.404(7) 1 calc R U P C 2
H1AC H 0.749719 0.335757 0.608257 0.159 Uiso 0.404(7) 1 calc R U P C 2
C55A C 0.8762(10) 0.3830(4) 0.4480(4) 0.100(4) Uani 0.404(7) 1 d D U P C 2
H55D H 0.920825 0.422308 0.425854 0.150 Uiso 0.404(7) 1 calc R U P C 2
H55E H 0.805494 0.384308 0.426176 0.150 Uiso 0.404(7) 1 calc R U P C 2
H55F H 0.924797 0.335578 0.442814 0.150 Uiso 0.404(7) 1 calc R U P C 2
C95 C 0.38058(19) 0.89616(12) 0.38259(11) 0.0609(5) Uani 1 1 d . . . . .
C97 C 0.4358(3) 0.88779(15) 0.30672(13) 0.0928(9) Uani 1 1 d . . . . .
H97A H 0.520075 0.891256 0.301833 0.139 Uiso 1 1 calc R U . . .
H97B H 0.398322 0.926796 0.276581 0.139 Uiso 1 1 calc R U . . .
H97C H 0.424160 0.840023 0.293659 0.139 Uiso 1 1 calc R U . . .
C98 C 0.3921(4) 0.97411(14) 0.39868(19) 0.1357(15) Uani 1 1 d . . . . .
H98A H 0.343185 0.985000 0.442467 0.204 Uiso 1 1 calc R U . . .
H98B H 0.366258 1.009438 0.361552 0.204 Uiso 1 1 calc R U . . .
H98C H 0.474265 0.977549 0.402281 0.204 Uiso 1 1 calc R U . . .
C96 C 0.2502(2) 0.8848(2) 0.38900(19) 0.1373(16) Uani 1 1 d . . . . .
H96A H 0.244793 0.836344 0.374907 0.206 Uiso 1 1 calc R U . . .
H96B H 0.209674 0.922640 0.359139 0.206 Uiso 1 1 calc R U . . .
H96C H 0.213535 0.888186 0.437031 0.206 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 C2 1.3712(19) . ?
O1 C14 1.3773(19) . ?
O55 C54 1.3714(19) . ?
O55 C56 1.3734(19) . ?
C67 C53 1.492(2) . ?
C67 C76 1.408(2) . ?
C67 C68 1.413(2) . ?
C54 C53 1.399(2) . ?
C54 C63 1.378(2) . ?
C53 C66 1.388(2) . ?
C2 C3 1.401(2) . ?
C2 C7 1.383(2) . ?
C56 C57 1.398(2) . ?
C56 C61 1.376(2) . ?
C14 C9 1.380(2) . ?
C14 C13 1.398(2) . ?
C3 C15 1.499(2) . ?
C3 C4 1.392(2) . ?
C63 C64 1.393(2) . ?
C63 C62 1.534(2) . ?
C15 C24 1.409(2) . ?
C15 C16 1.408(2) . ?
C37 C38 1.412(2) . ?
C37 C36 1.406(3) . ?
C37 C13 1.486(2) . ?
C7 C6 1.393(2) . ?
C7 C8 1.522(2) . ?
C38 C29 1.431(2) . ?
C38 C42 1.420(3) . ?
C65 C66 1.391(2) . ?
C65 C64 1.392(2) . ?
C65 C99 1.535(2) . ?
C29 C39 1.430(3) . ?
C29 C30 1.383(3) . ?
C76 C75 1.435(2) . ?
C76 C77 1.423(3) . ?
C68 C73 1.436(2) . ?
C68 C69 1.425(2) . ?
C36 C31 1.440(3) . ?
C36 C35 1.428(3) . ?
C9 C8 1.524(2) . ?
C9 C10 1.395(2) . ?
C13 C12 1.388(2) . ?
C24 C23 1.437(2) . ?
C24 C25 1.425(3) . ?
C57 C58 1.390(2) . ?
C57 C81 1.504(2) . ?
C61 C62 1.530(2) . ?
C61 C60 1.400(2) . ?
C73 C74 1.383(3) . ?
C73 C72 1.431(3) . ?
C5 C4 1.393(2) . ?
C5 C6 1.383(3) . ?
C5 C47 1.537(2) . ?
C21 C16 1.440(3) . ?
C21 C22 1.379(3) . ?
C21 C20 1.427(3) . ?
C75 C74 1.390(3) . ?
C75 C80 1.421(3) . ?
C23 C22 1.390(3) . ?
C23 C28 1.422(3) . ?
C16 C17 1.417(3) . ?
C8 C51 1.533(3) . ?
C8 C52 1.537(3) . ?
C62 C101 1.544(3) . ?
C62 C100 1.531(3) . ?
C58 C59 1.391(3) . ?
C77 C78 1.354(3) . ?
C59 C60 1.383(3) . ?
C59 C95 1.537(3) . ?
C99 C102 1.516(4) . ?
C99 C55 1.519(4) . ?
C99 C1 1.532(5) . ?
C99 C103 1.521(7) . ?
C99 C1A 1.516(7) . ?
C99 C55A 1.507(7) . ?
C12 C11 1.388(3) . ?
C39 C40 1.347(3) . ?
C10 C11 1.388(3) . ?
C42 C41 1.355(3) . ?
C31 C30 1.388(3) . ?
C31 C32 1.420(3) . ?
C69 C70 1.358(3) . ?
C35 C34 1.354(3) . ?
C11 C43 1.535(3) . ?
C25 C26 1.355(3) . ?
C80 C79 1.352(3) . ?
C78 C79 1.403(3) . ?
C47 C48 1.508(4) . ?
C47 C49 1.511(5) . ?
C47 C50 1.529(5) . ?
C47 C50A 1.532(8) . ?
C47 C49A 1.522(8) . ?
C47 C48A 1.532(9) . ?
C40 C41 1.404(3) . ?
C94 C90 1.448(2) . ?
C94 C93 1.360(3) . ?
C72 C71 1.347(3) . ?
C17 C18 1.358(3) . ?
C20 C19 1.338(3) . ?
C70 C71 1.411(3) . ?
C34 C33 1.415(3) . ?
C43 C45 1.606(7) . ?
C43 C44 1.548(10) . ?
C43 C46 1.430(7) . ?
C43 C45A 1.470(10) . ?
C43 C44A 1.598(7) . ?
C43 C46A 1.484(8) . ?
C32 C33 1.344(3) . ?
C88 C87 1.3900 . ?
C88 C89 1.3900 . ?
C87 C82 1.3900 . ?
C87 C86 1.463(3) . ?
C82 C81 1.3900 . ?
C82 C83 1.439(2) . ?
C81 C90 1.3900 . ?
C90 C89 1.3900 . ?
C89 C91 1.443(3) . ?
C19 C18 1.406(4) . ?
C28 C27 1.344(4) . ?
C26 C27 1.398(4) . ?
C93 C92 1.407(4) . ?
C91 C92 1.337(4) . ?
C84 C83 1.353(3) . ?
C84 C85 1.388(4) . ?
C86 C85 1.352(4) . ?
C95 C97 1.515(3) . ?
C95 C98 1.507(3) . ?
C95 C96 1.513(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 O1 C14 118.93(13) . . ?
C54 O55 C56 118.94(13) . . ?
C76 C67 C53 119.95(15) . . ?
C76 C67 C68 119.93(15) . . ?
C68 C67 C53 120.07(15) . . ?
O55 C54 C53 113.86(14) . . ?
O55 C54 C63 123.53(14) . . ?
C63 C54 C53 122.61(15) . . ?
C54 C53 C67 120.65(14) . . ?
C66 C53 C67 121.69(14) . . ?
C66 C53 C54 117.65(14) . . ?
O1 C2 C3 114.33(14) . . ?
O1 C2 C7 123.10(15) . . ?
C7 C2 C3 122.57(15) . . ?
O55 C56 C57 113.59(15) . . ?
O55 C56 C61 123.47(15) . . ?
C61 C56 C57 122.93(15) . . ?
O1 C14 C9 123.57(15) . . ?
O1 C14 C13 113.90(15) . . ?
C9 C14 C13 122.53(16) . . ?
C2 C3 C15 120.33(14) . . ?
C4 C3 C2 117.12(16) . . ?
C4 C3 C15 122.53(15) . . ?
C54 C63 C64 117.17(15) . . ?
C54 C63 C62 121.56(15) . . ?
C64 C63 C62 121.23(14) . . ?
C24 C15 C3 120.11(15) . . ?
C16 C15 C3 119.98(16) . . ?
C16 C15 C24 119.88(16) . . ?
C38 C37 C13 119.53(16) . . ?
C36 C37 C38 120.26(16) . . ?
C36 C37 C13 120.20(15) . . ?
C2 C7 C6 117.17(16) . . ?
C2 C7 C8 122.13(15) . . ?
C6 C7 C8 120.69(15) . . ?
C37 C38 C29 119.36(16) . . ?
C37 C38 C42 122.88(17) . . ?
C42 C38 C29 117.75(16) . . ?
C66 C65 C64 117.06(15) . . ?
C66 C65 C99 121.65(15) . . ?
C64 C65 C99 121.29(15) . . ?
C39 C29 C38 118.33(17) . . ?
C30 C29 C38 119.56(17) . . ?
C30 C29 C39 122.11(18) . . ?
C53 C66 C65 122.40(15) . . ?
C65 C64 C63 123.10(15) . . ?
C67 C76 C75 119.89(16) . . ?
C67 C76 C77 122.69(16) . . ?
C77 C76 C75 117.42(16) . . ?
C67 C68 C73 119.50(16) . . ?
C67 C68 C69 122.85(16) . . ?
C69 C68 C73 117.65(17) . . ?
C37 C36 C31 119.63(16) . . ?
C37 C36 C35 123.02(18) . . ?
C35 C36 C31 117.31(18) . . ?
C14 C9 C8 121.65(15) . . ?
C14 C9 C10 116.85(16) . . ?
C10 C9 C8 121.50(16) . . ?
C14 C13 C37 119.79(15) . . ?
C12 C13 C14 117.68(17) . . ?
C12 C13 C37 122.53(16) . . ?
C15 C24 C23 119.96(17) . . ?
C15 C24 C25 122.89(17) . . ?
C25 C24 C23 117.16(17) . . ?
C56 C57 C81 119.14(14) . . ?
C58 C57 C56 117.51(16) . . ?
C58 C57 C81 123.35(15) . . ?
C56 C61 C62 121.75(15) . . ?
C56 C61 C60 116.68(16) . . ?
C60 C61 C62 121.53(15) . . ?
C74 C73 C68 119.48(17) . . ?
C74 C73 C72 122.03(17) . . ?
C72 C73 C68 118.49(18) . . ?
C4 C5 C47 121.05(17) . . ?
C6 C5 C4 116.98(16) . . ?
C6 C5 C47 121.97(17) . . ?
C3 C4 C5 122.79(17) . . ?
C22 C21 C16 119.36(17) . . ?
C22 C21 C20 121.94(19) . . ?
C20 C21 C16 118.70(19) . . ?
C74 C75 C76 119.09(16) . . ?
C74 C75 C80 122.16(17) . . ?
C80 C75 C76 118.74(18) . . ?
C22 C23 C24 118.89(18) . . ?
C22 C23 C28 122.58(19) . . ?
C28 C23 C24 118.5(2) . . ?
C15 C16 C21 119.62(17) . . ?
C15 C16 C17 123.19(17) . . ?
C17 C16 C21 117.17(17) . . ?
C5 C6 C7 123.37(17) . . ?
C7 C8 C9 110.55(14) . . ?
C7 C8 C51 108.78(17) . . ?
C7 C8 C52 109.66(16) . . ?
C9 C8 C51 109.35(16) . . ?
C9 C8 C52 108.01(17) . . ?
C51 C8 C52 110.5(2) . . ?
C63 C62 C101 108.07(16) . . ?
C61 C62 C63 110.04(13) . . ?
C61 C62 C101 108.01(16) . . ?
C61 C62 C100 110.50(16) . . ?
C100 C62 C63 109.93(16) . . ?
C100 C62 C101 110.24(19) . . ?
C57 C58 C59 122.29(17) . . ?
C78 C77 C76 121.54(18) . . ?
C58 C59 C95 120.15(17) . . ?
C60 C59 C58 117.18(16) . . ?
C60 C59 C95 122.60(18) . . ?
C102 C99 C65 113.7(2) . . ?
C102 C99 C55 108.1(4) . . ?
C102 C99 C1 107.1(4) . . ?
C55 C99 C65 109.1(2) . . ?
C55 C99 C1 109.7(4) . . ?
C1 C99 C65 109.1(2) . . ?
C103 C99 C65 108.0(3) . . ?
C1A C99 C65 108.7(3) . . ?
C1A C99 C103 108.5(6) . . ?
C55A C99 C65 113.4(3) . . ?
C55A C99 C103 109.5(6) . . ?
C55A C99 C1A 108.5(5) . . ?
C73 C74 C75 122.06(16) . . ?
C13 C12 C11 122.61(17) . . ?
C40 C39 C29 121.55(19) . . ?
C21 C22 C23 122.25(17) . . ?
C11 C10 C9 123.58(18) . . ?
C59 C60 C61 123.40(17) . . ?
C41 C42 C38 121.61(19) . . ?
C30 C31 C36 118.87(17) . . ?
C30 C31 C32 122.41(19) . . ?
C32 C31 C36 118.71(19) . . ?
C70 C69 C68 121.57(18) . . ?
C29 C30 C31 122.23(18) . . ?
C34 C35 C36 121.2(2) . . ?
C12 C11 C43 122.00(19) . . ?
C10 C11 C12 116.75(17) . . ?
C10 C11 C43 121.24(19) . . ?
C26 C25 C24 121.6(2) . . ?
C79 C80 C75 121.44(19) . . ?
C77 C78 C79 120.8(2) . . ?
C48 C47 C5 109.2(2) . . ?
C48 C47 C49 109.5(3) . . ?
C48 C47 C50 109.3(4) . . ?
C49 C47 C5 108.2(2) . . ?
C49 C47 C50 109.4(4) . . ?
C50 C47 C5 111.3(2) . . ?
C50A C47 C5 109.8(4) . . ?
C50A C47 C48A 105.4(7) . . ?
C49A C47 C5 110.2(3) . . ?
C49A C47 C50A 109.4(7) . . ?
C49A C47 C48A 108.4(7) . . ?
C48A C47 C5 113.6(3) . . ?
C39 C40 C41 120.08(18) . . ?
C93 C94 C90 120.9(2) . . ?
C71 C72 C73 121.41(19) . . ?
C18 C17 C16 121.6(2) . . ?
C19 C20 C21 121.6(2) . . ?
C69 C70 C71 120.53(19) . . ?
C72 C71 C70 120.3(2) . . ?
C80 C79 C78 120.01(19) . . ?
C42 C41 C40 120.7(2) . . ?
C35 C34 C33 121.1(2) . . ?
C11 C43 C45 106.5(3) . . ?
C11 C43 C44 107.4(4) . . ?
C11 C43 C44A 107.5(3) . . ?
C44 C43 C45 99.8(5) . . ?
C46 C43 C11 115.9(4) . . ?
C46 C43 C45 108.3(6) . . ?
C46 C43 C44 117.3(8) . . ?
C45A C43 C11 115.7(4) . . ?
C45A C43 C44A 101.6(7) . . ?
C45A C43 C46A 116.7(7) . . ?
C46A C43 C11 109.5(3) . . ?
C46A C43 C44A 104.4(6) . . ?
C33 C32 C31 121.9(2) . . ?
C87 C88 C89 120.0 . . ?
C88 C87 C82 120.0 . . ?
C88 C87 C86 121.12(16) . . ?
C82 C87 C86 118.85(17) . . ?
C87 C82 C81 120.0 . . ?
C87 C82 C83 117.56(13) . . ?
C81 C82 C83 122.42(13) . . ?
C82 C81 C57 118.49(10) . . ?
C90 C81 C57 121.05(10) . . ?
C90 C81 C82 120.0 . . ?
C81 C90 C94 122.39(12) . . ?
C89 C90 C94 117.57(12) . . ?
C89 C90 C81 120.0 . . ?
C88 C89 C91 120.28(16) . . ?
C90 C89 C88 120.0 . . ?
C90 C89 C91 119.69(17) . . ?
C20 C19 C18 120.0(2) . . ?
C32 C33 C34 119.6(2) . . ?
C17 C18 C19 120.9(2) . . ?
C27 C28 C23 121.8(2) . . ?
C25 C26 C27 120.8(2) . . ?
C94 C93 C92 120.4(3) . . ?
C92 C91 C89 120.7(2) . . ?
C28 C27 C26 120.1(2) . . ?
C91 C92 C93 120.6(2) . . ?
C83 C84 C85 120.6(3) . . ?
C84 C83 C82 121.9(2) . . ?
C85 C86 C87 120.5(2) . . ?
C86 C85 C84 120.5(3) . . ?
C97 C95 C59 111.93(17) . . ?
C98 C95 C59 111.0(2) . . ?
C98 C95 C97 107.5(2) . . ?
C98 C95 C96 110.8(3) . . ?
C96 C95 C59 107.92(18) . . ?
C96 C95 C97 107.7(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.343
_oxdiff_exptl_absorpt_empirical_full_min 0.198
####################################################################### 
# 
# 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_20221124-4cbr_auto
_database_code_depnum_ccdc_archive 'CCDC 2308127'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2023-11-15 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2023-11-15
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C51 H46 O'
_chemical_formula_sum            'C51 H46 O'
_chemical_formula_weight         674.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHOBr
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3923(2)
_cell_length_b                   18.1449(5)
_cell_length_c                   19.2809(5)
_cell_angle_alpha                83.916(2)
_cell_angle_beta                 81.263(2)
_cell_angle_gamma                81.850(2)
_cell_volume                     3885.01(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    31418
_cell_measurement_temperature    285.7(8)
_cell_measurement_theta_max      75.9390
_cell_measurement_theta_min      2.3410
_shelx_estimated_absorpt_T_max   0.942
_shelx_estimated_absorpt_T_min   0.923
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            58580
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.588
_diffrn_reflns_theta_max         66.588
_diffrn_reflns_theta_min         2.327
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      285.7(8)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     78.00 117.00   0.50    0.15    --   73.14  15.00 120.00   78
  2  ω     70.00 114.00   0.50    0.15    --   76.87  15.00  90.00   88
  3  ω     58.00  98.00   0.50    0.15    --   62.79  15.00  60.00   80
  4  ω     66.00 108.00   0.50    0.15    --   76.87  15.00   0.00   84
  5  ω     72.00 116.00   0.50    0.15    --   76.87  15.00-120.00   88
  6  ω     66.00  99.00   0.50    0.15    --   76.87  15.00-150.00   66
  7  ω     64.00  96.00   0.50    0.15    --   62.79  15.00-180.00   64
  8  ω     29.00  54.00   0.50    0.15    --   62.79-129.00  65.00   50
  9  ω     31.00  72.00   0.50    0.15    --   73.14-129.00  65.00   82
 10  ω     31.00  88.00   0.50    0.15    --   73.14-125.00 150.00  114
 11  ω     55.00 100.00   0.50    0.15    --   76.87-129.00  65.00   90
 12  ω     25.00  76.00   0.50    0.15    --   62.79-125.00   0.00  102
 13  ω     31.00  94.00   0.50    0.15    --   73.14-125.00-150.00  126
 14  ω     38.00  97.00   0.50    0.15    --   76.87-125.00 -90.00  118
 15  ω     47.00  98.00   0.50    0.15    --   76.87-125.00  90.00  102
 16  ω    -75.00 -47.00   0.50    0.15    --  -81.55 125.00  90.00   56
 17  ω    -91.00 -66.00   0.50    0.15    --  -76.57 129.00 138.00   50
 18  ω    -86.00 -61.00   0.50    0.15    --  -71.67 129.00 138.00   50
 19  ω    -75.00 -50.00   0.50    0.15    --  -81.55 129.00 138.00   50
 20  ω    -65.00 -40.00   0.50    0.15    --  -63.59 129.00 138.00   50
 21  ω    -83.00 -57.00   0.50    0.15    --  -76.57 125.00  30.00   52
 22  ω    -61.00 -26.00   0.50    0.15    --  -63.59 125.00   0.00   70
 23  ω   -102.00 -45.00   0.50    0.15    --  -81.55 125.00  60.00  114
 24  ω   -102.00 -47.00   0.50    0.15    --  -81.55 125.00  30.00  110
 25  ω   -102.00 -52.00   0.50    0.15    --  -81.55 125.00 150.00  100
 26  ω    -88.00 -30.00   0.50    0.15    --  -71.67 125.00 -90.00  116
 27  ω    -74.00 -48.00   0.50    0.15    --  -76.57 125.00-120.00   52
 28  ω   -102.00 -74.00   0.50    0.15    --  -81.55 125.00-120.00   56
 29  ω    -91.00 -29.00   0.50    0.15    --  -71.67 125.00-150.00  124
 30  ω   -102.00 -44.00   0.50    0.15    --  -81.55 125.00-180.00  116
 31  ω   -102.00 -48.00   0.50    0.15    --  -81.55 125.00-150.00  108
 32  ω   -102.00 -76.00   0.50    0.15    --  -81.55 125.00 -90.00   52
 33  ω   -102.00 -44.00   0.50    0.15    --  -81.55 125.00 -60.00  116
 34  ω   -101.00 -75.00   0.50    0.15    --  -81.55 125.00 -30.00   52
 35  ω   -102.00 -77.00   0.50    0.15    --  -81.55 125.00   0.00   50
 36  ω   -102.00 -69.00   0.50    0.15    --  -81.55 125.00 120.00   66
 37  ω   -124.00 -75.00   0.50    0.15    --  -81.55 -15.00 150.00   98
 38  ω   -101.00 -63.00   0.50    0.15    --  -63.59 -15.00  90.00   76
 39  ω   -118.00 -70.00   0.50    0.15    --  -76.57 -15.00  60.00   96
 40  ω    -98.00 -73.00   0.50    0.15    --  -81.55 -15.00   0.00   50
 41  ω    -79.00 -54.00   0.50    0.15    --  -63.59 -15.00 -90.00   50
 42  ω   -124.00 -99.00   0.50    0.15    --  -81.55 -15.00 -60.00   50
 43  ω   -116.00 -77.00   0.50    0.15    --  -81.55 -15.00-120.00   78
 44  ω    -82.00 -54.00   0.50    0.15    --  -63.59 -15.00-150.00   56
 45  ω   -105.00 -55.00   0.50    0.15    --  -63.59 -15.00-180.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0379589000
_diffrn_orient_matrix_UB_12      -0.0841653000
_diffrn_orient_matrix_UB_13      0.0166515000
_diffrn_orient_matrix_UB_21      0.0334464000
_diffrn_orient_matrix_UB_22      -0.0093579000
_diffrn_orient_matrix_UB_23      -0.0793321000
_diffrn_orient_matrix_UB_31      0.1283364000
_diffrn_orient_matrix_UB_32      0.0155007000
_diffrn_orient_matrix_UB_33      0.0036219000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11486
_reflns_number_total             13643
_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       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.161
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       0.00120(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1047
_refine_ls_number_reflns         13643
_refine_ls_number_restraints     143
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0457
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0713P)²+0.5459P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1383
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C71-C70
 1.39 with sigma of 0.01
 C98-C96
 1.54 with sigma of 0.01
 C46-C47 \\sim C46-C47A
 with sigma of 0.02
 C46-C102 \\sim C46-C103
 with sigma of 0.02
 C46-C101 \\sim C46-C1A
 with sigma of 0.02
 C92-C94 \\sim C92-C94A
 with sigma of 0.02
 C92-C93 \\sim C92-C93A
 with sigma of 0.02
 C92-C95 \\sim C92-C95A
 with sigma of 0.02
 C43-C45 \\sim C43-C45A
 with sigma of 0.02
 C43-C44 \\sim C43-C44A
 with sigma of 0.02
 C43-C3 \\sim C43-C3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C47) \\sim Ueq, Uanis(C47A) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C1A)
\\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C45A) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C44A)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C93A) \\sim Ueq, Uanis(C93) \\sim Ueq,
Uanis(C94A) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C95A) \\sim Ueq, Uanis(C94)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C66)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C47A)=Sof(H47D)=Sof(H47E)=Sof(H47F)=Sof(C103)=Sof(H10G)=Sof(H10H)=
 Sof(H10I)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C102)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=Sof(C101)=Sof(H10D)=Sof(H10E)=Sof(H10F)=FVAR(1)
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C44A)=Sof(H44D)=Sof(H44E)=
 Sof(H44F)=Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(2)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(2)
 Sof(C95A)=Sof(H95D)=Sof(H95E)=Sof(H95F)=Sof(C93A)=Sof(H93D)=Sof(H93E)=
 Sof(H93F)=Sof(C94A)=Sof(H94D)=Sof(H94E)=Sof(H94F)=1-FVAR(3)
 Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=
 Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(H95C)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C59(H59), C61(H61), C53(H53), C84(H84), C12(H12), C14(H14), C8(H8), C6(H6),
 C79(H79), C39(H39), C91(H91), C42(H42), C55(H55), C35(H35), C22(H22), C30(H30),
  C25(H25), C40(H40), C83(H83), C81(H81), C90(H90), C17(H17), C77(H77),
 C88(H88), C20(H20), C41(H41), C82(H82), C34(H34), C89(H89), C66(H66), C32(H32),
  C19(H19), C33(H33), C18(H18), C28(H28), C26(H26), C76(H76), C71(H71),
 C27(H27), C75(H75), C74(H74), C69(H69), C67(H67), C68(H68)
5.b Idealised Me refined as rotating group:
 C99(H99A,H99B,H99C), C100(H10J,H10K,H10L), C49(H49A,H49B,H49C), C98(H98A,H98B,
 H98C), C48(H48A,H48B,H48C), C97(H97A,H97B,H97C), C93(H93A,H93B,H93C), C94(H94A,
 H94B,H94C), C47(H47A,H47B,H47C), C45(H45A,H45B,H45C), C95(H95A,H95B,H95C),
 C44(H44A,H44B,H44C), C50(H50A,H50B,H50C), C102(H10A,H10B,H10C), C3(H3A,H3B,
 H3C), C101(H10D,H10E,H10F), C47A(H47D,H47E,H47F), C103(H10G,H10H,H10I),
 C1A(H1AA,H1AB,H1AC), C3A(H3AA,H3AB,H3AC), C44A(H44D,H44E,H44F), C45A(H45D,H45E,
 H45F), C95A(H95D,H95E,H95F), C93A(H93D,H93E,H93F), C94A(H94D,H94E,H94F)
;
_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
O3 O 0.86030(8) 0.16314(5) 0.87669(5) 0.0488(2) Uani 1 1 d . . . . .
O50 O 0.58284(9) 0.67854(5) 0.58103(5) 0.0511(2) Uani 1 1 d . . . . .
C86 C 0.64507(11) 0.58617(7) 0.69389(6) 0.0412(3) Uani 1 1 d . . . . .
C2 C 0.80952(11) 0.11598(7) 0.92971(7) 0.0421(3) Uani 1 1 d . . . . .
C58 C 0.67228(11) 0.59198(7) 0.49443(6) 0.0423(3) Uani 1 1 d . . . . .
C11 C 0.82329(11) 0.03929(7) 0.92716(7) 0.0445(3) Uani 1 1 d . . . . .
C15 C 0.72714(12) 0.23534(7) 0.98510(6) 0.0435(3) Uani 1 1 d . . . . .
C51 C 0.53857(12) 0.72826(7) 0.52956(7) 0.0445(3) Uani 1 1 d . . . . .
C63 C 0.64461(11) 0.61122(7) 0.56313(6) 0.0410(3) Uani 1 1 d . . . . .
C62 C 0.67810(11) 0.56309(7) 0.62018(6) 0.0411(3) Uani 1 1 d . . . . .
C37 C 0.94015(11) 0.26787(8) 0.77779(7) 0.0446(3) Uani 1 1 d . . . . .
C87 C 0.73357(12) 0.60396(7) 0.73046(7) 0.0447(3) Uani 1 1 d . . . . .
C60 C 0.77104(11) 0.47113(7) 0.53895(7) 0.0445(3) Uani 1 1 d . . . . .
C4 C 0.92401(11) 0.13379(7) 0.81726(7) 0.0433(3) Uani 1 1 d . . . . .
C85 C 0.52559(11) 0.58755(7) 0.72691(7) 0.0433(3) Uani 1 1 d . . . . .
C1 C 0.74274(11) 0.15171(7) 0.98656(7) 0.0443(3) Uani 1 1 d . . . . .
C59 C 0.73545(12) 0.52158(8) 0.48414(7) 0.0456(3) Uani 1 1 d . . . . .
H59 H 0.754839 0.507553 0.438370 0.055 Uiso 1 1 calc R U . . .
C38 C 0.82190(12) 0.30424(8) 0.77861(7) 0.0449(3) Uani 1 1 d . . . . .
C56 C 0.56013(12) 0.71617(8) 0.45881(7) 0.0461(3) Uani 1 1 d . . . . .
C36 C 1.03172(12) 0.30729(8) 0.79002(7) 0.0478(3) Uani 1 1 d . . . . .
C52 C 0.47134(12) 0.79286(8) 0.55462(7) 0.0484(3) Uani 1 1 d . . . . .
C61 C 0.74108(11) 0.49383(7) 0.60693(7) 0.0447(3) Uani 1 1 d . . . . .
H61 H 0.764135 0.461426 0.644571 0.054 Uiso 1 1 calc R U . . .
C29 C 0.79601(12) 0.38137(8) 0.79091(7) 0.0480(3) Uani 1 1 d . . . . .
C24 C 0.82498(12) 0.27317(8) 0.99015(7) 0.0466(3) Uani 1 1 d . . . . .
C5 C 0.96679(11) 0.18726(8) 0.76565(7) 0.0469(3) Uani 1 1 d . . . . .
C9 C 0.94466(11) 0.05829(8) 0.80856(7) 0.0468(3) Uani 1 1 d . . . . .
C53 C 0.42334(13) 0.84616(8) 0.50616(8) 0.0539(3) Uani 1 1 d . . . . .
H53 H 0.377938 0.889382 0.522109 0.065 Uiso 1 1 calc R U . . .
C16 C 0.61472(12) 0.27692(8) 0.97644(7) 0.0480(3) Uani 1 1 d . . . . .
C92 C 0.84042(13) 0.39409(8) 0.52504(8) 0.0532(3) Uani 1 1 d D . . . .
C84 C 0.43191(13) 0.57147(8) 0.69226(8) 0.0529(3) Uani 1 1 d . . . . .
H84 H 0.448972 0.559926 0.645643 0.064 Uiso 1 1 calc R U . . .
C12 C 0.76822(12) -0.00236(8) 0.98512(8) 0.0509(3) Uani 1 1 d . . . . .
H12 H 0.776570 -0.054040 0.984565 0.061 Uiso 1 1 calc R U . . .
C14 C 0.69041(12) 0.10696(8) 1.04243(7) 0.0508(3) Uani 1 1 d . . . . .
H14 H 0.645941 0.129641 1.080804 0.061 Uiso 1 1 calc R U . . .
C13 C 0.70206(12) 0.02934(8) 1.04314(8) 0.0509(3) Uani 1 1 d . . . . .
C57 C 0.63978(13) 0.64697(8) 0.43216(7) 0.0508(3) Uani 1 1 d . . . . .
C21 C 0.60212(14) 0.35714(8) 0.97111(7) 0.0534(3) Uani 1 1 d . . . . .
C10 C 0.89605(13) 0.00090(8) 0.86515(8) 0.0528(3) Uani 1 1 d . . . . .
C64 C 0.45605(13) 0.80108(7) 0.63193(8) 0.0506(3) Uani 1 1 d . . . . .
C78 C 0.70301(13) 0.62003(8) 0.80303(7) 0.0519(3) Uani 1 1 d . . . . .
C80 C 0.49568(13) 0.60452(8) 0.79911(7) 0.0505(3) Uani 1 1 d . . . . .
C23 C 0.81084(14) 0.35307(8) 0.98547(7) 0.0544(3) Uani 1 1 d . . . . .
C8 C 1.01118(13) 0.03674(9) 0.74532(8) 0.0568(4) Uani 1 1 d . . . . .
H8 H 1.025910 -0.013893 0.738496 0.068 Uiso 1 1 calc R U . . .
C6 C 1.03243(13) 0.16257(9) 0.70375(8) 0.0562(4) Uani 1 1 d . . . . .
H6 H 1.061271 0.197624 0.668932 0.067 Uiso 1 1 calc R U . . .
C73 C 0.34507(14) 0.79468(8) 0.67366(8) 0.0556(4) Uani 1 1 d . . . . .
C54 C 0.44095(13) 0.83706(8) 0.43422(8) 0.0529(3) Uani 1 1 d . . . . .
C79 C 0.58521(14) 0.61972(9) 0.83504(8) 0.0576(4) Uani 1 1 d . . . . .
H79 H 0.565704 0.629992 0.881946 0.069 Uiso 1 1 calc R U . . .
C39 C 0.67500(13) 0.41676(9) 0.79299(8) 0.0566(4) Uani 1 1 d . . . . .
H39 H 0.657117 0.466835 0.801734 0.068 Uiso 1 1 calc R U . . .
C91 C 0.85490(13) 0.60705(8) 0.69897(8) 0.0541(3) Uani 1 1 d . . . . .
H91 H 0.876885 0.597846 0.651915 0.065 Uiso 1 1 calc R U . . .
C42 C 0.72492(13) 0.26675(9) 0.76811(8) 0.0557(4) Uani 1 1 d . . . . .
H42 H 0.739334 0.216487 0.759821 0.067 Uiso 1 1 calc R U . . .
C55 C 0.50929(13) 0.77211(8) 0.41261(7) 0.0526(3) Uani 1 1 d . . . . .
H55 H 0.522138 0.765262 0.364800 0.063 Uiso 1 1 calc R U . . .
C7 C 1.05649(14) 0.08720(9) 0.69206(8) 0.0597(4) Uani 1 1 d . . . . .
C35 C 1.15106(13) 0.27247(10) 0.79554(8) 0.0581(4) Uani 1 1 d . . . . .
H35 H 1.170039 0.221448 0.791246 0.070 Uiso 1 1 calc R U . . .
C22 C 0.70020(15) 0.39276(8) 0.97506(8) 0.0591(4) Uani 1 1 d . . . . .
H22 H 0.691965 0.444714 0.970644 0.071 Uiso 1 1 calc R U . . .
C31 C 1.00531(13) 0.38557(8) 0.79978(8) 0.0541(3) Uani 1 1 d . . . . .
C65 C 0.55760(14) 0.80912(8) 0.66253(9) 0.0583(4) Uani 1 1 d . . . . .
C30 C 0.88830(14) 0.42029(8) 0.80016(8) 0.0559(4) Uani 1 1 d . . . . .
H30 H 0.871362 0.470927 0.806776 0.067 Uiso 1 1 calc R U . . .
C46 C 0.64215(14) -0.01826(9) 1.10583(8) 0.0616(4) Uani 1 1 d D . . . .
C25 C 0.94036(14) 0.23492(10) 1.00007(9) 0.0635(4) Uani 1 1 d . . . . .
H25 H 0.952375 0.182991 1.002502 0.076 Uiso 1 1 calc R U . . .
C40 C 0.58668(14) 0.37889(10) 0.78251(8) 0.0627(4) Uani 1 1 d . . . . .
H40 H 0.508796 0.402961 0.783564 0.075 Uiso 1 1 calc R U . . .
C83 C 0.31784(14) 0.57261(10) 0.72579(9) 0.0648(4) Uani 1 1 d . . . . .
H83 H 0.258102 0.562135 0.701763 0.078 Uiso 1 1 calc R U . . .
C81 C 0.37474(14) 0.60473(10) 0.83178(9) 0.0650(4) Uani 1 1 d . . . . .
H81 H 0.354630 0.615655 0.878481 0.078 Uiso 1 1 calc R U . . .
C90 C 0.93872(14) 0.62308(10) 0.73606(10) 0.0655(4) Uani 1 1 d . . . . .
H90 H 1.016844 0.625153 0.714066 0.079 Uiso 1 1 calc R U . . .
C17 C 0.51194(14) 0.24288(10) 0.97080(9) 0.0649(4) Uani 1 1 d . . . . .
H17 H 0.517691 0.191067 0.972958 0.078 Uiso 1 1 calc R U . . .
C96 C 0.38090(15) 0.89616(10) 0.38313(9) 0.0659(4) Uani 1 1 d D . . . .
C72 C 0.33672(17) 0.79538(9) 0.74893(9) 0.0698(5) Uani 1 1 d . . . . .
C77 C 0.24021(15) 0.78556(9) 0.64562(10) 0.0682(4) Uani 1 1 d . . . . .
H77 H 0.243984 0.782942 0.597408 0.082 Uiso 1 1 calc R U . . .
C88 C 0.79499(15) 0.63556(10) 0.83973(9) 0.0658(4) Uani 1 1 d . . . . .
H88 H 0.776183 0.645165 0.886829 0.079 Uiso 1 1 calc R U . . .
C20 C 0.48825(16) 0.39793(11) 0.96140(9) 0.0694(5) Uani 1 1 d . . . . .
H20 H 0.479728 0.449879 0.957388 0.083 Uiso 1 1 calc R U . . .
C41 C 0.61212(14) 0.30307(10) 0.77000(9) 0.0643(4) Uani 1 1 d . . . . .
H41 H 0.550544 0.277327 0.762876 0.077 Uiso 1 1 calc R U . . .
C82 C 0.28902(15) 0.58947(10) 0.79655(10) 0.0700(5) Uani 1 1 d . . . . .
H82 H 0.210631 0.590046 0.818914 0.084 Uiso 1 1 calc R U . . .
C34 C 1.23699(14) 0.31259(12) 0.80693(9) 0.0713(5) Uani 1 1 d . . . . .
H34 H 1.313708 0.288599 0.810928 0.086 Uiso 1 1 calc R U . . .
C70 C 0.54970(17) 0.80713(10) 0.73720(10) 0.0719(5) Uani 1 1 d D . . . .
C89 C 0.90849(16) 0.63669(11) 0.80788(10) 0.0704(5) Uani 1 1 d . . . . .
H89 H 0.967103 0.646420 0.833150 0.085 Uiso 1 1 calc R U . . .
C66 C 0.67132(15) 0.81718(10) 0.62178(11) 0.0706(5) Uani 1 1 d . U . . .
H66 H 0.678060 0.819881 0.572930 0.085 Uiso 1 1 calc R U . . .
C32 C 1.10000(16) 0.42499(11) 0.80977(10) 0.0708(5) Uani 1 1 d . . . . .
H32 H 1.084275 0.476086 0.814315 0.085 Uiso 1 1 calc R U . . .
C19 C 0.39336(17) 0.36318(13) 0.95791(10) 0.0798(5) Uani 1 1 d . . . . .
H19 H 0.319677 0.390984 0.952585 0.096 Uiso 1 1 calc R U . . .
C99 C 0.75676(17) 0.67210(11) 0.39110(9) 0.0804(6) Uani 1 1 d . . . . .
H99A H 0.738154 0.707998 0.352780 0.121 Uiso 1 1 calc R U . . .
H99B H 0.807479 0.629561 0.372935 0.121 Uiso 1 1 calc R U . . .
H99C H 0.797363 0.694353 0.422074 0.121 Uiso 1 1 calc R U . . .
C33 C 1.21159(17) 0.39023(12) 0.81278(10) 0.0774(5) Uani 1 1 d . . . . .
H33 H 1.272163 0.417387 0.818743 0.093 Uiso 1 1 calc R U . . .
C18 C 0.40512(15) 0.28482(13) 0.96230(11) 0.0797(5) Uani 1 1 d . . . . .
H18 H 0.339002 0.261155 0.959369 0.096 Uiso 1 1 calc R U . . .
C43 C 1.13116(17) 0.06042(12) 0.62390(10) 0.0819(6) Uani 1 1 d D . . . .
C100 C 0.5761(2) 0.60874(11) 0.38418(10) 0.0845(6) Uani 1 1 d . . . . .
H10J H 0.507114 0.589754 0.411132 0.127 Uiso 1 1 calc R U . . .
H10K H 0.629883 0.568241 0.364390 0.127 Uiso 1 1 calc R U . . .
H10L H 0.551477 0.644270 0.346949 0.127 Uiso 1 1 calc R U . . .
C28 C 0.91130(19) 0.38972(11) 0.99138(10) 0.0765(5) Uani 1 1 d . . . . .
H28 H 0.902940 0.441648 0.988413 0.092 Uiso 1 1 calc R U . . .
C26 C 1.03249(17) 0.27194(13) 1.00603(11) 0.0825(6) Uani 1 1 d . . . . .
H26 H 1.106140 0.245281 1.013410 0.099 Uiso 1 1 calc R U . . .
C76 C 0.13421(17) 0.78058(11) 0.68824(13) 0.0860(6) Uani 1 1 d . . . . .
H76 H 0.066283 0.775216 0.668863 0.103 Uiso 1 1 calc R U . . .
C71 C 0.4400(2) 0.79991(11) 0.77786(10) 0.0828(6) Uani 1 1 d D . . . .
H71 H 0.435152 0.798017 0.826587 0.099 Uiso 1 1 calc R U . . .
C49 C 1.00087(18) -0.05182(11) 0.89178(12) 0.0948(7) Uani 1 1 d . . . . .
H49A H 1.046606 -0.024135 0.915204 0.142 Uiso 1 1 calc R U . . .
H49B H 1.051235 -0.073481 0.852606 0.142 Uiso 1 1 calc R U . . .
H49C H 0.970224 -0.090777 0.924170 0.142 Uiso 1 1 calc R U . . .
C98 C 0.4357(2) 0.88779(13) 0.30712(10) 0.0949(7) Uani 1 1 d D . . . .
H98A H 0.520020 0.890835 0.302158 0.142 Uiso 1 1 calc R U . . .
H98B H 0.398527 0.927016 0.277133 0.142 Uiso 1 1 calc R U . . .
H98C H 0.423109 0.840236 0.293984 0.142 Uiso 1 1 calc R U . . .
C27 C 1.01816(19) 0.35051(13) 1.00117(12) 0.0884(6) Uani 1 1 d . . . . .
H27 H 1.082561 0.375506 1.004730 0.106 Uiso 1 1 calc R U . . .
C75 C 0.1269(2) 0.78352(12) 0.76198(14) 0.0957(7) Uani 1 1 d . . . . .
H75 H 0.053781 0.780982 0.790555 0.115 Uiso 1 1 calc R U . . .
C74 C 0.2240(2) 0.78992(12) 0.79068(12) 0.0903(6) Uani 1 1 d . . . . .
H74 H 0.217647 0.790816 0.839251 0.108 Uiso 1 1 calc R U . . .
C69 C 0.6564(2) 0.81173(12) 0.76707(13) 0.0967(7) Uani 1 1 d . U . . .
H69 H 0.652815 0.810641 0.815675 0.116 Uiso 1 1 calc R U . . .
C48 C 0.8158(2) -0.04338(13) 0.83258(12) 0.0994(8) Uani 1 1 d . . . . .
H48A H 0.785810 -0.080695 0.867202 0.149 Uiso 1 1 calc R U . . .
H48B H 0.861656 -0.067118 0.793135 0.149 Uiso 1 1 calc R U . . .
H48C H 0.749921 -0.009956 0.817060 0.149 Uiso 1 1 calc R U . . .
C67 C 0.76931(19) 0.82098(12) 0.65205(14) 0.0914(6) Uani 1 1 d . U . . .
H67 H 0.842210 0.825872 0.623962 0.110 Uiso 1 1 calc R U . . .
C68 C 0.7621(2) 0.81763(13) 0.72533(17) 0.1044(8) Uani 1 1 d . U . . .
H68 H 0.830529 0.819464 0.745595 0.125 Uiso 1 1 calc R U . . .
C97 C 0.25031(19) 0.8849(2) 0.38957(15) 0.1424(13) Uani 1 1 d . . . . .
H97A H 0.244645 0.835879 0.376841 0.214 Uiso 1 1 calc R U . . .
H97B H 0.210406 0.921777 0.358667 0.214 Uiso 1 1 calc R U . . .
H97C H 0.213129 0.889774 0.437269 0.214 Uiso 1 1 calc R U . . .
C93 C 0.8693(5) 0.3468(2) 0.59138(18) 0.0908(18) Uani 0.594(6) 1 d D U P A 1
H93A H 0.907245 0.298242 0.579469 0.136 Uiso 0.594(6) 1 calc R U P A 1
H93B H 0.796741 0.341933 0.623098 0.136 Uiso 0.594(6) 1 calc R U P A 1
H93C H 0.922344 0.370396 0.613601 0.136 Uiso 0.594(6) 1 calc R U P A 1
C94 C 0.9575(4) 0.4034(2) 0.4771(3) 0.104(2) Uani 0.594(6) 1 d D U P A 1
H94A H 1.006224 0.429481 0.500136 0.156 Uiso 0.594(6) 1 calc R U P A 1
H94B H 0.940847 0.431508 0.433912 0.156 Uiso 0.594(6) 1 calc R U P A 1
H94C H 0.999361 0.355102 0.467196 0.156 Uiso 0.594(6) 1 calc R U P A 1
C47 C 0.6642(5) -0.10102(19) 1.0935(2) 0.114(2) Uani 0.667(6) 1 d D U P B 1
H47A H 0.633534 -0.108300 1.051337 0.171 Uiso 0.667(6) 1 calc R U P B 1
H47B H 0.624299 -0.129158 1.132820 0.171 Uiso 0.667(6) 1 calc R U P B 1
H47C H 0.748624 -0.117707 1.088498 0.171 Uiso 0.667(6) 1 calc R U P B 1
C45 C 1.2579(4) 0.0740(8) 0.6224(4) 0.155(5) Uani 0.490(7) 1 d D U P C 1
H45A H 1.305081 0.057002 0.580065 0.233 Uiso 0.490(7) 1 calc R U P C 1
H45B H 1.289395 0.047176 0.662583 0.233 Uiso 0.490(7) 1 calc R U P C 1
H45C H 1.260752 0.126466 0.623436 0.233 Uiso 0.490(7) 1 calc R U P C 1
C95 C 0.7643(4) 0.3508(2) 0.4892(3) 0.109(2) Uani 0.594(6) 1 d D U P A 1
H95A H 0.809557 0.304120 0.476806 0.163 Uiso 0.594(6) 1 calc R U P A 1
H95B H 0.742263 0.379647 0.447357 0.163 Uiso 0.594(6) 1 calc R U P A 1
H95C H 0.693349 0.341461 0.520801 0.163 Uiso 0.594(6) 1 calc R U P A 1
C44 C 1.0870(6) 0.1143(4) 0.5596(3) 0.107(2) Uani 0.490(7) 1 d D U P C 1
H44A H 1.100534 0.164455 0.564381 0.160 Uiso 0.490(7) 1 calc R U P C 1
H44B H 1.003126 0.112933 0.559586 0.160 Uiso 0.490(7) 1 calc R U P C 1
H44C H 1.130879 0.098009 0.516204 0.160 Uiso 0.490(7) 1 calc R U P C 1
C50 C 0.3931(3) 0.97421(12) 0.39920(16) 0.1376(12) Uani 1 1 d . . . . .
H50A H 0.342980 0.985576 0.442440 0.206 Uiso 1 1 calc R U . . .
H50B H 0.368978 1.009415 0.361598 0.206 Uiso 1 1 calc R U . . .
H50C H 0.474944 0.977236 0.403782 0.206 Uiso 1 1 calc R U . . .
C102 C 0.6906(4) -0.0067(3) 1.17180(17) 0.1028(18) Uani 0.667(6) 1 d D U P B 1
H10A H 0.775677 -0.021243 1.165874 0.154 Uiso 0.667(6) 1 calc R U P B 1
H10B H 0.653568 -0.036580 1.210887 0.154 Uiso 0.667(6) 1 calc R U P B 1
H10C H 0.673544 0.045057 1.180685 0.154 Uiso 0.667(6) 1 calc R U P B 1
C3 C 1.1100(11) -0.0125(5) 0.6056(5) 0.173(6) Uani 0.490(7) 1 d D U P C 1
H3A H 1.149120 -0.020643 0.558784 0.259 Uiso 0.490(7) 1 calc R U P C 1
H3B H 1.025483 -0.013501 0.607589 0.259 Uiso 0.490(7) 1 calc R U P C 1
H3C H 1.141426 -0.051106 0.638310 0.259 Uiso 0.490(7) 1 calc R U P C 1
C101 C 0.5089(3) 0.0070(3) 1.1144(2) 0.1074(19) Uani 0.667(6) 1 d D U P B 1
H10D H 0.493752 0.057785 1.126504 0.161 Uiso 0.667(6) 1 calc R U P B 1
H10E H 0.469358 -0.024461 1.151180 0.161 Uiso 0.667(6) 1 calc R U P B 1
H10F H 0.479090 0.003703 1.071041 0.161 Uiso 0.667(6) 1 calc R U P B 1
C47A C 0.5458(8) -0.0561(6) 1.0828(4) 0.105(4) Uani 0.333(6) 1 d D U P B 2
H47D H 0.487920 -0.018962 1.063648 0.158 Uiso 0.333(6) 1 calc R U P B 2
H47E H 0.507056 -0.084153 1.122643 0.158 Uiso 0.333(6) 1 calc R U P B 2
H47F H 0.581562 -0.089230 1.047558 0.158 Uiso 0.333(6) 1 calc R U P B 2
C103 C 0.7349(7) -0.0778(5) 1.1353(5) 0.111(4) Uani 0.333(6) 1 d D U P B 2
H10G H 0.779920 -0.104839 1.097621 0.166 Uiso 0.333(6) 1 calc R U P B 2
H10H H 0.694993 -0.111720 1.169394 0.166 Uiso 0.333(6) 1 calc R U P B 2
H10I H 0.788187 -0.054214 1.157288 0.166 Uiso 0.333(6) 1 calc R U P B 2
C1A C 0.5842(11) 0.0270(4) 1.1683(4) 0.120(4) Uani 0.333(6) 1 d D U P B 2
H1AA H 0.643119 0.052714 1.182919 0.180 Uiso 0.333(6) 1 calc R U P B 2
H1AB H 0.553768 -0.006317 1.206796 0.180 Uiso 0.333(6) 1 calc R U P B 2
H1AC H 0.519772 0.062643 1.154184 0.180 Uiso 0.333(6) 1 calc R U P B 2
C3A C 1.0626(7) 0.0065(6) 0.5949(4) 0.140(4) Uani 0.510(7) 1 d D U P C 2
H3AA H 1.114655 -0.019677 0.559035 0.210 Uiso 0.510(7) 1 calc R U P C 2
H3AB H 0.995421 0.034223 0.575141 0.210 Uiso 0.510(7) 1 calc R U P C 2
H3AC H 1.034616 -0.028709 0.632339 0.210 Uiso 0.510(7) 1 calc R U P C 2
C44A C 1.1806(12) 0.1183(4) 0.5755(5) 0.185(6) Uani 0.510(7) 1 d D U P C 2
H44D H 1.211951 0.151672 0.601338 0.277 Uiso 0.510(7) 1 calc R U P C 2
H44E H 1.118953 0.145599 0.550709 0.277 Uiso 0.510(7) 1 calc R U P C 2
H44F H 1.243777 0.095948 0.542443 0.277 Uiso 0.510(7) 1 calc R U P C 2
C45A C 1.2409(4) 0.0025(4) 0.6481(3) 0.0983(19) Uani 0.510(7) 1 d D U P C 2
H45D H 1.293517 -0.013679 0.607286 0.147 Uiso 0.510(7) 1 calc R U P C 2
H45E H 1.210507 -0.039963 0.675244 0.147 Uiso 0.510(7) 1 calc R U P C 2
H45F H 1.284129 0.026535 0.676348 0.147 Uiso 0.510(7) 1 calc R U P C 2
C95A C 0.8739(8) 0.3832(3) 0.4476(3) 0.104(3) Uani 0.406(6) 1 d D U P A 2
H95D H 0.919451 0.334896 0.442109 0.156 Uiso 0.406(6) 1 calc R U P A 2
H95E H 0.921027 0.421226 0.425317 0.156 Uiso 0.406(6) 1 calc R U P A 2
H95F H 0.802454 0.386434 0.426044 0.156 Uiso 0.406(6) 1 calc R U P A 2
C93A C 0.7643(6) 0.3344(3) 0.5584(5) 0.111(3) Uani 0.406(6) 1 d D U P A 2
H93D H 0.803762 0.286295 0.546018 0.166 Uiso 0.406(6) 1 calc R U P A 2
H93E H 0.687933 0.343678 0.541719 0.166 Uiso 0.406(6) 1 calc R U P A 2
H93F H 0.753006 0.335380 0.608691 0.166 Uiso 0.406(6) 1 calc R U P A 2
C94A C 0.9524(6) 0.3840(4) 0.5609(5) 0.122(4) Uani 0.406(6) 1 d D U P A 2
H94D H 0.930650 0.394198 0.609397 0.182 Uiso 0.406(6) 1 calc R U P A 2
H94E H 1.006277 0.417955 0.537671 0.182 Uiso 0.406(6) 1 calc R U P A 2
H94F H 0.990955 0.333604 0.558394 0.182 Uiso 0.406(6) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O3 C2 1.3738(15) . ?
O3 C4 1.3749(15) . ?
O50 C51 1.3734(15) . ?
O50 C63 1.3707(15) . ?
C86 C62 1.5020(17) . ?
C86 C87 1.4051(18) . ?
C86 C85 1.4103(18) . ?
C2 C11 1.3833(18) . ?
C2 C1 1.3994(18) . ?
C58 C63 1.3841(17) . ?
C58 C59 1.3923(18) . ?
C58 C57 1.5332(18) . ?
C11 C12 1.3987(19) . ?
C11 C10 1.5209(19) . ?
C15 C1 1.5005(18) . ?
C15 C24 1.4095(19) . ?
C15 C16 1.4148(19) . ?
C51 C56 1.3841(18) . ?
C51 C52 1.3953(19) . ?
C63 C62 1.3956(18) . ?
C62 C61 1.3842(18) . ?
C37 C38 1.4122(18) . ?
C37 C36 1.4062(19) . ?
C37 C5 1.4870(19) . ?
C87 C78 1.4402(18) . ?
C87 C91 1.4290(19) . ?
C60 C59 1.3925(19) . ?
C60 C61 1.3940(18) . ?
C60 C92 1.5337(18) . ?
C4 C5 1.3968(19) . ?
C4 C9 1.3804(19) . ?
C85 C84 1.4200(19) . ?
C85 C80 1.4373(18) . ?
C1 C14 1.3899(19) . ?
C38 C29 1.4262(19) . ?
C38 C42 1.426(2) . ?
C56 C57 1.5285(19) . ?
C56 C55 1.3991(19) . ?
C36 C35 1.430(2) . ?
C36 C31 1.436(2) . ?
C52 C53 1.386(2) . ?
C52 C64 1.4950(19) . ?
C29 C39 1.433(2) . ?
C29 C30 1.389(2) . ?
C24 C23 1.431(2) . ?
C24 C25 1.427(2) . ?
C5 C6 1.3899(19) . ?
C9 C10 1.523(2) . ?
C9 C8 1.397(2) . ?
C53 C54 1.395(2) . ?
C16 C21 1.436(2) . ?
C16 C17 1.422(2) . ?
C92 C93 1.515(3) . ?
C92 C94 1.522(4) . ?
C92 C95 1.529(4) . ?
C92 C95A 1.512(5) . ?
C92 C93A 1.512(5) . ?
C92 C94A 1.522(6) . ?
C84 C83 1.359(2) . ?
C12 C13 1.381(2) . ?
C14 C13 1.395(2) . ?
C13 C46 1.5388(19) . ?
C57 C99 1.545(2) . ?
C57 C100 1.531(2) . ?
C21 C22 1.383(2) . ?
C21 C20 1.428(2) . ?
C10 C49 1.537(2) . ?
C10 C48 1.538(2) . ?
C64 C73 1.404(2) . ?
C64 C65 1.408(2) . ?
C78 C79 1.390(2) . ?
C78 C88 1.424(2) . ?
C80 C79 1.390(2) . ?
C80 C81 1.425(2) . ?
C23 C22 1.392(2) . ?
C23 C28 1.427(2) . ?
C8 C7 1.390(2) . ?
C6 C7 1.391(2) . ?
C73 C72 1.441(2) . ?
C73 C77 1.421(2) . ?
C54 C55 1.383(2) . ?
C54 C96 1.537(2) . ?
C39 C40 1.346(2) . ?
C91 C90 1.356(2) . ?
C42 C41 1.356(2) . ?
C7 C43 1.538(2) . ?
C35 C34 1.355(2) . ?
C31 C30 1.391(2) . ?
C31 C32 1.422(2) . ?
C65 C70 1.426(2) . ?
C65 C66 1.427(2) . ?
C46 C47 1.525(4) . ?
C46 C102 1.507(4) . ?
C46 C101 1.511(4) . ?
C46 C47A 1.516(6) . ?
C46 C103 1.528(6) . ?
C46 C1A 1.541(7) . ?
C25 C26 1.349(2) . ?
C40 C41 1.404(2) . ?
C83 C82 1.409(2) . ?
C81 C82 1.345(2) . ?
C90 C89 1.414(2) . ?
C17 C18 1.363(2) . ?
C96 C98 1.517(3) . ?
C96 C97 1.515(3) . ?
C96 C50 1.511(3) . ?
C72 C71 1.392(3) . ?
C72 C74 1.418(3) . ?
C77 C76 1.362(3) . ?
C88 C89 1.346(2) . ?
C20 C19 1.340(3) . ?
C34 C33 1.410(3) . ?
C70 C71 1.386(3) . ?
C70 C69 1.438(3) . ?
C66 C67 1.349(3) . ?
C32 C33 1.343(3) . ?
C19 C18 1.404(3) . ?
C43 C45 1.494(6) . ?
C43 C44 1.593(6) . ?
C43 C3 1.466(8) . ?
C43 C3A 1.531(7) . ?
C43 C44A 1.445(6) . ?
C43 C45A 1.608(5) . ?
C28 C27 1.349(3) . ?
C26 C27 1.406(3) . ?
C76 C75 1.418(3) . ?
C75 C74 1.334(3) . ?
C69 C68 1.353(3) . ?
C67 C68 1.398(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 O3 C4 119.16(10) . . ?
C63 O50 C51 119.30(10) . . ?
C87 C86 C62 120.08(11) . . ?
C87 C86 C85 120.27(11) . . ?
C85 C86 C62 119.62(11) . . ?
O3 C2 C11 122.72(12) . . ?
O3 C2 C1 114.64(11) . . ?
C11 C2 C1 122.64(12) . . ?
C63 C58 C59 117.01(12) . . ?
C63 C58 C57 121.53(12) . . ?
C59 C58 C57 121.41(11) . . ?
C2 C11 C12 116.91(12) . . ?
C2 C11 C10 122.30(12) . . ?
C12 C11 C10 120.78(12) . . ?
C24 C15 C1 120.38(12) . . ?
C24 C15 C16 119.54(13) . . ?
C16 C15 C1 120.06(12) . . ?
O50 C51 C56 123.14(12) . . ?
O50 C51 C52 114.14(11) . . ?
C56 C51 C52 122.71(12) . . ?
O50 C63 C58 123.32(11) . . ?
O50 C63 C62 114.38(11) . . ?
C58 C63 C62 122.30(12) . . ?
C63 C62 C86 120.38(11) . . ?
C61 C62 C86 121.32(11) . . ?
C61 C62 C63 118.29(11) . . ?
C38 C37 C5 119.69(12) . . ?
C36 C37 C38 120.12(13) . . ?
C36 C37 C5 120.17(12) . . ?
C86 C87 C78 119.68(12) . . ?
C86 C87 C91 122.99(12) . . ?
C91 C87 C78 117.33(12) . . ?
C59 C60 C61 117.04(12) . . ?
C59 C60 C92 121.43(12) . . ?
C61 C60 C92 121.52(12) . . ?
O3 C4 C5 114.10(11) . . ?
O3 C4 C9 123.59(12) . . ?
C9 C4 C5 122.31(12) . . ?
C86 C85 C84 122.84(12) . . ?
C86 C85 C80 119.58(12) . . ?
C84 C85 C80 117.57(12) . . ?
C2 C1 C15 120.20(11) . . ?
C14 C1 C2 117.46(12) . . ?
C14 C1 C15 122.33(12) . . ?
C58 C59 C60 123.29(12) . . ?
C37 C38 C29 119.75(12) . . ?
C37 C38 C42 122.64(13) . . ?
C29 C38 C42 117.61(12) . . ?
C51 C56 C57 121.77(12) . . ?
C51 C56 C55 116.51(13) . . ?
C55 C56 C57 121.67(12) . . ?
C37 C36 C35 122.94(14) . . ?
C37 C36 C31 119.52(12) . . ?
C35 C36 C31 117.50(13) . . ?
C51 C52 C64 118.33(12) . . ?
C53 C52 C51 117.97(13) . . ?
C53 C52 C64 123.70(13) . . ?
C62 C61 C60 122.06(12) . . ?
C38 C29 C39 118.83(13) . . ?
C30 C29 C38 119.43(13) . . ?
C30 C29 C39 121.73(14) . . ?
C15 C24 C23 120.09(13) . . ?
C15 C24 C25 122.63(13) . . ?
C25 C24 C23 117.29(13) . . ?
C4 C5 C37 119.74(12) . . ?
C6 C5 C37 122.22(12) . . ?
C6 C5 C4 118.03(13) . . ?
C4 C9 C10 121.52(12) . . ?
C4 C9 C8 117.13(13) . . ?
C8 C9 C10 121.34(13) . . ?
C52 C53 C54 122.11(13) . . ?
C15 C16 C21 119.77(13) . . ?
C15 C16 C17 122.87(14) . . ?
C17 C16 C21 117.34(13) . . ?
C93 C92 C60 113.59(16) . . ?
C93 C92 C94 108.2(3) . . ?
C93 C92 C95 106.9(3) . . ?
C94 C92 C60 109.70(17) . . ?
C94 C92 C95 109.4(3) . . ?
C95 C92 C60 108.89(18) . . ?
C95A C92 C60 113.2(2) . . ?
C95A C92 C93A 108.3(4) . . ?
C95A C92 C94A 110.1(4) . . ?
C93A C92 C60 109.0(2) . . ?
C93A C92 C94A 107.6(5) . . ?
C94A C92 C60 108.4(2) . . ?
C83 C84 C85 121.40(14) . . ?
C13 C12 C11 123.34(13) . . ?
C1 C14 C13 122.50(13) . . ?
C12 C13 C14 117.14(13) . . ?
C12 C13 C46 121.90(13) . . ?
C14 C13 C46 120.95(14) . . ?
C58 C57 C99 108.11(12) . . ?
C56 C57 C58 110.18(10) . . ?
C56 C57 C99 108.07(13) . . ?
C56 C57 C100 110.46(12) . . ?
C100 C57 C58 109.81(13) . . ?
C100 C57 C99 110.16(15) . . ?
C22 C21 C16 119.42(13) . . ?
C22 C21 C20 121.80(15) . . ?
C20 C21 C16 118.78(15) . . ?
C11 C10 C9 110.63(11) . . ?
C11 C10 C49 108.53(14) . . ?
C11 C10 C48 109.58(13) . . ?
C9 C10 C49 109.49(13) . . ?
C9 C10 C48 108.24(14) . . ?
C49 C10 C48 110.36(17) . . ?
C73 C64 C52 120.49(13) . . ?
C73 C64 C65 120.95(14) . . ?
C65 C64 C52 118.35(13) . . ?
C79 C78 C87 119.13(13) . . ?
C79 C78 C88 122.15(14) . . ?
C88 C78 C87 118.71(13) . . ?
C79 C80 C85 119.26(13) . . ?
C79 C80 C81 122.01(14) . . ?
C81 C80 C85 118.73(14) . . ?
C22 C23 C24 119.30(13) . . ?
C22 C23 C28 121.94(15) . . ?
C28 C23 C24 118.76(15) . . ?
C7 C8 C9 123.28(14) . . ?
C5 C6 C7 122.27(14) . . ?
C64 C73 C72 118.92(15) . . ?
C64 C73 C77 123.26(15) . . ?
C77 C73 C72 117.80(15) . . ?
C53 C54 C96 120.01(14) . . ?
C55 C54 C53 117.16(13) . . ?
C55 C54 C96 122.78(14) . . ?
C80 C79 C78 122.02(13) . . ?
C40 C39 C29 121.22(15) . . ?
C90 C91 C87 121.56(14) . . ?
C41 C42 C38 121.20(15) . . ?
C54 C55 C56 123.54(13) . . ?
C8 C7 C6 116.96(13) . . ?
C8 C7 C43 121.22(16) . . ?
C6 C7 C43 121.82(15) . . ?
C34 C35 C36 121.11(16) . . ?
C21 C22 C23 121.86(14) . . ?
C30 C31 C36 119.29(13) . . ?
C30 C31 C32 122.04(15) . . ?
C32 C31 C36 118.66(14) . . ?
C64 C65 C70 119.80(16) . . ?
C64 C65 C66 122.60(15) . . ?
C70 C65 C66 117.58(16) . . ?
C29 C30 C31 121.78(14) . . ?
C13 C46 C1A 113.6(3) . . ?
C47 C46 C13 111.30(18) . . ?
C102 C46 C13 109.44(16) . . ?
C102 C46 C47 109.5(3) . . ?
C102 C46 C101 109.4(3) . . ?
C101 C46 C13 108.29(17) . . ?
C101 C46 C47 108.9(3) . . ?
C47A C46 C13 110.2(3) . . ?
C47A C46 C103 109.2(6) . . ?
C47A C46 C1A 108.0(6) . . ?
C103 C46 C13 110.3(3) . . ?
C103 C46 C1A 105.5(6) . . ?
C26 C25 C24 121.87(17) . . ?
C39 C40 C41 120.02(14) . . ?
C84 C83 C82 120.77(15) . . ?
C82 C81 C80 121.45(15) . . ?
C91 C90 C89 120.64(15) . . ?
C18 C17 C16 121.19(18) . . ?
C98 C96 C54 111.96(14) . . ?
C97 C96 C54 107.88(15) . . ?
C97 C96 C98 107.52(19) . . ?
C50 C96 C54 111.13(16) . . ?
C50 C96 C98 107.43(19) . . ?
C50 C96 C97 110.9(2) . . ?
C71 C72 C73 118.72(16) . . ?
C71 C72 C74 122.65(19) . . ?
C74 C72 C73 118.62(19) . . ?
C76 C77 C73 121.03(19) . . ?
C89 C88 C78 121.61(15) . . ?
C19 C20 C21 121.60(17) . . ?
C42 C41 C40 121.12(15) . . ?
C81 C82 C83 120.10(14) . . ?
C35 C34 C33 120.88(16) . . ?
C65 C70 C69 118.48(19) . . ?
C71 C70 C65 118.63(16) . . ?
C71 C70 C69 122.88(19) . . ?
C88 C89 C90 120.10(15) . . ?
C67 C66 C65 121.9(2) . . ?
C33 C32 C31 121.63(18) . . ?
C20 C19 C18 120.03(16) . . ?
C32 C33 C34 120.08(16) . . ?
C17 C18 C19 121.04(18) . . ?
C7 C43 C44 107.7(2) . . ?
C7 C43 C45A 106.0(2) . . ?
C45 C43 C7 109.1(3) . . ?
C45 C43 C44 103.9(5) . . ?
C3 C43 C7 115.3(4) . . ?
C3 C43 C45 117.9(6) . . ?
C3 C43 C44 101.5(6) . . ?
C3A C43 C7 108.1(3) . . ?
C3A C43 C45A 99.7(4) . . ?
C44A C43 C7 115.3(3) . . ?
C44A C43 C3A 118.1(7) . . ?
C44A C43 C45A 107.9(5) . . ?
C27 C28 C23 121.28(18) . . ?
C25 C26 C27 120.58(18) . . ?
C77 C76 C75 120.4(2) . . ?
C70 C71 C72 122.86(17) . . ?
C28 C27 C26 120.21(17) . . ?
C74 C75 C76 120.49(19) . . ?
C75 C74 C72 121.6(2) . . ?
C68 C69 C70 120.8(2) . . ?
C66 C67 C68 120.5(2) . . ?
C69 C68 C67 120.7(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.817
_oxdiff_exptl_absorpt_empirical_full_min 0.464
####################################################################### 
# 
# 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_mo_210907h_0m
_database_code_depnum_ccdc_archive 'CCDC 2180328'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2022-06-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2022-06-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H34 O'
_chemical_formula_sum            'C29 H34 O'
_chemical_formula_weight         398.56
_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 0.0033 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'

_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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.2535(18)
_cell_length_b                   14.900(3)
_cell_length_c                   17.885(4)
_cell_angle_alpha                90
_cell_angle_beta                 101.861(4)
_cell_angle_gamma                90
_cell_volume                     2413.2(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3514
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6319
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1031 before and 0.0592 after correction.
The Ratio of minimum to maximum transmission is 0.8474.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16876
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.795
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2606
_reflns_number_total             4243
_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 V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4243
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0567
_refine_ls_restrained_S_all      1.042
_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)+(0.0913P)²+0.3454P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1763
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1-C2 \\sim C1A-C2
 with sigma of 0.02
 C2-C28 \\sim C2-C28A
 with sigma of 0.02
 C2-C29 \\sim C2-C29A
 with sigma of 0.02
 C19-C22 \\sim C19-C22A
 with sigma of 0.02
 C19-C20 \\sim C19-C20A
 with sigma of 0.02
 C19-C21 \\sim C19-C21A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C28A) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C29) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C22A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C20A) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(C21A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(1)
 Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(2)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C23(H23),
 C24(H24), C25(H25)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C28A(H28D,H28E,H28F), C29A(H29D,H29E,H29F), C1A(H1AA,H1AB,H1AC),
 C20A(H20D,H20E,H20F), C22A(H22D,H22E,H22F), C21A(H21D,H21E,H21F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.74442(17) 0.46461(11) 0.68251(9) 0.0479(5) Uani 1 1 d . . . . .
C1 C 0.7426(6) 0.2051(2) 0.3971(2) 0.0757(15) Uani 0.817(7) 1 d D U P A 1
H1A H 0.742477 0.180007 0.347673 0.114 Uiso 0.817(7) 1 calc R U P A 1
H1B H 0.650848 0.191467 0.411682 0.114 Uiso 0.817(7) 1 calc R U P A 1
H1C H 0.822757 0.180014 0.433870 0.114 Uiso 0.817(7) 1 calc R U P A 1
C2 C 0.7613(3) 0.30630(17) 0.39414(14) 0.0521(7) Uani 1 1 d D . . . .
C3 C 0.7583(3) 0.34678(15) 0.47271(13) 0.0401(6) Uani 1 1 d . . . . .
C4 C 0.6375(3) 0.33392(15) 0.50606(13) 0.0407(6) Uani 1 1 d . . . . .
H4 H 0.560113 0.298842 0.480123 0.049 Uiso 1 1 calc R U . . .
C5 C 0.6249(2) 0.37062(14) 0.57662(12) 0.0351(5) Uani 1 1 d . . . . .
C6 C 0.7414(2) 0.42276(15) 0.61337(12) 0.0358(5) Uani 1 1 d . . . . .
C7 C 0.6241(2) 0.45541(15) 0.71681(12) 0.0358(6) Uani 1 1 d . . . . .
C8 C 0.6344(2) 0.50297(14) 0.78515(12) 0.0365(6) Uani 1 1 d . . . . .
C9 C 0.7608(3) 0.56214(15) 0.81828(13) 0.0394(6) Uani 1 1 d . . . . .
C10 C 0.8200(3) 0.55789(18) 0.89656(14) 0.0521(7) Uani 1 1 d . . . . .
H10 H 0.784732 0.515129 0.926222 0.062 Uiso 1 1 calc R U . . .
C11 C 0.9295(3) 0.6159(2) 0.93051(17) 0.0692(9) Uani 1 1 d . . . . .
H11 H 0.966690 0.612376 0.982846 0.083 Uiso 1 1 calc R U . . .
C12 C 0.9842(3) 0.6786(2) 0.88817(19) 0.0702(9) Uani 1 1 d . . . . .
H12 H 1.058403 0.717576 0.911422 0.084 Uiso 1 1 calc R U . . .
C13 C 0.8726(3) 0.39858(16) 0.51305(13) 0.0434(6) Uani 1 1 d . . . . .
H13 H 0.955985 0.408381 0.492679 0.052 Uiso 1 1 calc R U . . .
C14 C 0.8653(3) 0.43591(16) 0.58280(14) 0.0440(6) Uani 1 1 d . . . . .
H14 H 0.943728 0.469887 0.609204 0.053 Uiso 1 1 calc R U . . .
C15 C 0.4891(3) 0.35294(16) 0.61026(13) 0.0403(6) Uani 1 1 d . . . . .
C16 C 0.5038(2) 0.40158(14) 0.68692(13) 0.0373(6) Uani 1 1 d . . . . .
C17 C 0.3922(3) 0.39508(16) 0.72873(13) 0.0437(6) Uani 1 1 d . . . . .
H17 H 0.311161 0.358734 0.709881 0.052 Uiso 1 1 calc R U . . .
C18 C 0.3963(3) 0.44050(16) 0.79744(13) 0.0423(6) Uani 1 1 d . . . . .
C19 C 0.2714(3) 0.42974(19) 0.84140(14) 0.0517(7) Uani 1 1 d D . . . .
C20 C 0.2783(6) 0.3348(3) 0.8751(4) 0.0789(19) Uani 0.870(12) 1 d D U P B 1
H20A H 0.271687 0.291558 0.834775 0.118 Uiso 0.870(12) 1 calc R U P B 1
H20B H 0.197609 0.326439 0.900598 0.118 Uiso 0.870(12) 1 calc R U P B 1
H20C H 0.370007 0.327126 0.911009 0.118 Uiso 0.870(12) 1 calc R U P B 1
C21 C 0.2837(6) 0.4989(4) 0.9064(3) 0.0863(18) Uani 0.870(12) 1 d D U P B 1
H21A H 0.371808 0.487676 0.944130 0.130 Uiso 0.870(12) 1 calc R U P B 1
H21B H 0.199168 0.493921 0.929595 0.130 Uiso 0.870(12) 1 calc R U P B 1
H21C H 0.287695 0.558306 0.886125 0.130 Uiso 0.870(12) 1 calc R U P B 1
C22 C 0.1200(5) 0.4434(5) 0.7887(3) 0.0717(15) Uani 0.870(12) 1 d D U P B 1
H22A H 0.111887 0.504129 0.770356 0.108 Uiso 0.870(12) 1 calc R U P B 1
H22B H 0.043763 0.431839 0.816648 0.108 Uiso 0.870(12) 1 calc R U P B 1
H22C H 0.109587 0.402900 0.746246 0.108 Uiso 0.870(12) 1 calc R U P B 1
C23 C 0.5179(3) 0.49437(16) 0.82319(13) 0.0414(6) Uani 1 1 d . . . . .
H23 H 0.522249 0.526509 0.868170 0.050 Uiso 1 1 calc R U . . .
C24 C 0.9285(3) 0.68377(18) 0.81053(19) 0.0625(8) Uani 1 1 d . . . . .
H24 H 0.964941 0.726554 0.781353 0.075 Uiso 1 1 calc R U . . .
C25 C 0.8185(3) 0.62543(16) 0.77604(15) 0.0498(7) Uani 1 1 d . . . . .
H25 H 0.782800 0.628848 0.723574 0.060 Uiso 1 1 calc R U . . .
C26 C 0.3507(3) 0.3880(2) 0.55490(16) 0.0705(9) Uani 1 1 d . . . . .
H26A H 0.359213 0.451671 0.548598 0.106 Uiso 1 1 calc R U . . .
H26B H 0.264710 0.375362 0.575316 0.106 Uiso 1 1 calc R U . . .
H26C H 0.341927 0.358944 0.506278 0.106 Uiso 1 1 calc R U . . .
C27 C 0.4750(4) 0.25141(19) 0.62244(17) 0.0696(9) Uani 1 1 d . . . . .
H27A H 0.461471 0.221166 0.574099 0.104 Uiso 1 1 calc R U . . .
H27B H 0.391556 0.240018 0.645299 0.104 Uiso 1 1 calc R U . . .
H27C H 0.563093 0.229648 0.655515 0.104 Uiso 1 1 calc R U . . .
C28 C 0.6270(8) 0.3417(4) 0.3363(2) 0.111(3) Uani 0.817(7) 1 d D . P A 1
H28A H 0.634511 0.405667 0.331898 0.167 Uiso 0.817(7) 1 calc R U P A 1
H28B H 0.538173 0.326994 0.353399 0.167 Uiso 0.817(7) 1 calc R U P A 1
H28C H 0.624568 0.314523 0.287343 0.167 Uiso 0.817(7) 1 calc R U P A 1
C29 C 0.9059(8) 0.3240(6) 0.3705(4) 0.149(4) Uani 0.817(7) 1 d D U P A 1
H29A H 0.985454 0.300389 0.408488 0.223 Uiso 0.817(7) 1 calc R U P A 1
H29B H 0.918896 0.387445 0.365532 0.223 Uiso 0.817(7) 1 calc R U P A 1
H29C H 0.905420 0.295283 0.322369 0.223 Uiso 0.817(7) 1 calc R U P A 1
C28A C 0.626(3) 0.253(2) 0.3558(16) 0.133(11) Uani 0.183(7) 1 d D U P A 2
H28D H 0.592897 0.274539 0.304413 0.199 Uiso 0.183(7) 1 calc R U P A 2
H28E H 0.548939 0.261112 0.383778 0.199 Uiso 0.183(7) 1 calc R U P A 2
H28F H 0.651028 0.190853 0.354823 0.199 Uiso 0.183(7) 1 calc R U P A 2
C29A C 0.767(3) 0.3844(10) 0.3397(8) 0.073(7) Uani 0.183(7) 1 d D . P A 2
H29D H 0.860432 0.414083 0.353596 0.109 Uiso 0.183(7) 1 calc R U P A 2
H29E H 0.689086 0.426059 0.342877 0.109 Uiso 0.183(7) 1 calc R U P A 2
H29F H 0.753952 0.362113 0.288405 0.109 Uiso 0.183(7) 1 calc R U P A 2
C1A C 0.893(3) 0.247(2) 0.3972(16) 0.135(11) Uani 0.183(7) 1 d D U P A 2
H1AA H 0.861235 0.189614 0.375417 0.203 Uiso 0.183(7) 1 calc R U P A 2
H1AB H 0.942987 0.239252 0.449376 0.203 Uiso 0.183(7) 1 calc R U P A 2
H1AC H 0.958785 0.274086 0.368733 0.203 Uiso 0.183(7) 1 calc R U P A 2
C20A C 0.340(4) 0.378(3) 0.9164(18) 0.090(12) Uani 0.130(12) 1 d D U P B 2
H20D H 0.391796 0.325650 0.903867 0.135 Uiso 0.130(12) 1 calc R U P B 2
H20E H 0.263456 0.359477 0.941853 0.135 Uiso 0.130(12) 1 calc R U P B 2
H20F H 0.408512 0.416144 0.949550 0.135 Uiso 0.130(12) 1 calc R U P B 2
C22A C 0.130(3) 0.398(4) 0.791(2) 0.094(14) Uani 0.130(12) 1 d D U P B 2
H22D H 0.048212 0.412561 0.813676 0.142 Uiso 0.130(12) 1 calc R U P B 2
H22E H 0.134419 0.333982 0.784216 0.142 Uiso 0.130(12) 1 calc R U P B 2
H22F H 0.117955 0.426601 0.741725 0.142 Uiso 0.130(12) 1 calc R U P B 2
C21A C 0.247(6) 0.5256(19) 0.870(3) 0.128(19) Uani 0.130(12) 1 d D U P B 2
H21D H 0.196387 0.561081 0.827472 0.192 Uiso 0.130(12) 1 calc R U P B 2
H21E H 0.341257 0.552597 0.890338 0.192 Uiso 0.130(12) 1 calc R U P B 2
H21F H 0.189515 0.522813 0.908318 0.192 Uiso 0.130(12) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C6 1.380(3) . ?
O1 C7 1.384(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C2 1.519(4) . ?
C2 C3 1.535(3) . ?
C2 C28 1.538(5) . ?
C2 C29 1.507(5) . ?
C2 C28A 1.519(17) . ?
C2 C29A 1.524(13) . ?
C2 C1A 1.496(16) . ?
C3 C4 1.384(3) . ?
C3 C13 1.386(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.402(3) . ?
C5 C6 1.381(3) . ?
C5 C15 1.524(3) . ?
C6 C14 1.382(3) . ?
C7 C8 1.399(3) . ?
C7 C16 1.387(3) . ?
C8 C9 1.487(3) . ?
C8 C23 1.393(3) . ?
C9 C10 1.396(3) . ?
C9 C25 1.382(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.375(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.363(4) . ?
C12 H12 0.9300 . ?
C12 C24 1.380(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.380(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.532(3) . ?
C15 C26 1.540(4) . ?
C15 C27 1.538(4) . ?
C16 C17 1.397(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.396(3) . ?
C18 C19 1.534(3) . ?
C18 C23 1.382(3) . ?
C19 C20 1.533(5) . ?
C19 C21 1.541(5) . ?
C19 C22 1.532(4) . ?
C19 C20A 1.568(17) . ?
C19 C22A 1.507(19) . ?
C19 C21A 1.546(19) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C24 C25 1.383(4) . ?
C25 H25 0.9300 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C28A H28D 0.9600 . ?
C28A H28E 0.9600 . ?
C28A H28F 0.9600 . ?
C29A H29D 0.9600 . ?
C29A H29E 0.9600 . ?
C29A H29F 0.9600 . ?
C1A H1AA 0.9600 . ?
C1A H1AB 0.9600 . ?
C1A H1AC 0.9600 . ?
C20A H20D 0.9600 . ?
C20A H20E 0.9600 . ?
C20A H20F 0.9600 . ?
C22A H22D 0.9600 . ?
C22A H22E 0.9600 . ?
C22A H22F 0.9600 . ?
C21A H21D 0.9600 . ?
C21A H21E 0.9600 . ?
C21A H21F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 O1 C7 118.85(17) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 C3 109.5(2) . . ?
C1 C2 C28 106.4(4) . . ?
C3 C2 C28 108.5(2) . . ?
C29 C2 C1 107.3(4) . . ?
C29 C2 C3 111.9(3) . . ?
C29 C2 C28 113.1(5) . . ?
C28A C2 C3 116.7(9) . . ?
C28A C2 C29A 103.9(17) . . ?
C29A C2 C3 107.1(6) . . ?
C1A C2 C3 111.5(11) . . ?
C1A C2 C28A 107(2) . . ?
C1A C2 C29A 109.9(17) . . ?
C4 C3 C2 120.6(2) . . ?
C4 C3 C13 116.8(2) . . ?
C13 C3 C2 122.7(2) . . ?
C3 C4 H4 118.0 . . ?
C3 C4 C5 123.9(2) . . ?
C5 C4 H4 118.0 . . ?
C4 C5 C15 121.1(2) . . ?
C6 C5 C4 116.5(2) . . ?
C6 C5 C15 122.42(19) . . ?
O1 C6 C5 123.40(19) . . ?
O1 C6 C14 115.2(2) . . ?
C5 C6 C14 121.4(2) . . ?
O1 C7 C8 114.9(2) . . ?
O1 C7 C16 122.80(19) . . ?
C16 C7 C8 122.3(2) . . ?
C7 C8 C9 123.7(2) . . ?
C23 C8 C7 117.3(2) . . ?
C23 C8 C9 118.95(19) . . ?
C10 C9 C8 119.1(2) . . ?
C25 C9 C8 123.2(2) . . ?
C25 C9 C10 117.6(2) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 C9 121.1(3) . . ?
C11 C10 H10 119.5 . . ?
C10 C11 H11 119.7 . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11 119.7 . . ?
C11 C12 H12 120.2 . . ?
C11 C12 C24 119.5(3) . . ?
C24 C12 H12 120.2 . . ?
C3 C13 H13 119.3 . . ?
C14 C13 C3 121.4(2) . . ?
C14 C13 H13 119.3 . . ?
C6 C14 H14 120.0 . . ?
C13 C14 C6 119.9(2) . . ?
C13 C14 H14 120.0 . . ?
C5 C15 C16 110.07(18) . . ?
C5 C15 C26 109.37(19) . . ?
C5 C15 C27 109.1(2) . . ?
C16 C15 C26 108.9(2) . . ?
C16 C15 C27 109.46(19) . . ?
C27 C15 C26 110.0(2) . . ?
C7 C16 C15 122.33(19) . . ?
C7 C16 C17 117.2(2) . . ?
C17 C16 C15 120.5(2) . . ?
C16 C17 H17 118.4 . . ?
C18 C17 C16 123.2(2) . . ?
C18 C17 H17 118.4 . . ?
C17 C18 C19 120.9(2) . . ?
C23 C18 C17 116.6(2) . . ?
C23 C18 C19 122.5(2) . . ?
C18 C19 C21 111.7(3) . . ?
C18 C19 C20A 105.8(12) . . ?
C18 C19 C21A 104.1(18) . . ?
C20 C19 C18 108.8(2) . . ?
C20 C19 C21 109.2(3) . . ?
C22 C19 C18 111.2(3) . . ?
C22 C19 C20 108.9(3) . . ?
C22 C19 C21 106.9(3) . . ?
C22A C19 C18 112.1(16) . . ?
C22A C19 C20A 121(2) . . ?
C22A C19 C21A 109(2) . . ?
C21A C19 C20A 104(2) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C8 C23 H23 118.3 . . ?
C18 C23 C8 123.3(2) . . ?
C18 C23 H23 118.3 . . ?
C12 C24 H24 119.9 . . ?
C12 C24 C25 120.1(3) . . ?
C25 C24 H24 119.9 . . ?
C9 C25 C24 121.1(3) . . ?
C9 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C15 C26 H26A 109.5 . . ?
C15 C26 H26B 109.5 . . ?
C15 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C15 C27 H27A 109.5 . . ?
C15 C27 H27B 109.5 . . ?
C15 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C2 C28 H28A 109.5 . . ?
C2 C28 H28B 109.5 . . ?
C2 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C2 C29 H29A 109.5 . . ?
C2 C29 H29B 109.5 . . ?
C2 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C2 C28A H28D 109.5 . . ?
C2 C28A H28E 109.5 . . ?
C2 C28A H28F 109.5 . . ?
H28D C28A H28E 109.5 . . ?
H28D C28A H28F 109.5 . . ?
H28E C28A H28F 109.5 . . ?
C2 C29A H29D 109.5 . . ?
C2 C29A H29E 109.5 . . ?
C2 C29A H29F 109.5 . . ?
H29D C29A H29E 109.5 . . ?
H29D C29A H29F 109.5 . . ?
H29E C29A H29F 109.5 . . ?
C2 C1A H1AA 109.5 . . ?
C2 C1A H1AB 109.5 . . ?
C2 C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
C19 C20A H20D 109.5 . . ?
C19 C20A H20E 109.5 . . ?
C19 C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C19 C22A H22D 109.5 . . ?
C19 C22A H22E 109.5 . . ?
C19 C22A H22F 109.5 . . ?
H22D C22A H22E 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
C19 C21A H21D 109.5 . . ?
C19 C21A H21E 109.5 . . ?
C19 C21A H21F 109.5 . . ?
H21D C21A H21E 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 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 C6 C14 C13 -178.7(2) . . . . ?
O1 C7 C8 C9 2.2(3) . . . . ?
O1 C7 C8 C23 -178.43(19) . . . . ?
O1 C7 C16 C15 -4.4(3) . . . . ?
O1 C7 C16 C17 177.4(2) . . . . ?
C1 C2 C3 C4 -58.0(4) . . . . ?
C1 C2 C3 C13 123.2(3) . . . . ?
C2 C3 C4 C5 -178.3(2) . . . . ?
C2 C3 C13 C14 178.4(2) . . . . ?
C3 C4 C5 C6 0.4(3) . . . . ?
C3 C4 C5 C15 -179.5(2) . . . . ?
C3 C13 C14 C6 -0.7(4) . . . . ?
C4 C3 C13 C14 -0.5(3) . . . . ?
C4 C5 C6 O1 178.9(2) . . . . ?
C4 C5 C6 C14 -1.6(3) . . . . ?
C4 C5 C15 C16 -179.5(2) . . . . ?
C4 C5 C15 C26 -59.9(3) . . . . ?
C4 C5 C15 C27 60.4(3) . . . . ?
C5 C6 C14 C13 1.8(4) . . . . ?
C5 C15 C16 C7 2.0(3) . . . . ?
C5 C15 C16 C17 -179.9(2) . . . . ?
C6 O1 C7 C8 -177.59(19) . . . . ?
C6 O1 C7 C16 3.9(3) . . . . ?
C6 C5 C15 C16 0.7(3) . . . . ?
C6 C5 C15 C26 120.3(3) . . . . ?
C6 C5 C15 C27 -119.4(2) . . . . ?
C7 O1 C6 C5 -1.0(3) . . . . ?
C7 O1 C6 C14 179.5(2) . . . . ?
C7 C8 C9 C10 -136.3(2) . . . . ?
C7 C8 C9 C25 47.4(3) . . . . ?
C7 C8 C23 C18 1.2(3) . . . . ?
C7 C16 C17 C18 0.7(3) . . . . ?
C8 C7 C16 C15 177.1(2) . . . . ?
C8 C7 C16 C17 -1.1(3) . . . . ?
C8 C9 C10 C11 -175.1(2) . . . . ?
C8 C9 C25 C24 174.8(2) . . . . ?
C9 C8 C23 C18 -179.4(2) . . . . ?
C9 C10 C11 C12 -0.7(4) . . . . ?
C10 C9 C25 C24 -1.5(4) . . . . ?
C10 C11 C12 C24 0.1(5) . . . . ?
C11 C12 C24 C25 -0.3(4) . . . . ?
C12 C24 C25 C9 1.0(4) . . . . ?
C13 C3 C4 C5 0.7(3) . . . . ?
C15 C5 C6 O1 -1.3(3) . . . . ?
C15 C5 C6 C14 178.2(2) . . . . ?
C15 C16 C17 C18 -177.5(2) . . . . ?
C16 C7 C8 C9 -179.2(2) . . . . ?
C16 C7 C8 C23 0.1(3) . . . . ?
C16 C17 C18 C19 -179.2(2) . . . . ?
C16 C17 C18 C23 0.5(3) . . . . ?
C17 C18 C19 C20 70.2(4) . . . . ?
C17 C18 C19 C21 -169.1(4) . . . . ?
C17 C18 C19 C22 -49.7(4) . . . . ?
C17 C18 C19 C20A 112(2) . . . . ?
C17 C18 C19 C22A -22(2) . . . . ?
C17 C18 C19 C21A -139(2) . . . . ?
C17 C18 C23 C8 -1.5(3) . . . . ?
C19 C18 C23 C8 178.1(2) . . . . ?
C23 C8 C9 C10 44.4(3) . . . . ?
C23 C8 C9 C25 -131.9(2) . . . . ?
C23 C18 C19 C20 -109.5(4) . . . . ?
C23 C18 C19 C21 11.3(4) . . . . ?
C23 C18 C19 C22 130.7(4) . . . . ?
C23 C18 C19 C20A -68(2) . . . . ?
C23 C18 C19 C22A 159(2) . . . . ?
C23 C18 C19 C21A 41(3) . . . . ?
C25 C9 C10 C11 1.3(4) . . . . ?
C26 C15 C16 C7 -117.9(3) . . . . ?
C26 C15 C16 C17 60.2(3) . . . . ?
C27 C15 C16 C7 121.9(2) . . . . ?
C27 C15 C16 C17 -60.0(3) . . . . ?
C28 C2 C3 C4 57.7(4) . . . . ?
C28 C2 C3 C13 -121.1(4) . . . . ?
C29 C2 C3 C4 -176.8(5) . . . . ?
C29 C2 C3 C13 4.3(6) . . . . ?
C28A C2 C3 C4 0.6(18) . . . . ?
C28A C2 C3 C13 -178.2(18) . . . . ?
C29A C2 C3 C4 116.5(12) . . . . ?
C29A C2 C3 C13 -62.4(12) . . . . ?
C1A C2 C3 C4 -123.2(19) . . . . ?
C1A C2 C3 C13 57.9(19) . . . . ?


_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_mo_190719c
_database_code_depnum_ccdc_archive 'CCDC 2180349'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2022-06-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2022-06-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C35 H38 O'
_chemical_formula_sum            'C35 H38 O'
_chemical_formula_weight         474.65
_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 0.0033 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'

_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           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.6293(12)
_cell_length_b                   12.4614(17)
_cell_length_c                   26.146(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.519(2)
_cell_angle_gamma                90
_cell_volume                     2802.8(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    293
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      2.26
_shelx_estimated_absorpt_T_max   0.993
_shelx_estimated_absorpt_T_min   0.990
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            20821
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.563
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4484
_reflns_number_total             5698
_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 v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         5698
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0553
_refine_ls_restrained_S_all      1.076
_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)+(0.0539P)²+1.4106P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1499
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C10-C1AA \\sim C10-C21A
 with sigma of 0.02
 C1AA-C34A \\sim C21A-C34
 with sigma of 0.02
 C1AA-C33A \\sim C21A-C33
 with sigma of 0.02
 C1AA-C32A \\sim C21A-C32
 with sigma of 0.02
 C10-C34A \\sim C10-C34
 with sigma of 0.04
 C10-C33A \\sim C10-C33
 with sigma of 0.04
 C10-C32A \\sim C10-C32
 with sigma of 0.04
 C34A-C33A \\sim C34-C33
 with sigma of 0.04
 C34A-C32A \\sim C34-C32
 with sigma of 0.04
 C33A-C32A \\sim C33-C32
 with sigma of 0.04
 C28-C31A \\sim C28-C31
 with sigma of 0.02
 C28-C29A \\sim C28-C29
 with sigma of 0.02
 C28-C30A \\sim C28-C30
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq, Uanis(C30A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C33A) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C32)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C34)=Sof(H34D)=Sof(H34E)=Sof(H34F)=
 Sof(C33)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C21A)=1-FVAR(1)
 Sof(C1AA)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C33A)=Sof(H33A)=
 Sof(H33B)=Sof(H33C)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
 Sof(C29)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C31)=Sof(H31D)=Sof(H31E)=Sof(H31F)=
 Sof(C30)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(2)
 Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C29A)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C3(H3), C11(H11), C5(H5), C15(H15), C21(H21), C19(H19), C16(H16),
 C25(H25), C23(H23), C22(H22), C17(H17), C18(H18), C24(H24)
5.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C31A(H31A,H31B,H31C), C29A(H29A,
 H29B,H29C), C30A(H30A,H30B,H30C), C34A(H34A,H34B,H34C), C33A(H33A,H33B,H33C),
 C32A(H32A,H32B,H32C), C32(H32D,H32E,H32F), C34(H34D,H34E,H34F), C33(H33D,H33E,
 H33F), C29(H29D,H29E,H29F), C31(H31D,H31E,H31F), C30(H30D,H30E,H30F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 -0.00484(12) 0.26510(9) 0.24730(4) 0.0352(3) Uani 1 1 d . . . . .
C13 C -0.08127(17) 0.29488(12) 0.28956(6) 0.0284(3) Uani 1 1 d . . . . .
C6 C -0.20753(18) 0.34783(13) 0.19085(6) 0.0312(3) Uani 1 1 d . . . . .
C8 C -0.21647(17) 0.35533(12) 0.28607(6) 0.0296(3) Uani 1 1 d . . . . .
C1 C -0.07260(17) 0.28713(12) 0.19872(6) 0.0298(3) Uani 1 1 d . . . . .
C12 C -0.01324(18) 0.25938(13) 0.33722(6) 0.0316(3) Uani 1 1 d . . . . .
C7 C -0.28977(17) 0.39584(13) 0.23481(6) 0.0314(3) Uani 1 1 d . . . . .
C9 C -0.28210(19) 0.38275(13) 0.33141(6) 0.0355(4) Uani 1 1 d . . . . .
H9 H -0.372038 0.424153 0.329300 0.043 Uiso 1 1 calc R U . . .
C10 C -0.2190(2) 0.35092(14) 0.37951(6) 0.0378(4) Uani 1 1 d D . . . .
C3 C -0.0583(2) 0.26977(14) 0.10804(6) 0.0387(4) Uani 1 1 d . . . . .
H3 H -0.008694 0.242920 0.080431 0.046 Uiso 1 1 calc R U . . .
C14 C 0.15156(19) 0.18243(13) 0.16381(6) 0.0348(4) Uani 1 1 d . . . . .
C11 C -0.0848(2) 0.28832(14) 0.38099(6) 0.0384(4) Uani 1 1 d . . . . .
H11 H -0.041257 0.264855 0.412690 0.046 Uiso 1 1 calc R U . . .
C2 C 0.00503(18) 0.24713(13) 0.15757(6) 0.0329(3) Uani 1 1 d . . . . .
C4 C -0.1924(2) 0.33073(14) 0.09804(6) 0.0388(4) Uani 1 1 d . . . . .
C5 C -0.26434(19) 0.36820(14) 0.14011(6) 0.0375(4) Uani 1 1 d . . . . .
H5 H -0.354520 0.408746 0.134386 0.045 Uiso 1 1 calc R U . . .
C20 C 0.12937(19) 0.19128(13) 0.34195(6) 0.0342(4) Uani 1 1 d . . . . .
C15 C 0.1754(2) 0.10165(14) 0.20028(7) 0.0422(4) Uani 1 1 d . . . . .
H15 H 0.101890 0.089929 0.223840 0.051 Uiso 1 1 calc R U . . .
C21 C 0.1278(2) 0.09466(15) 0.36796(7) 0.0459(4) Uani 1 1 d . . . . .
H21 H 0.037332 0.072548 0.382008 0.055 Uiso 1 1 calc R U . . .
C28 C -0.2542(2) 0.36003(17) 0.04314(7) 0.0488(5) Uani 1 1 d D . . . .
C27 C -0.46353(19) 0.36490(17) 0.22886(7) 0.0455(4) Uani 1 1 d . . . . .
H27A H -0.510587 0.394134 0.197403 0.068 Uiso 1 1 calc R U . . .
H27B H -0.514781 0.393164 0.257236 0.068 Uiso 1 1 calc R U . . .
H27C H -0.473261 0.288155 0.228256 0.068 Uiso 1 1 calc R U . . .
C1AA C -0.2873(8) 0.3829(6) 0.4303(3) 0.048(3) Uani 0.644(15) 1 d D . P A 1
C26 C -0.2729(2) 0.51927(14) 0.23316(7) 0.0440(4) Uani 1 1 d . . . . .
H26A H -0.164638 0.538004 0.235780 0.066 Uiso 1 1 calc R U . . .
H26B H -0.322090 0.550484 0.261283 0.066 Uiso 1 1 calc R U . . .
H26C H -0.321428 0.545963 0.201380 0.066 Uiso 1 1 calc R U . . .
C19 C 0.2657(2) 0.19894(16) 0.12998(7) 0.0482(5) Uani 1 1 d . . . . .
H19 H 0.253027 0.253323 0.105653 0.058 Uiso 1 1 calc R U . . .
C16 C 0.3078(2) 0.03850(16) 0.20182(8) 0.0515(5) Uani 1 1 d . . . . .
H16 H 0.321949 -0.015535 0.226281 0.062 Uiso 1 1 calc R U . . .
C25 C 0.2667(2) 0.22189(17) 0.32233(8) 0.0528(5) Uani 1 1 d . . . . .
H25 H 0.270728 0.286424 0.304628 0.063 Uiso 1 1 calc R U . . .
C23 C 0.3943(3) 0.06178(18) 0.35371(8) 0.0575(5) Uani 1 1 d . . . . .
H23 H 0.482106 0.018346 0.357371 0.069 Uiso 1 1 calc R U . . .
C22 C 0.2591(3) 0.03036(17) 0.37336(8) 0.0575(5) Uani 1 1 d . . . . .
H22 H 0.255370 -0.034844 0.390520 0.069 Uiso 1 1 calc R U . . .
C17 C 0.4186(2) 0.05480(18) 0.16760(9) 0.0581(6) Uani 1 1 d . . . . .
H17 H 0.506523 0.011514 0.168566 0.070 Uiso 1 1 calc R U . . .
C18 C 0.3981(3) 0.13576(19) 0.13190(9) 0.0611(6) Uani 1 1 d . . . . .
H18 H 0.473325 0.148063 0.109001 0.073 Uiso 1 1 calc R U . . .
C24 C 0.3986(2) 0.1582(2) 0.32855(9) 0.0619(6) Uani 1 1 d . . . . .
H24 H 0.490358 0.180924 0.315592 0.074 Uiso 1 1 calc R U . . .
C31A C -0.1681(7) 0.3090(5) 0.00226(13) 0.081(2) Uani 0.621(7) 1 d D . P B 1
H31A H -0.170942 0.232409 0.005987 0.122 Uiso 0.621(7) 1 calc R U P B 1
H31B H -0.062097 0.333034 0.005280 0.122 Uiso 0.621(7) 1 calc R U P B 1
H31C H -0.215933 0.328729 -0.030799 0.122 Uiso 0.621(7) 1 calc R U P B 1
C29A C -0.2325(5) 0.4861(3) 0.03712(15) 0.0640(13) Uani 0.621(7) 1 d D . P B 1
H29A H -0.266727 0.507222 0.002764 0.096 Uiso 0.621(7) 1 calc R U P B 1
H29B H -0.124692 0.504198 0.043996 0.096 Uiso 0.621(7) 1 calc R U P B 1
H29C H -0.292838 0.522901 0.060954 0.096 Uiso 0.621(7) 1 calc R U P B 1
C30A C -0.4271(6) 0.3397(5) 0.0357(3) 0.0723(17) Uani 0.621(7) 1 d D U P B 1
H30A H -0.478535 0.377949 0.061352 0.108 Uiso 0.621(7) 1 calc R U P B 1
H30B H -0.446820 0.264274 0.038706 0.108 Uiso 0.621(7) 1 calc R U P B 1
H30C H -0.465716 0.364070 0.002241 0.108 Uiso 0.621(7) 1 calc R U P B 1
C34A C -0.3174(10) 0.2822(6) 0.4603(3) 0.084(2) Uani 0.644(15) 1 d D . P A 1
H34A H -0.393729 0.239044 0.441128 0.126 Uiso 0.644(15) 1 calc R U P A 1
H34B H -0.355024 0.301357 0.492641 0.126 Uiso 0.644(15) 1 calc R U P A 1
H34C H -0.222543 0.242197 0.466085 0.126 Uiso 0.644(15) 1 calc R U P A 1
C33A C -0.4384(10) 0.4448(8) 0.4209(3) 0.088(3) Uani 0.644(15) 1 d D U P A 1
H33A H -0.418298 0.512238 0.404932 0.132 Uiso 0.644(15) 1 calc R U P A 1
H33B H -0.482119 0.457528 0.453014 0.132 Uiso 0.644(15) 1 calc R U P A 1
H33C H -0.510277 0.403914 0.398838 0.132 Uiso 0.644(15) 1 calc R U P A 1
C32A C -0.1659(8) 0.4506(8) 0.4611(3) 0.090(3) Uani 0.644(15) 1 d D . P A 1
H32A H -0.071231 0.410426 0.466770 0.135 Uiso 0.644(15) 1 calc R U P A 1
H32B H -0.203591 0.469304 0.493513 0.135 Uiso 0.644(15) 1 calc R U P A 1
H32C H -0.146476 0.514877 0.442365 0.135 Uiso 0.644(15) 1 calc R U P A 1
C32 C -0.241(3) 0.5072(10) 0.4387(6) 0.106(6) Uani 0.356(15) 1 d D . P A 2
H32D H -0.278336 0.553681 0.411240 0.160 Uiso 0.356(15) 1 calc R U P A 2
H32E H -0.129057 0.510141 0.442546 0.160 Uiso 0.356(15) 1 calc R U P A 2
H32F H -0.281502 0.530026 0.470038 0.160 Uiso 0.356(15) 1 calc R U P A 2
C34 C -0.251(2) 0.3235(16) 0.4743(4) 0.109(7) Uani 0.356(15) 1 d D . P A 2
H34D H -0.141985 0.330961 0.484333 0.164 Uiso 0.356(15) 1 calc R U P A 2
H34E H -0.274187 0.249516 0.466886 0.164 Uiso 0.356(15) 1 calc R U P A 2
H34F H -0.310093 0.347343 0.501751 0.164 Uiso 0.356(15) 1 calc R U P A 2
C33 C -0.4710(14) 0.3910(18) 0.4184(5) 0.100(5) Uani 0.356(15) 1 d D U P A 2
H33D H -0.514371 0.402157 0.450687 0.150 Uiso 0.356(15) 1 calc R U P A 2
H33E H -0.505627 0.323168 0.404336 0.150 Uiso 0.356(15) 1 calc R U P A 2
H33F H -0.504540 0.447457 0.395099 0.150 Uiso 0.356(15) 1 calc R U P A 2
C21A C -0.2930(16) 0.3914(11) 0.4265(5) 0.054(5) Uani 0.356(15) 1 d D . P A 2
C29 C -0.1336(12) 0.4275(8) 0.0207(3) 0.094(4) Uani 0.379(7) 1 d D . P B 2
H29D H -0.159835 0.436337 -0.015401 0.141 Uiso 0.379(7) 1 calc R U P B 2
H29E H -0.034168 0.392984 0.026059 0.141 Uiso 0.379(7) 1 calc R U P B 2
H29F H -0.129264 0.496495 0.037084 0.141 Uiso 0.379(7) 1 calc R U P B 2
C31 C -0.2591(10) 0.2493(7) 0.0097(3) 0.070(2) Uani 0.379(7) 1 d D . P B 2
H31D H -0.338527 0.202976 0.020923 0.104 Uiso 0.379(7) 1 calc R U P B 2
H31E H -0.160200 0.213982 0.014378 0.104 Uiso 0.379(7) 1 calc R U P B 2
H31F H -0.281609 0.265952 -0.026007 0.104 Uiso 0.379(7) 1 calc R U P B 2
C30 C -0.4142(13) 0.4000(12) 0.0377(5) 0.109(5) Uani 0.379(7) 1 d D U P B 2
H30D H -0.449058 0.403903 0.001928 0.163 Uiso 0.379(7) 1 calc R U P B 2
H30E H -0.418181 0.470091 0.052699 0.163 Uiso 0.379(7) 1 calc R U P B 2
H30F H -0.480255 0.352066 0.054777 0.163 Uiso 0.379(7) 1 calc R U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C13 1.3816(18) . ?
O1 C1 1.3833(17) . ?
C13 C8 1.386(2) . ?
C13 C12 1.406(2) . ?
C6 C1 1.390(2) . ?
C6 C7 1.520(2) . ?
C6 C5 1.401(2) . ?
C8 C7 1.522(2) . ?
C8 C9 1.396(2) . ?
C1 C2 1.403(2) . ?
C12 C11 1.390(2) . ?
C12 C20 1.492(2) . ?
C7 C27 1.544(2) . ?
C7 C26 1.546(2) . ?
C9 H9 0.9300 . ?
C9 C10 1.388(2) . ?
C10 C11 1.394(2) . ?
C10 C1AA 1.548(5) . ?
C10 C21A 1.515(12) . ?
C3 H3 0.9300 . ?
C3 C2 1.394(2) . ?
C3 C4 1.391(2) . ?
C14 C2 1.498(2) . ?
C14 C15 1.391(2) . ?
C14 C19 1.390(2) . ?
C11 H11 0.9300 . ?
C4 C5 1.386(2) . ?
C4 C28 1.536(2) . ?
C5 H5 0.9300 . ?
C20 C21 1.383(2) . ?
C20 C25 1.381(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.385(2) . ?
C21 H21 0.9300 . ?
C21 C22 1.387(3) . ?
C28 C31A 1.491(4) . ?
C28 C29A 1.591(4) . ?
C28 C30A 1.511(6) . ?
C28 C29 1.493(8) . ?
C28 C31 1.632(7) . ?
C28 C30 1.464(9) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C1AA C34A 1.512(9) . ?
C1AA C33A 1.519(7) . ?
C1AA C32A 1.524(8) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C19 H19 0.9300 . ?
C19 C18 1.385(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.375(3) . ?
C25 H25 0.9300 . ?
C25 C24 1.387(3) . ?
C23 H23 0.9300 . ?
C23 C22 1.368(3) . ?
C23 C24 1.371(3) . ?
C22 H22 0.9300 . ?
C17 H17 0.9300 . ?
C17 C18 1.376(3) . ?
C18 H18 0.9300 . ?
C24 H24 0.9300 . ?
C31A H31A 0.9600 . ?
C31A H31B 0.9600 . ?
C31A H31C 0.9600 . ?
C29A H29A 0.9600 . ?
C29A H29B 0.9600 . ?
C29A H29C 0.9600 . ?
C30A H30A 0.9600 . ?
C30A H30B 0.9600 . ?
C30A H30C 0.9600 . ?
C34A H34A 0.9600 . ?
C34A H34B 0.9600 . ?
C34A H34C 0.9600 . ?
C33A H33A 0.9600 . ?
C33A H33B 0.9600 . ?
C33A H33C 0.9600 . ?
C32A H32A 0.9600 . ?
C32A H32B 0.9600 . ?
C32A H32C 0.9600 . ?
C32 H32D 0.9600 . ?
C32 H32E 0.9600 . ?
C32 H32F 0.9600 . ?
C32 C21A 1.538(13) . ?
C34 H34D 0.9600 . ?
C34 H34E 0.9600 . ?
C34 H34F 0.9600 . ?
C34 C21A 1.530(13) . ?
C33 H33D 0.9600 . ?
C33 H33E 0.9600 . ?
C33 H33F 0.9600 . ?
C33 C21A 1.535(13) . ?
C29 H29D 0.9600 . ?
C29 H29E 0.9600 . ?
C29 H29F 0.9600 . ?
C31 H31D 0.9600 . ?
C31 H31E 0.9600 . ?
C31 H31F 0.9600 . ?
C30 H30D 0.9600 . ?
C30 H30E 0.9600 . ?
C30 H30F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 O1 C1 119.16(12) . . ?
O1 C13 C8 123.09(13) . . ?
O1 C13 C12 115.59(13) . . ?
C8 C13 C12 121.32(14) . . ?
C1 C6 C7 122.52(13) . . ?
C1 C6 C5 117.73(14) . . ?
C5 C6 C7 119.69(14) . . ?
C13 C8 C7 121.83(13) . . ?
C13 C8 C9 118.23(14) . . ?
C9 C8 C7 119.88(14) . . ?
O1 C1 C6 122.17(13) . . ?
O1 C1 C2 116.15(13) . . ?
C6 C1 C2 121.66(14) . . ?
C13 C12 C20 122.44(14) . . ?
C11 C12 C13 117.78(14) . . ?
C11 C12 C20 119.77(14) . . ?
C6 C7 C8 110.42(12) . . ?
C6 C7 C27 109.45(13) . . ?
C6 C7 C26 108.64(13) . . ?
C8 C7 C27 109.80(13) . . ?
C8 C7 C26 108.72(13) . . ?
C27 C7 C26 109.79(14) . . ?
C8 C9 H9 118.6 . . ?
C10 C9 C8 122.88(15) . . ?
C10 C9 H9 118.6 . . ?
C9 C10 C11 116.77(15) . . ?
C9 C10 C1AA 123.8(3) . . ?
C9 C10 C21A 118.6(6) . . ?
C11 C10 C1AA 119.5(3) . . ?
C11 C10 C21A 124.5(6) . . ?
C2 C3 H3 118.5 . . ?
C4 C3 H3 118.5 . . ?
C4 C3 C2 122.97(15) . . ?
C15 C14 C2 122.85(15) . . ?
C19 C14 C2 119.05(15) . . ?
C19 C14 C15 117.99(15) . . ?
C12 C11 C10 122.98(15) . . ?
C12 C11 H11 118.5 . . ?
C10 C11 H11 118.5 . . ?
C1 C2 C14 123.91(14) . . ?
C3 C2 C1 117.67(14) . . ?
C3 C2 C14 118.42(14) . . ?
C3 C4 C28 121.86(15) . . ?
C5 C4 C3 116.92(15) . . ?
C5 C4 C28 121.16(15) . . ?
C6 C5 H5 118.5 . . ?
C4 C5 C6 123.03(15) . . ?
C4 C5 H5 118.5 . . ?
C21 C20 C12 119.71(15) . . ?
C25 C20 C12 122.56(15) . . ?
C25 C20 C21 117.71(16) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.55(17) . . ?
C16 C15 H15 119.7 . . ?
C20 C21 H21 119.6 . . ?
C20 C21 C22 120.88(19) . . ?
C22 C21 H21 119.6 . . ?
C4 C28 C29A 106.99(19) . . ?
C4 C28 C31 107.0(3) . . ?
C31A C28 C4 114.4(2) . . ?
C31A C28 C29A 106.3(3) . . ?
C31A C28 C30A 112.2(4) . . ?
C30A C28 C4 110.3(3) . . ?
C30A C28 C29A 106.0(3) . . ?
C29 C28 C4 107.4(3) . . ?
C29 C28 C31 104.8(5) . . ?
C30 C28 C4 115.3(5) . . ?
C30 C28 C29 116.8(7) . . ?
C30 C28 C31 104.5(6) . . ?
C7 C27 H27A 109.5 . . ?
C7 C27 H27B 109.5 . . ?
C7 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C34A C1AA C10 108.9(5) . . ?
C34A C1AA C33A 109.0(6) . . ?
C34A C1AA C32A 109.0(6) . . ?
C33A C1AA C10 111.8(6) . . ?
C33A C1AA C32A 110.4(6) . . ?
C32A C1AA C10 107.6(4) . . ?
C7 C26 H26A 109.5 . . ?
C7 C26 H26B 109.5 . . ?
C7 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C14 C19 H19 119.4 . . ?
C18 C19 C14 121.10(18) . . ?
C18 C19 H19 119.4 . . ?
C15 C16 H16 119.6 . . ?
C17 C16 C15 120.74(18) . . ?
C17 C16 H16 119.6 . . ?
C20 C25 H25 119.4 . . ?
C20 C25 C24 121.23(19) . . ?
C24 C25 H25 119.4 . . ?
C22 C23 H23 120.4 . . ?
C22 C23 C24 119.12(19) . . ?
C24 C23 H23 120.4 . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.72(19) . . ?
C23 C22 H22 119.6 . . ?
C16 C17 H17 120.3 . . ?
C16 C17 C18 119.41(18) . . ?
C18 C17 H17 120.3 . . ?
C19 C18 H18 119.9 . . ?
C17 C18 C19 120.18(19) . . ?
C17 C18 H18 119.9 . . ?
C25 C24 H24 119.8 . . ?
C23 C24 C25 120.3(2) . . ?
C23 C24 H24 119.8 . . ?
C28 C31A H31A 109.5 . . ?
C28 C31A H31B 109.5 . . ?
C28 C31A H31C 109.5 . . ?
H31A C31A H31B 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
C28 C29A H29A 109.5 . . ?
C28 C29A H29B 109.5 . . ?
C28 C29A H29C 109.5 . . ?
H29A C29A H29B 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
C28 C30A H30A 109.5 . . ?
C28 C30A H30B 109.5 . . ?
C28 C30A H30C 109.5 . . ?
H30A C30A H30B 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
C1AA C34A H34A 109.5 . . ?
C1AA C34A H34B 109.5 . . ?
C1AA C34A H34C 109.5 . . ?
H34A C34A H34B 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C1AA C33A H33A 109.5 . . ?
C1AA C33A H33B 109.5 . . ?
C1AA C33A H33C 109.5 . . ?
H33A C33A H33B 109.5 . . ?
H33A C33A H33C 109.5 . . ?
H33B C33A H33C 109.5 . . ?
C1AA C32A H32A 109.5 . . ?
C1AA C32A H32B 109.5 . . ?
C1AA C32A H32C 109.5 . . ?
H32A C32A H32B 109.5 . . ?
H32A C32A H32C 109.5 . . ?
H32B C32A H32C 109.5 . . ?
H32D C32 H32E 109.5 . . ?
H32D C32 H32F 109.5 . . ?
H32E C32 H32F 109.5 . . ?
C21A C32 H32D 109.5 . . ?
C21A C32 H32E 109.5 . . ?
C21A C32 H32F 109.5 . . ?
H34D C34 H34E 109.5 . . ?
H34D C34 H34F 109.5 . . ?
H34E C34 H34F 109.5 . . ?
C21A C34 H34D 109.5 . . ?
C21A C34 H34E 109.5 . . ?
C21A C34 H34F 109.5 . . ?
H33D C33 H33E 109.5 . . ?
H33D C33 H33F 109.5 . . ?
H33E C33 H33F 109.5 . . ?
C21A C33 H33D 109.5 . . ?
C21A C33 H33E 109.5 . . ?
C21A C33 H33F 109.5 . . ?
C10 C21A C32 110.2(8) . . ?
C10 C21A C34 113.0(10) . . ?
C10 C21A C33 111.6(9) . . ?
C34 C21A C32 107.6(11) . . ?
C34 C21A C33 106.4(11) . . ?
C33 C21A C32 107.9(11) . . ?
C28 C29 H29D 109.5 . . ?
C28 C29 H29E 109.5 . . ?
C28 C29 H29F 109.5 . . ?
H29D C29 H29E 109.5 . . ?
H29D C29 H29F 109.5 . . ?
H29E C29 H29F 109.5 . . ?
C28 C31 H31D 109.5 . . ?
C28 C31 H31E 109.5 . . ?
C28 C31 H31F 109.5 . . ?
H31D C31 H31E 109.5 . . ?
H31D C31 H31F 109.5 . . ?
H31E C31 H31F 109.5 . . ?
C28 C30 H30D 109.5 . . ?
C28 C30 H30E 109.5 . . ?
C28 C30 H30F 109.5 . . ?
H30D C30 H30E 109.5 . . ?
H30D C30 H30F 109.5 . . ?
H30E C30 H30F 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 C13 C8 C7 -1.3(2) . . . . ?
O1 C13 C8 C9 -178.66(14) . . . . ?
O1 C13 C12 C11 179.28(14) . . . . ?
O1 C13 C12 C20 -1.8(2) . . . . ?
O1 C1 C2 C3 -178.69(14) . . . . ?
O1 C1 C2 C14 1.0(2) . . . . ?
C13 O1 C1 C6 6.6(2) . . . . ?
C13 O1 C1 C2 -175.04(13) . . . . ?
C13 C8 C7 C6 7.8(2) . . . . ?
C13 C8 C7 C27 128.54(16) . . . . ?
C13 C8 C7 C26 -111.33(17) . . . . ?
C13 C8 C9 C10 -0.9(2) . . . . ?
C13 C12 C11 C10 -0.4(3) . . . . ?
C13 C12 C20 C21 -125.33(17) . . . . ?
C13 C12 C20 C25 56.4(2) . . . . ?
C6 C1 C2 C3 -0.3(2) . . . . ?
C6 C1 C2 C14 179.30(15) . . . . ?
C8 C13 C12 C11 -1.0(2) . . . . ?
C8 C13 C12 C20 177.99(14) . . . . ?
C8 C9 C10 C11 -0.4(3) . . . . ?
C8 C9 C10 C1AA 178.3(4) . . . . ?
C8 C9 C10 C21A 175.8(6) . . . . ?
C1 O1 C13 C8 -6.4(2) . . . . ?
C1 O1 C13 C12 173.34(13) . . . . ?
C1 C6 C7 C8 -7.6(2) . . . . ?
C1 C6 C7 C27 -128.55(16) . . . . ?
C1 C6 C7 C26 111.58(17) . . . . ?
C1 C6 C5 C4 0.0(3) . . . . ?
C12 C13 C8 C7 178.95(14) . . . . ?
C12 C13 C8 C9 1.6(2) . . . . ?
C12 C20 C21 C22 -179.35(17) . . . . ?
C12 C20 C25 C24 178.23(19) . . . . ?
C7 C6 C1 O1 0.8(2) . . . . ?
C7 C6 C1 C2 -177.40(15) . . . . ?
C7 C6 C5 C4 177.45(16) . . . . ?
C7 C8 C9 C10 -178.29(15) . . . . ?
C9 C8 C7 C6 -174.92(14) . . . . ?
C9 C8 C7 C27 -54.1(2) . . . . ?
C9 C8 C7 C26 65.98(19) . . . . ?
C9 C10 C11 C12 1.1(3) . . . . ?
C9 C10 C1AA C34A 125.3(6) . . . . ?
C9 C10 C1AA C33A 4.8(8) . . . . ?
C9 C10 C1AA C32A -116.6(6) . . . . ?
C9 C10 C21A C32 -79.0(13) . . . . ?
C9 C10 C21A C34 160.6(12) . . . . ?
C9 C10 C21A C33 40.8(14) . . . . ?
C3 C4 C5 C6 0.4(3) . . . . ?
C3 C4 C28 C31A 5.7(4) . . . . ?
C3 C4 C28 C29A -111.7(3) . . . . ?
C3 C4 C28 C30A 133.4(3) . . . . ?
C3 C4 C28 C29 -62.7(5) . . . . ?
C3 C4 C28 C31 49.4(4) . . . . ?
C3 C4 C28 C30 165.1(7) . . . . ?
C14 C15 C16 C17 0.4(3) . . . . ?
C14 C19 C18 C17 0.1(3) . . . . ?
C11 C12 C20 C21 53.6(2) . . . . ?
C11 C12 C20 C25 -124.71(19) . . . . ?
C11 C10 C1AA C34A -55.9(7) . . . . ?
C11 C10 C1AA C33A -176.4(6) . . . . ?
C11 C10 C1AA C32A 62.1(7) . . . . ?
C11 C10 C21A C32 97.0(13) . . . . ?
C11 C10 C21A C34 -23.4(15) . . . . ?
C11 C10 C21A C33 -143.2(12) . . . . ?
C2 C3 C4 C5 -0.9(3) . . . . ?
C2 C3 C4 C28 176.32(17) . . . . ?
C2 C14 C15 C16 174.87(17) . . . . ?
C2 C14 C19 C18 -175.28(19) . . . . ?
C4 C3 C2 C1 0.8(3) . . . . ?
C4 C3 C2 C14 -178.84(16) . . . . ?
C5 C6 C1 O1 178.18(14) . . . . ?
C5 C6 C1 C2 -0.1(2) . . . . ?
C5 C6 C7 C8 175.14(14) . . . . ?
C5 C6 C7 C27 54.2(2) . . . . ?
C5 C6 C7 C26 -65.72(19) . . . . ?
C5 C4 C28 C31A -177.2(4) . . . . ?
C5 C4 C28 C29A 65.3(3) . . . . ?
C5 C4 C28 C30A -49.5(4) . . . . ?
C5 C4 C28 C29 114.4(5) . . . . ?
C5 C4 C28 C31 -133.6(4) . . . . ?
C5 C4 C28 C30 -17.9(7) . . . . ?
C20 C12 C11 C10 -179.44(15) . . . . ?
C20 C21 C22 C23 1.0(3) . . . . ?
C20 C25 C24 C23 1.2(4) . . . . ?
C15 C14 C2 C1 42.1(2) . . . . ?
C15 C14 C2 C3 -138.26(18) . . . . ?
C15 C14 C19 C18 1.1(3) . . . . ?
C15 C16 C17 C18 0.8(3) . . . . ?
C21 C20 C25 C24 -0.1(3) . . . . ?
C28 C4 C5 C6 -176.78(17) . . . . ?
C1AA C10 C11 C12 -177.7(4) . . . . ?
C19 C14 C2 C1 -141.72(18) . . . . ?
C19 C14 C2 C3 37.9(2) . . . . ?
C19 C14 C15 C16 -1.3(3) . . . . ?
C16 C17 C18 C19 -1.1(4) . . . . ?
C25 C20 C21 C22 -0.9(3) . . . . ?
C22 C23 C24 C25 -1.2(3) . . . . ?
C24 C23 C22 C21 0.1(3) . . . . ?
C21A C10 C11 C12 -174.9(6) . . . . ?


_olex2_exptl_crystal_mounting_method ?
_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_mo_191118b_0m
_database_code_depnum_ccdc_archive 'CCDC 2180351'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2022-06-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2019-12-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C43 H42 O'
_chemical_formula_sum            'C43 H42 O'
_chemical_formula_weight         574.76
_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 0.0033 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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.3608(17)
_cell_length_b                   14.084(3)
_cell_length_c                   14.199(3)
_cell_angle_alpha                66.933(3)
_cell_angle_beta                 81.559(3)
_cell_angle_gamma                75.738(3)
_cell_volume                     1666.6(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3712
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      26.939
_cell_measurement_theta_min      2.514
_shelx_estimated_absorpt_T_max   0.990
_shelx_estimated_absorpt_T_min   0.987
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0526 before and 0.0400 after correction. The Ratio of minimum to maximum transmission is 0.9093. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14017
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.170
_diffrn_reflns_theta_min         1.561
_diffrn_ambient_temperature      297(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4855
_reflns_number_total             7284
_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 v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         7284
_refine_ls_number_restraints     1159
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0651
_refine_ls_restrained_S_all      1.171
_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)+(0.1122P)²+0.4491P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1890
_refine_ls_wR_factor_ref         0.2188
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C36, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11), C15(H15), C16(H16), C17(H17), C20(H20),
 C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31),
  C32(H32), C33(H33)
4.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37C,H37B,H37A), C38(H38A,H38B,
 H38C), C39(H39B,H39C,H39A), C41(H41A,H41B,H41C), C42(H42C,H42A,H42B), C43(H43A,
 H43C,H43B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_special_details      
;
The structure was solved using Direct Methods (ShelXS). RE = 0.2, Nqual =  -1, Ralpha = 0.041
;
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
C1 C 0.1430(2) 0.16299(15) 0.24872(14) 0.0352(4) Uani 1 1 d . U . . .
O1 O 0.01155(15) 0.23549(11) 0.23891(11) 0.0435(4) Uani 1 1 d . . . . .
C2 C 0.2367(2) 0.16493(16) 0.31607(14) 0.0377(4) Uani 1 1 d . U . . .
C3 C 0.3709(2) 0.09438(17) 0.33145(15) 0.0424(5) Uani 1 1 d . U . . .
H3 H 0.4340 0.0948 0.3761 0.051 Uiso 1 1 calc R . . . .
C4 C 0.4150(2) 0.02250(17) 0.28228(15) 0.0408(5) Uani 1 1 d . U . . .
C5 C 0.3188(2) 0.02532(16) 0.21523(14) 0.0377(4) Uani 1 1 d . U . . .
H5 H 0.3466 -0.0216 0.1813 0.045 Uiso 1 1 calc R . . . .
C6 C 0.1818(2) 0.09537(15) 0.19610(14) 0.0328(4) Uani 1 1 d . U . . .
C7 C 0.0815(2) 0.09781(15) 0.11872(14) 0.0334(4) Uani 1 1 d . U . . .
C8 C -0.0607(2) 0.18113(14) 0.11352(14) 0.0331(4) Uani 1 1 d . U . . .
C9 C -0.1718(2) 0.19808(15) 0.04880(15) 0.0381(4) Uani 1 1 d . U . . .
H9 H -0.1560 0.1588 0.0073 0.046 Uiso 1 1 calc R . . . .
C10 C -0.3037(2) 0.27026(15) 0.04368(16) 0.0415(5) Uani 1 1 d . U . . .
C11 C -0.3250(2) 0.32771(16) 0.10725(17) 0.0439(5) Uani 1 1 d . U . . .
H11 H -0.4131 0.3764 0.1056 0.053 Uiso 1 1 calc R . . . .
C12 C -0.2195(2) 0.31460(15) 0.17266(15) 0.0378(4) Uani 1 1 d . U . . .
C13 C -0.0876(2) 0.24182(15) 0.17340(14) 0.0346(4) Uani 1 1 d . U . . .
C14 C -0.2482(2) 0.37511(16) 0.24198(16) 0.0403(5) Uani 1 1 d . U . . .
C15 C -0.3467(3) 0.3510(2) 0.32379(18) 0.0530(5) Uani 1 1 d . U . . .
H15 H -0.3929 0.2954 0.3367 0.064 Uiso 1 1 calc R . . . .
C16 C -0.3811(3) 0.4076(2) 0.3897(2) 0.0656(7) Uani 1 1 d . U . . .
H16 H -0.4479 0.3886 0.4457 0.079 Uiso 1 1 calc R . . . .
C17 C -0.3162(3) 0.4900(2) 0.3712(2) 0.0636(7) Uani 1 1 d . U . . .
H17 H -0.3401 0.5279 0.4143 0.076 Uiso 1 1 calc R . . . .
C18 C -0.2128(3) 0.51872(17) 0.28722(17) 0.0491(5) Uani 1 1 d . U . . .
C19 C -0.1760(2) 0.45953(16) 0.22235(16) 0.0419(5) Uani 1 1 d . U . . .
C20 C -0.0686(3) 0.48830(18) 0.14020(17) 0.0496(5) Uani 1 1 d . U . . .
H20 H -0.0435 0.4512 0.0964 0.060 Uiso 1 1 calc R . . . .
C21 C -0.0021(3) 0.5694(2) 0.1247(2) 0.0654(7) Uani 1 1 d . U . . .
H21 H 0.0690 0.5863 0.0712 0.079 Uiso 1 1 calc R . . . .
C22 C -0.0397(4) 0.6275(2) 0.1885(2) 0.0721(7) Uani 1 1 d . U . . .
H22 H 0.0059 0.6831 0.1767 0.086 Uiso 1 1 calc R . . . .
C23 C -0.1409(3) 0.6035(2) 0.2661(2) 0.0641(7) Uani 1 1 d . U . . .
H23 H -0.1649 0.6432 0.3075 0.077 Uiso 1 1 calc R . . . .
C24 C 0.1936(2) 0.24335(16) 0.36734(15) 0.0384(4) Uani 1 1 d . U . . .
C25 C 0.2655(2) 0.32521(18) 0.33692(17) 0.0484(5) Uani 1 1 d . U . . .
H25 H 0.3374 0.3319 0.2834 0.058 Uiso 1 1 calc R . . . .
C26 C 0.2334(3) 0.39913(19) 0.3844(2) 0.0561(6) Uani 1 1 d . U . . .
H26 H 0.2837 0.4541 0.3623 0.067 Uiso 1 1 calc R . . . .
C27 C 0.1290(3) 0.39036(19) 0.46267(19) 0.0546(6) Uani 1 1 d . U . . .
H27 H 0.1092 0.4390 0.4946 0.066 Uiso 1 1 calc R . . . .
C28 C 0.0496(2) 0.30795(17) 0.49645(16) 0.0462(5) Uani 1 1 d . U . . .
C29 C 0.0816(2) 0.23314(16) 0.44768(15) 0.0395(4) Uani 1 1 d . U . . .
C30 C 0.0011(3) 0.15168(18) 0.48200(17) 0.0489(5) Uani 1 1 d . U . . .
H30 H 0.0215 0.1019 0.4514 0.059 Uiso 1 1 calc R . . . .
C31 C -0.1063(3) 0.1449(2) 0.5595(2) 0.0639(7) Uani 1 1 d . U . . .
H31 H -0.1586 0.0911 0.5811 0.077 Uiso 1 1 calc R . . . .
C32 C -0.1374(3) 0.2195(2) 0.60650(19) 0.0673(7) Uani 1 1 d . U . . .
H32 H -0.2107 0.2149 0.6590 0.081 Uiso 1 1 calc R . . . .
C33 C -0.0622(3) 0.2976(2) 0.57645(19) 0.0595(6) Uani 1 1 d . U . . .
H33 H -0.0842 0.3457 0.6090 0.071 Uiso 1 1 calc R . . . .
C34 C 0.1641(2) 0.1243(2) 0.01283(16) 0.0493(5) Uani 1 1 d . U . . .
H34A H 0.1024 0.1252 -0.0360 0.074 Uiso 1 1 calc GR . . . .
H34B H 0.2531 0.0719 0.0165 0.074 Uiso 1 1 calc GR . . . .
H34C H 0.1883 0.1923 -0.0081 0.074 Uiso 1 1 calc GR . . . .
C35 C 0.0416(2) -0.01056(16) 0.15179(19) 0.0484(5) Uani 1 1 d . U . . .
H35A H -0.0044 -0.0291 0.2198 0.073 Uiso 1 1 calc GR . . . .
H35B H 0.1296 -0.0626 0.1510 0.073 Uiso 1 1 calc GR . . . .
H35C H -0.0254 -0.0077 0.1052 0.073 Uiso 1 1 calc GR . . . .
C36 C -0.4214(3) 0.29201(18) -0.0313(2) 0.0541(6) Uani 1 1 d . U . . .
C37 C -0.4047(4) 0.3928(3) -0.1234(3) 0.1157(14) Uani 1 1 d . U . . .
H37C H -0.3213 0.3773 -0.1670 0.173 Uiso 1 1 calc GR . . . .
H37B H -0.3899 0.4447 -0.0997 0.173 Uiso 1 1 calc GR . . . .
H37A H -0.4924 0.4197 -0.1611 0.173 Uiso 1 1 calc GR . . . .
C38 C -0.4166(5) 0.2003(3) -0.0587(4) 0.1273(16) Uani 1 1 d . U . . .
H38A H -0.3303 0.1912 -0.1026 0.191 Uiso 1 1 calc GR . . . .
H38B H -0.5033 0.2121 -0.0938 0.191 Uiso 1 1 calc GR . . . .
H38C H -0.4131 0.1381 0.0025 0.191 Uiso 1 1 calc GR . . . .
C39 C -0.5775(3) 0.3179(3) 0.0152(3) 0.0997(11) Uani 1 1 d . U . . .
H39B H -0.6485 0.3294 -0.0326 0.150 Uiso 1 1 calc GR . . . .
H39C H -0.5889 0.3804 0.0300 0.150 Uiso 1 1 calc GR . . . .
H39A H -0.5930 0.2601 0.0775 0.150 Uiso 1 1 calc GR . . . .
C40 C 0.5620(2) -0.05765(19) 0.30598(17) 0.0506(6) Uani 1 1 d . U . . .
C41 C 0.6775(3) -0.0138(3) 0.3347(3) 0.0880(10) Uani 1 1 d . U . . .
H41A H 0.6861 0.0534 0.2825 0.132 Uiso 1 1 calc GR . . . .
H41B H 0.7713 -0.0620 0.3403 0.132 Uiso 1 1 calc GR . . . .
H41C H 0.6472 -0.0056 0.3991 0.132 Uiso 1 1 calc GR . . . .
C42 C 0.5360(4) -0.1536(3) 0.3987(4) 0.1234(16) Uani 1 1 d . U . . .
H42C H 0.4848 -0.1939 0.3793 0.185 Uiso 1 1 calc GR . . . .
H42A H 0.4776 -0.1315 0.4508 0.185 Uiso 1 1 calc GR . . . .
H42B H 0.6292 -0.1964 0.4248 0.185 Uiso 1 1 calc GR . . . .
C43 C 0.6304(4) -0.0845(3) 0.2145(3) 0.1063(13) Uani 1 1 d . U . . .
H43A H 0.5747 -0.1272 0.2025 0.160 Uiso 1 1 calc GR . . . .
H43C H 0.7303 -0.1227 0.2272 0.160 Uiso 1 1 calc GR . . . .
H43B H 0.6300 -0.0207 0.1552 0.160 Uiso 1 1 calc GR . . . .


_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
C1 O1 1.377(2) . ?
C1 C2 1.401(3) . ?
C1 C6 1.380(3) . ?
O1 C13 1.372(2) . ?
C2 C3 1.382(3) . ?
C2 C24 1.496(3) . ?
C3 C4 1.395(3) . ?
C4 C5 1.387(3) . ?
C4 C40 1.534(3) . ?
C5 C6 1.400(3) . ?
C6 C7 1.532(2) . ?
C7 C8 1.532(2) . ?
C7 C34 1.536(3) . ?
C7 C35 1.536(3) . ?
C8 C9 1.403(2) . ?
C8 C13 1.385(2) . ?
C9 C10 1.383(3) . ?
C10 C11 1.396(3) . ?
C10 C36 1.538(3) . ?
C11 C12 1.385(3) . ?
C12 C13 1.396(3) . ?
C12 C14 1.495(3) . ?
C14 C15 1.359(3) . ?
C14 C19 1.424(3) . ?
C15 C16 1.410(3) . ?
C16 C17 1.358(4) . ?
C17 C18 1.414(4) . ?
C18 C19 1.425(3) . ?
C18 C23 1.422(4) . ?
C19 C20 1.422(3) . ?
C20 C21 1.361(3) . ?
C21 C22 1.399(4) . ?
C22 C23 1.337(4) . ?
C24 C25 1.370(3) . ?
C24 C29 1.420(3) . ?
C25 C26 1.402(3) . ?
C26 C27 1.356(4) . ?
C27 C28 1.419(3) . ?
C28 C29 1.426(3) . ?
C28 C33 1.415(3) . ?
C29 C30 1.415(3) . ?
C30 C31 1.368(3) . ?
C31 C32 1.406(4) . ?
C32 C33 1.345(4) . ?
C36 C37 1.531(4) . ?
C36 C38 1.477(4) . ?
C36 C39 1.532(4) . ?
C40 C41 1.541(4) . ?
C40 C42 1.514(4) . ?
C40 C43 1.504(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 113.90(16) . . ?
O1 C1 C6 123.75(16) . . ?
C6 C1 C2 122.34(17) . . ?
C13 O1 C1 118.86(14) . . ?
C1 C2 C24 120.61(17) . . ?
C3 C2 C1 118.11(17) . . ?
C3 C2 C24 121.26(17) . . ?
C2 C3 C4 122.20(17) . . ?
C3 C4 C40 120.07(18) . . ?
C5 C4 C3 117.16(17) . . ?
C5 C4 C40 122.74(18) . . ?
C4 C5 C6 123.22(17) . . ?
C1 C6 C5 116.94(16) . . ?
C1 C6 C7 121.79(16) . . ?
C5 C6 C7 121.25(16) . . ?
C6 C7 C34 108.88(16) . . ?
C6 C7 C35 109.66(16) . . ?
C8 C7 C6 110.13(14) . . ?
C8 C7 C34 109.77(16) . . ?
C8 C7 C35 108.93(15) . . ?
C35 C7 C34 109.46(17) . . ?
C9 C8 C7 121.25(16) . . ?
C13 C8 C7 122.05(15) . . ?
C13 C8 C9 116.69(17) . . ?
C10 C9 C8 123.28(18) . . ?
C9 C10 C11 117.20(17) . . ?
C9 C10 C36 122.80(18) . . ?
C11 C10 C36 119.95(18) . . ?
C12 C11 C10 122.21(18) . . ?
C11 C12 C13 118.06(18) . . ?
C11 C12 C14 120.71(17) . . ?
C13 C12 C14 121.22(17) . . ?
O1 C13 C8 123.37(16) . . ?
O1 C13 C12 114.10(16) . . ?
C8 C13 C12 122.53(17) . . ?
C15 C14 C12 119.7(2) . . ?
C15 C14 C19 119.29(19) . . ?
C19 C14 C12 120.96(18) . . ?
C14 C15 C16 122.0(2) . . ?
C17 C16 C15 119.8(2) . . ?
C16 C17 C18 120.7(2) . . ?
C17 C18 C19 119.2(2) . . ?
C17 C18 C23 122.4(2) . . ?
C23 C18 C19 118.4(2) . . ?
C14 C19 C18 119.0(2) . . ?
C20 C19 C14 123.02(18) . . ?
C20 C19 C18 118.0(2) . . ?
C21 C20 C19 120.9(2) . . ?
C20 C21 C22 120.7(3) . . ?
C23 C22 C21 120.3(3) . . ?
C22 C23 C18 121.7(2) . . ?
C25 C24 C2 119.08(19) . . ?
C25 C24 C29 119.82(19) . . ?
C29 C24 C2 121.10(18) . . ?
C24 C25 C26 121.7(2) . . ?
C27 C26 C25 119.9(2) . . ?
C26 C27 C28 120.8(2) . . ?
C27 C28 C29 119.2(2) . . ?
C33 C28 C27 122.4(2) . . ?
C33 C28 C29 118.4(2) . . ?
C24 C29 C28 118.5(2) . . ?
C30 C29 C24 122.94(19) . . ?
C30 C29 C28 118.5(2) . . ?
C31 C30 C29 121.1(2) . . ?
C30 C31 C32 119.8(3) . . ?
C33 C32 C31 120.8(2) . . ?
C32 C33 C28 121.5(2) . . ?
C37 C36 C10 107.8(2) . . ?
C37 C36 C39 104.7(3) . . ?
C38 C36 C10 112.6(2) . . ?
C38 C36 C37 114.1(3) . . ?
C38 C36 C39 106.1(3) . . ?
C39 C36 C10 111.4(2) . . ?
C4 C40 C41 111.7(2) . . ?
C42 C40 C4 108.5(2) . . ?
C42 C40 C41 106.5(3) . . ?
C43 C40 C4 111.85(19) . . ?
C43 C40 C41 105.4(3) . . ?
C43 C40 C42 112.8(3) . . ?

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 C13 C8 -2.2(3) . . . . ?
C1 O1 C13 C12 177.38(17) . . . . ?
C1 C2 C3 C4 0.1(3) . . . . ?
C1 C2 C24 C25 -108.3(2) . . . . ?
C1 C2 C24 C29 72.7(3) . . . . ?
C1 C6 C7 C8 -1.4(3) . . . . ?
C1 C6 C7 C34 119.0(2) . . . . ?
C1 C6 C7 C35 -121.2(2) . . . . ?
O1 C1 C2 C3 179.56(18) . . . . ?
O1 C1 C2 C24 -2.1(3) . . . . ?
O1 C1 C6 C5 -179.33(18) . . . . ?
O1 C1 C6 C7 1.8(3) . . . . ?
C2 C1 O1 C13 178.83(17) . . . . ?
C2 C1 C6 C5 2.0(3) . . . . ?
C2 C1 C6 C7 -176.94(18) . . . . ?
C2 C3 C4 C5 0.9(3) . . . . ?
C2 C3 C4 C40 -177.1(2) . . . . ?
C2 C24 C25 C26 -177.83(19) . . . . ?
C2 C24 C29 C28 177.46(17) . . . . ?
C2 C24 C29 C30 -2.1(3) . . . . ?
C3 C2 C24 C25 70.0(3) . . . . ?
C3 C2 C24 C29 -109.0(2) . . . . ?
C3 C4 C5 C6 -0.5(3) . . . . ?
C3 C4 C40 C41 -30.7(3) . . . . ?
C3 C4 C40 C42 86.3(3) . . . . ?
C3 C4 C40 C43 -148.6(3) . . . . ?
C4 C5 C6 C1 -0.9(3) . . . . ?
C4 C5 C6 C7 178.04(19) . . . . ?
C5 C4 C40 C41 151.4(2) . . . . ?
C5 C4 C40 C42 -91.6(3) . . . . ?
C5 C4 C40 C43 33.5(4) . . . . ?
C5 C6 C7 C8 179.77(17) . . . . ?
C5 C6 C7 C34 -59.8(2) . . . . ?
C5 C6 C7 C35 59.9(2) . . . . ?
C6 C1 O1 C13 0.0(3) . . . . ?
C6 C1 C2 C3 -1.6(3) . . . . ?
C6 C1 C2 C24 176.75(19) . . . . ?
C6 C7 C8 C9 -179.32(17) . . . . ?
C6 C7 C8 C13 -0.6(3) . . . . ?
C7 C8 C9 C10 178.13(19) . . . . ?
C7 C8 C13 O1 2.4(3) . . . . ?
C7 C8 C13 C12 -177.06(18) . . . . ?
C8 C9 C10 C11 -0.4(3) . . . . ?
C8 C9 C10 C36 176.9(2) . . . . ?
C9 C8 C13 O1 -178.79(18) . . . . ?
C9 C8 C13 C12 1.7(3) . . . . ?
C9 C10 C11 C12 0.4(3) . . . . ?
C9 C10 C36 C37 -99.4(3) . . . . ?
C9 C10 C36 C38 27.3(4) . . . . ?
C9 C10 C36 C39 146.3(3) . . . . ?
C10 C11 C12 C13 0.5(3) . . . . ?
C10 C11 C12 C14 -178.1(2) . . . . ?
C11 C10 C36 C37 77.9(3) . . . . ?
C11 C10 C36 C38 -155.4(3) . . . . ?
C11 C10 C36 C39 -36.5(3) . . . . ?
C11 C12 C13 O1 178.78(18) . . . . ?
C11 C12 C13 C8 -1.7(3) . . . . ?
C11 C12 C14 C15 71.3(3) . . . . ?
C11 C12 C14 C19 -107.4(2) . . . . ?
C12 C14 C15 C16 -178.0(2) . . . . ?
C12 C14 C19 C18 176.57(17) . . . . ?
C12 C14 C19 C20 -3.1(3) . . . . ?
C13 C8 C9 C10 -0.6(3) . . . . ?
C13 C12 C14 C15 -107.4(2) . . . . ?
C13 C12 C14 C19 74.0(3) . . . . ?
C14 C12 C13 O1 -2.6(3) . . . . ?
C14 C12 C13 C8 176.97(18) . . . . ?
C14 C15 C16 C17 0.9(4) . . . . ?
C14 C19 C20 C21 -179.7(2) . . . . ?
C15 C14 C19 C18 -2.0(3) . . . . ?
C15 C14 C19 C20 178.3(2) . . . . ?
C15 C16 C17 C18 -0.9(4) . . . . ?
C16 C17 C18 C19 -0.6(4) . . . . ?
C16 C17 C18 C23 -179.1(2) . . . . ?
C17 C18 C19 C14 2.0(3) . . . . ?
C17 C18 C19 C20 -178.3(2) . . . . ?
C17 C18 C23 C22 177.7(3) . . . . ?
C18 C19 C20 C21 0.6(3) . . . . ?
C19 C14 C15 C16 0.6(3) . . . . ?
C19 C18 C23 C22 -0.8(4) . . . . ?
C19 C20 C21 C22 -1.0(4) . . . . ?
C20 C21 C22 C23 0.6(4) . . . . ?
C21 C22 C23 C18 0.4(4) . . . . ?
C23 C18 C19 C14 -179.41(19) . . . . ?
C23 C18 C19 C20 0.3(3) . . . . ?
C24 C2 C3 C4 -178.25(19) . . . . ?
C24 C25 C26 C27 0.1(3) . . . . ?
C24 C29 C30 C31 -179.8(2) . . . . ?
C25 C24 C29 C28 -1.5(3) . . . . ?
C25 C24 C29 C30 178.95(19) . . . . ?
C25 C26 C27 C28 -1.0(4) . . . . ?
C26 C27 C28 C29 0.6(3) . . . . ?
C26 C27 C28 C33 -178.7(2) . . . . ?
C27 C28 C29 C24 0.6(3) . . . . ?
C27 C28 C29 C30 -179.78(19) . . . . ?
C27 C28 C33 C32 179.2(2) . . . . ?
C28 C29 C30 C31 0.6(3) . . . . ?
C29 C24 C25 C26 1.2(3) . . . . ?
C29 C28 C33 C32 -0.1(3) . . . . ?
C29 C30 C31 C32 -0.3(4) . . . . ?
C30 C31 C32 C33 -0.3(4) . . . . ?
C31 C32 C33 C28 0.5(4) . . . . ?
C33 C28 C29 C24 179.96(18) . . . . ?
C33 C28 C29 C30 -0.5(3) . . . . ?
C34 C7 C8 C9 60.8(2) . . . . ?
C34 C7 C8 C13 -120.5(2) . . . . ?
C35 C7 C8 C9 -59.0(2) . . . . ?
C35 C7 C8 C13 119.7(2) . . . . ?
C36 C10 C11 C12 -177.0(2) . . . . ?
C40 C4 C5 C6 177.42(19) . . . . ?

_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_y
_database_code_depnum_ccdc_archive 'CCDC 2180336'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2022-06-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2022-06-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H36 O'
_chemical_formula_sum            'C33 H36 O'
_chemical_formula_weight         448.62
_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 0.0033 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'

_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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.2553(15)
_cell_length_b                   20.450(4)
_cell_length_c                   18.243(4)
_cell_angle_alpha                90
_cell_angle_beta                 100.989(4)
_cell_angle_gamma                90
_cell_volume                     2657.2(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4451
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.86
_cell_measurement_theta_min      2.27
_shelx_estimated_absorpt_T_max   0.993
_shelx_estimated_absorpt_T_min   0.993
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6132
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0970 before and 0.0562 after correction.
The Ratio of minimum to maximum transmission is 0.8220.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26719
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.124
_diffrn_reflns_theta_min         1.511
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3660
_reflns_number_total             7811
_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 v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         7811
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1499
_refine_ls_R_factor_gt           0.0723
_refine_ls_restrained_S_all      1.019
_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)+(0.1225P)²+0.0576P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1984
_refine_ls_wR_factor_ref         0.2446
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C29A)=Sof(C28A)=Sof(C27A)=1-FVAR(1)
 Sof(C29)=Sof(C27)=Sof(C28)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C20(H20), C19(H19), C11(H11), C10(H10), C8(H8), C16(H16),
 C15(H15), C14(H14), C5(H5), C3(H3)
3.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C25(H25A,H25B,H25C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C24(H24A,
 H24B,H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_special_details      
;
The structure was solved using Direct Methods (ShelXS). RE = 0.2, Nqual =  -1, Ralpha = 0.047
;
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
C21 C 0.3145(4) 0.05985(13) -0.03316(16) 0.0807(8) Uani 1 1 d . . . . .
H21 H 0.312887 0.023168 -0.063398 0.097 Uiso 1 1 calc R U . . .
C22 C 0.1645(4) 0.07414(13) -0.00240(15) 0.0729(7) Uani 1 1 d . . . . .
H22 H 0.059561 0.047137 -0.012418 0.088 Uiso 1 1 calc R U . . .
O1 O 0.43919(18) 0.30801(7) 0.00533(8) 0.0567(4) Uani 1 1 d . . . . .
C33 C 0.4447(7) 0.4646(2) -0.29894(17) 0.154(2) Uani 1 1 d . . . . .
H33A H 0.473787 0.493543 -0.336610 0.231 Uiso 1 1 calc R U . . .
H33B H 0.330518 0.478619 -0.284416 0.231 Uiso 1 1 calc R U . . .
H33C H 0.429180 0.420972 -0.318468 0.231 Uiso 1 1 calc R U . . .
C20 C 0.4706(4) 0.09987(13) -0.01960(14) 0.0711(7) Uani 1 1 d . . . . .
H20 H 0.574293 0.089616 -0.040505 0.085 Uiso 1 1 calc R U . . .
C19 C 0.4748(3) 0.15412(11) 0.02393(12) 0.0544(5) Uani 1 1 d . . . . .
H19 H 0.580185 0.180980 0.031433 0.065 Uiso 1 1 calc R U . . .
C11 C 0.3717(3) 0.34404(12) -0.11825(12) 0.0635(6) Uani 1 1 d . . . . .
H11 H 0.268749 0.316088 -0.125349 0.076 Uiso 1 1 calc R U . . .
C10 C 0.4068(3) 0.38145(12) -0.17673(12) 0.0627(6) Uani 1 1 d . . . . .
H10 H 0.327681 0.378206 -0.223107 0.075 Uiso 1 1 calc R U . . .
C29 C 1.0391(11) 0.3367(5) 0.3183(4) 0.107(4) Uani 0.587(11) 1 d . . P A 1
H29A H 1.099951 0.328854 0.369035 0.160 Uiso 1 1 calc R U . . .
H29B H 1.030685 0.382983 0.309275 0.160 Uiso 1 1 calc R U . . .
H29C H 1.110623 0.316857 0.285073 0.160 Uiso 1 1 calc R U . . .
C27 C 0.8892(8) 0.2336(2) 0.3279(3) 0.0722(18) Uani 0.587(11) 1 d . . P A 1
H27A H 0.952908 0.213173 0.292423 0.108 Uiso 1 1 calc R U . . .
H27B H 0.773205 0.211141 0.328368 0.108 Uiso 1 1 calc R U . . .
H27C H 0.967033 0.231570 0.376732 0.108 Uiso 1 1 calc R U . . .
C28 C 0.7220(8) 0.3322(4) 0.3534(2) 0.092(3) Uani 0.587(11) 1 d . . P A 1
H28A H 0.784558 0.329373 0.404682 0.138 Uiso 1 1 calc R U . . .
H28B H 0.609855 0.306179 0.346091 0.138 Uiso 1 1 calc R U . . .
H28C H 0.689692 0.376947 0.341200 0.138 Uiso 1 1 calc R U . . .
C25 C 0.9716(3) 0.37405(13) 0.03132(13) 0.0697(7) Uani 1 1 d . . . . .
H25A H 0.970431 0.329416 0.014914 0.105 Uiso 1 1 calc R U . . .
H25B H 1.054644 0.378253 0.078800 0.105 Uiso 1 1 calc R U . . .
H25C H 1.014368 0.401731 -0.004531 0.105 Uiso 1 1 calc R U . . .
C32 C 0.7801(7) 0.4398(2) -0.2541(3) 0.173(2) Uani 1 1 d . . . . .
H32A H 0.751607 0.400554 -0.282972 0.260 Uiso 1 1 calc R U . . .
H32B H 0.871457 0.430291 -0.209981 0.260 Uiso 1 1 calc R U . . .
H32C H 0.829702 0.472003 -0.283377 0.260 Uiso 1 1 calc R U . . .
C31 C 0.6341(5) 0.53629(14) -0.20724(16) 0.0954(10) Uani 1 1 d . . . . .
H31A H 0.653568 0.562538 -0.248724 0.143 Uiso 1 1 calc R U . . .
H31B H 0.742712 0.538952 -0.167979 0.143 Uiso 1 1 calc R U . . .
H31C H 0.526197 0.552037 -0.189292 0.143 Uiso 1 1 calc R U . . .
C13 C 0.1620(3) 0.12810(11) 0.04390(12) 0.0537(5) Uani 1 1 d . . . . .
C18 C 0.3210(2) 0.17014(9) 0.05791(11) 0.0437(4) Uani 1 1 d . . . . .
C17 C 0.3212(2) 0.22407(10) 0.10682(10) 0.0444(5) Uani 1 1 d . . . . .
C2 C 0.4885(3) 0.26774(9) 0.12778(10) 0.0434(4) Uani 1 1 d . . . . .
C1 C 0.5478(2) 0.30948(9) 0.07593(10) 0.0427(4) Uani 1 1 d . . . . .
C12 C 0.4882(3) 0.34770(9) -0.04916(10) 0.0469(5) Uani 1 1 d . . . . .
C7 C 0.6415(3) 0.38879(9) -0.03674(10) 0.0441(4) Uani 1 1 d . . . . .
C8 C 0.6723(3) 0.42577(10) -0.09771(10) 0.0512(5) Uani 1 1 d . . . . .
H8 H 0.776031 0.453392 -0.090884 0.061 Uiso 1 1 calc R U . . .
C9 C 0.5578(3) 0.42373(11) -0.16761(11) 0.0551(5) Uani 1 1 d . . . . .
C30 C 0.6023(4) 0.46585(12) -0.23203(12) 0.0695(7) Uani 1 1 d . . . . .
C16 C 0.1684(3) 0.23397(12) 0.13928(13) 0.0618(6) Uani 1 1 d . . . . .
H16 H 0.169007 0.268650 0.172302 0.074 Uiso 1 1 calc R U . . .
C15 C 0.0111(3) 0.19309(15) 0.12392(16) 0.0744(7) Uani 1 1 d . . . . .
H15 H -0.092107 0.201444 0.145883 0.089 Uiso 1 1 calc R U . . .
C14 C 0.0083(3) 0.14186(14) 0.07763(16) 0.0714(7) Uani 1 1 d . . . . .
H14 H -0.097276 0.115127 0.067840 0.086 Uiso 1 1 calc R U . . .
C23 C 0.7709(3) 0.39457(10) 0.03899(10) 0.0471(5) Uani 1 1 d . . . . .
C6 C 0.7033(3) 0.34982(9) 0.09538(10) 0.0431(4) Uani 1 1 d . . . . .
C5 C 0.7975(3) 0.34795(10) 0.16963(10) 0.0490(5) Uani 1 1 d . . . . .
H5 H 0.901904 0.374710 0.183720 0.059 Uiso 1 1 calc R U . . .
C4 C 0.7434(3) 0.30823(10) 0.22343(10) 0.0494(5) Uani 1 1 d . . . . .
C26 C 0.8468(3) 0.30802(13) 0.30514(12) 0.0655(6) Uani 1 1 d . . . . .
C3 C 0.5874(3) 0.26877(10) 0.20051(11) 0.0478(5) Uani 1 1 d . . . . .
H3 H 0.547666 0.241877 0.235564 0.057 Uiso 1 1 calc R U . . .
C24 C 0.7718(4) 0.46601(11) 0.06623(13) 0.0698(7) Uani 1 1 d . . . . .
H24A H 0.854380 0.469891 0.113847 0.105 Uiso 1 1 calc R U . . .
H24B H 0.646993 0.478416 0.070966 0.105 Uiso 1 1 calc R U . . .
H24C H 0.814548 0.494168 0.030816 0.105 Uiso 1 1 calc R U . . .
C29A C 1.047(2) 0.3080(13) 0.3105(8) 0.193(11) Uani 0.413(11) 1 d . . P A 2
C28A C 0.8158(17) 0.3866(5) 0.3342(5) 0.114(4) Uani 0.413(11) 1 d . . P A 2
C27A C 0.778(2) 0.2647(7) 0.3563(5) 0.152(9) Uani 0.413(11) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C21 H21 0.9300 . ?
C21 C22 1.348(4) . ?
C21 C20 1.381(4) . ?
C22 H22 0.9300 . ?
C22 C13 1.392(4) . ?
O1 C1 1.376(2) . ?
O1 C12 1.381(2) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C33 C30 1.506(4) . ?
C20 H20 0.9300 . ?
C20 C19 1.361(3) . ?
C19 H19 0.9300 . ?
C19 C18 1.415(3) . ?
C11 H11 0.9300 . ?
C11 C10 1.375(3) . ?
C11 C12 1.379(3) . ?
C10 H10 0.9300 . ?
C10 C9 1.380(3) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C29 C26 1.490(7) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C27 C26 1.592(5) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C28 C26 1.465(5) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C25 C23 1.547(3) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C32 C30 1.520(4) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C31 C30 1.514(4) . ?
C13 C18 1.422(3) . ?
C13 C14 1.401(3) . ?
C18 C17 1.418(3) . ?
C17 C2 1.497(3) . ?
C17 C16 1.368(3) . ?
C2 C1 1.401(2) . ?
C2 C3 1.383(3) . ?
C1 C6 1.388(3) . ?
C12 C7 1.378(3) . ?
C7 C8 1.398(3) . ?
C7 C23 1.520(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.384(3) . ?
C9 C30 1.540(3) . ?
C16 H16 0.9300 . ?
C16 C15 1.399(3) . ?
C15 H15 0.9300 . ?
C15 C14 1.343(4) . ?
C14 H14 0.9300 . ?
C23 C6 1.526(3) . ?
C23 C24 1.543(3) . ?
C6 C5 1.397(3) . ?
C5 H5 0.9300 . ?
C5 C4 1.387(3) . ?
C4 C26 1.536(3) . ?
C4 C3 1.388(3) . ?
C26 C29A 1.434(18) . ?
C26 C28A 1.721(9) . ?
C26 C27A 1.444(10) . ?
C3 H3 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C22 C21 H21 120.1 . . ?
C22 C21 C20 119.8(3) . . ?
C20 C21 H21 120.1 . . ?
C21 C22 H22 119.0 . . ?
C21 C22 C13 122.0(2) . . ?
C13 C22 H22 119.0 . . ?
C1 O1 C12 118.73(14) . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
C21 C20 H20 119.5 . . ?
C19 C20 C21 120.9(2) . . ?
C19 C20 H20 119.5 . . ?
C20 C19 H19 119.6 . . ?
C20 C19 C18 120.8(2) . . ?
C18 C19 H19 119.6 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.5(2) . . ?
C12 C11 H11 119.8 . . ?
C11 C10 H10 119.5 . . ?
C11 C10 C9 121.00(19) . . ?
C9 C10 H10 119.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
C22 C13 C18 119.0(2) . . ?
C22 C13 C14 122.0(2) . . ?
C14 C13 C18 119.1(2) . . ?
C19 C18 C13 117.5(2) . . ?
C19 C18 C17 123.31(17) . . ?
C17 C18 C13 119.13(18) . . ?
C18 C17 C2 121.90(16) . . ?
C16 C17 C18 118.91(19) . . ?
C16 C17 C2 119.07(19) . . ?
C1 C2 C17 121.97(17) . . ?
C3 C2 C17 120.09(16) . . ?
C3 C2 C1 117.93(17) . . ?
O1 C1 C2 115.07(15) . . ?
O1 C1 C6 123.01(15) . . ?
C6 C1 C2 121.92(16) . . ?
C11 C12 O1 115.40(16) . . ?
C7 C12 O1 123.40(16) . . ?
C7 C12 C11 121.20(17) . . ?
C12 C7 C8 116.48(17) . . ?
C12 C7 C23 122.45(16) . . ?
C8 C7 C23 121.07(16) . . ?
C7 C8 H8 118.0 . . ?
C9 C8 C7 123.90(19) . . ?
C9 C8 H8 118.0 . . ?
C10 C9 C8 116.95(18) . . ?
C10 C9 C30 122.38(19) . . ?
C8 C9 C30 120.6(2) . . ?
C33 C30 C32 109.3(3) . . ?
C33 C30 C31 107.9(3) . . ?
C33 C30 C9 111.8(2) . . ?
C32 C30 C9 108.6(2) . . ?
C31 C30 C32 108.9(3) . . ?
C31 C30 C9 110.26(19) . . ?
C17 C16 H16 119.3 . . ?
C17 C16 C15 121.5(2) . . ?
C15 C16 H16 119.3 . . ?
C16 C15 H15 119.8 . . ?
C14 C15 C16 120.4(2) . . ?
C14 C15 H15 119.8 . . ?
C13 C14 H14 119.5 . . ?
C15 C14 C13 121.0(2) . . ?
C15 C14 H14 119.5 . . ?
C7 C23 C25 109.01(16) . . ?
C7 C23 C6 110.10(15) . . ?
C7 C23 C24 109.29(16) . . ?
C6 C23 C25 109.11(16) . . ?
C6 C23 C24 109.44(16) . . ?
C24 C23 C25 109.88(18) . . ?
C1 C6 C23 122.29(16) . . ?
C1 C6 C5 117.09(16) . . ?
C5 C6 C23 120.62(16) . . ?
C6 C5 H5 118.3 . . ?
C4 C5 C6 123.38(18) . . ?
C4 C5 H5 118.3 . . ?
C5 C4 C26 122.46(18) . . ?
C5 C4 C3 116.85(17) . . ?
C3 C4 C26 120.67(18) . . ?
C29 C26 C27 101.9(4) . . ?
C29 C26 C4 115.1(3) . . ?
C28 C26 C29 115.9(5) . . ?
C28 C26 C27 106.1(4) . . ?
C28 C26 C4 109.8(3) . . ?
C4 C26 C27 106.9(2) . . ?
C4 C26 C28A 103.2(3) . . ?
C29A C26 C4 111.5(6) . . ?
C29A C26 C28A 99.8(10) . . ?
C29A C26 C27A 115.2(10) . . ?
C27A C26 C4 117.7(4) . . ?
C27A C26 C28A 107.0(7) . . ?
C2 C3 C4 122.82(17) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 H3 118.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 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
C21 C22 C13 C18 1.3(3) . . . . ?
C21 C22 C13 C14 -178.1(2) . . . . ?
C21 C20 C19 C18 1.5(4) . . . . ?
C22 C21 C20 C19 -0.6(4) . . . . ?
C22 C13 C18 C19 -0.5(3) . . . . ?
C22 C13 C18 C17 -178.14(19) . . . . ?
C22 C13 C14 C15 178.0(2) . . . . ?
O1 C1 C6 C23 -2.1(3) . . . . ?
O1 C1 C6 C5 177.99(17) . . . . ?
O1 C12 C7 C8 179.92(17) . . . . ?
O1 C12 C7 C23 -0.5(3) . . . . ?
C20 C21 C22 C13 -0.8(4) . . . . ?
C20 C19 C18 C13 -0.9(3) . . . . ?
C20 C19 C18 C17 176.7(2) . . . . ?
C19 C18 C17 C2 -1.5(3) . . . . ?
C19 C18 C17 C16 -177.38(19) . . . . ?
C11 C10 C9 C8 1.0(4) . . . . ?
C11 C10 C9 C30 179.4(2) . . . . ?
C11 C12 C7 C8 -0.4(3) . . . . ?
C11 C12 C7 C23 179.2(2) . . . . ?
C10 C11 C12 O1 179.9(2) . . . . ?
C10 C11 C12 C7 0.2(4) . . . . ?
C10 C9 C30 C33 10.9(4) . . . . ?
C10 C9 C30 C32 -109.9(4) . . . . ?
C10 C9 C30 C31 130.9(3) . . . . ?
C25 C23 C6 C1 -117.9(2) . . . . ?
C25 C23 C6 C5 62.0(2) . . . . ?
C13 C18 C17 C2 176.08(17) . . . . ?
C13 C18 C17 C16 0.2(3) . . . . ?
C18 C13 C14 C15 -1.4(3) . . . . ?
C18 C17 C2 C1 68.2(3) . . . . ?
C18 C17 C2 C3 -113.1(2) . . . . ?
C18 C17 C16 C15 -1.5(3) . . . . ?
C17 C2 C1 O1 1.1(3) . . . . ?
C17 C2 C1 C6 -179.81(18) . . . . ?
C17 C2 C3 C4 -179.92(18) . . . . ?
C17 C16 C15 C14 1.4(4) . . . . ?
C2 C17 C16 C15 -177.5(2) . . . . ?
C2 C1 C6 C23 178.93(17) . . . . ?
C2 C1 C6 C5 -1.0(3) . . . . ?
C1 O1 C12 C11 -179.39(18) . . . . ?
C1 O1 C12 C7 0.3(3) . . . . ?
C1 C2 C3 C4 -1.2(3) . . . . ?
C1 C6 C5 C4 0.1(3) . . . . ?
C12 O1 C1 C2 -179.95(17) . . . . ?
C12 O1 C1 C6 1.0(3) . . . . ?
C12 C11 C10 C9 -0.5(4) . . . . ?
C12 C7 C8 C9 0.9(3) . . . . ?
C12 C7 C23 C25 119.2(2) . . . . ?
C12 C7 C23 C6 -0.5(3) . . . . ?
C12 C7 C23 C24 -120.7(2) . . . . ?
C7 C8 C9 C10 -1.2(3) . . . . ?
C7 C8 C9 C30 -179.68(19) . . . . ?
C7 C23 C6 C1 1.7(3) . . . . ?
C7 C23 C6 C5 -178.38(17) . . . . ?
C8 C7 C23 C25 -61.2(2) . . . . ?
C8 C7 C23 C6 179.11(17) . . . . ?
C8 C7 C23 C24 58.9(2) . . . . ?
C8 C9 C30 C33 -170.7(3) . . . . ?
C8 C9 C30 C32 68.5(3) . . . . ?
C8 C9 C30 C31 -50.7(3) . . . . ?
C16 C17 C2 C1 -115.8(2) . . . . ?
C16 C17 C2 C3 62.8(3) . . . . ?
C16 C15 C14 C13 0.1(4) . . . . ?
C14 C13 C18 C19 178.94(19) . . . . ?
C14 C13 C18 C17 1.3(3) . . . . ?
C23 C7 C8 C9 -178.68(19) . . . . ?
C23 C6 C5 C4 -179.81(18) . . . . ?
C6 C5 C4 C26 -178.72(19) . . . . ?
C6 C5 C4 C3 0.2(3) . . . . ?
C5 C4 C26 C29 -17.9(5) . . . . ?
C5 C4 C26 C27 -130.3(3) . . . . ?
C5 C4 C26 C28 115.1(4) . . . . ?
C5 C4 C26 C29A -43.8(12) . . . . ?
C5 C4 C26 C28A 62.5(5) . . . . ?
C5 C4 C26 C27A 180.0(9) . . . . ?
C5 C4 C3 C2 0.4(3) . . . . ?
C26 C4 C3 C2 179.33(19) . . . . ?
C3 C2 C1 O1 -177.53(16) . . . . ?
C3 C2 C1 C6 1.5(3) . . . . ?
C3 C4 C26 C29 163.2(5) . . . . ?
C3 C4 C26 C27 50.9(3) . . . . ?
C3 C4 C26 C28 -63.8(4) . . . . ?
C3 C4 C26 C29A 137.4(11) . . . . ?
C3 C4 C26 C28A -116.4(5) . . . . ?
C3 C4 C26 C27A 1.1(10) . . . . ?
C24 C23 C6 C1 121.8(2) . . . . ?
C24 C23 C6 C5 -58.2(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_20221124-ch3cn_auto
_database_code_depnum_ccdc_archive 'CCDC 2308128'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2023-11-15 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2023-11-15
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C51 H46 O'
_chemical_formula_sum            'C51 H46 O'
_chemical_formula_weight         674.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         CHON
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3790(2)
_cell_length_b                   18.1303(3)
_cell_length_c                   19.2624(4)
_cell_angle_alpha                83.876(2)
_cell_angle_beta                 81.273(2)
_cell_angle_gamma                81.763(2)
_cell_volume                     3872.71(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    20313
_cell_measurement_temperature    291(1)
_cell_measurement_theta_max      75.0710
_cell_measurement_theta_min      2.3700
_shelx_estimated_absorpt_T_max   0.960
_shelx_estimated_absorpt_T_min   0.928
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49955
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         2.329
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      291(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     56.00  98.00   0.50    0.51    --   62.89  15.00 120.00   84
  2  ω     77.00 121.00   0.50    0.51    --   76.75  15.00 150.00   88
  3  ω     65.00 117.00   0.50    0.51    --   76.75  15.00  90.00  104
  4  ω     65.00 121.00   0.50    0.51    --   76.75  15.00  30.00  112
  5  ω     26.00  51.00   0.50    0.51    --   62.89-125.00-180.00   50
  6  ω     23.00  57.00   0.50    0.51    --   62.89-125.00-150.00   68
  7  ω     42.00  98.00   0.50    0.51    --   76.75-125.00 -30.00  112
  8  ω     41.00  97.00   0.50    0.51    --   76.75-125.00 -90.00  112
  9  ω     45.00  80.00   0.50    0.51    --   76.75-125.00  30.00   70
 10  ω     28.00  57.00   0.50    0.51    --   62.89-125.00 150.00   58
 11  ω     31.00  86.00   0.50    0.51    --   72.93-125.00 120.00  110
 12  ω     35.00  96.00   0.50    0.51    --   76.75-125.00  60.00  122
 13  ω     35.00  98.00   0.50    0.51    --   76.75-125.00-150.00  126
 14  ω   -111.00 -72.00   0.50    0.51    --  -81.49 -15.00-120.00   78
 15  ω    -97.00 -71.00   0.50    0.51    --  -63.72 -15.00-180.00   52
 16  ω    -97.00 -56.00   0.50    0.51    --  -63.72 -15.00-150.00   82
 17  ω   -105.00 -71.00   0.50    0.51    --  -76.43 -15.00-150.00   68
 18  ω   -101.00 -68.00   0.50    0.51    --  -63.72 -15.00 -90.00   66
 19  ω   -120.00 -80.00   0.50    0.51    --  -81.49 -15.00-180.00   80
 20  ω   -116.00 -69.00   0.50    0.51    --  -76.43 -15.00 -90.00   94
 21  ω    -94.00 -69.00   0.50    0.51    --  -63.72 -15.00 -60.00   50
 22  ω   -124.00 -72.00   0.50    0.51    --  -81.49 -15.00 120.00  104
 23  ω   -103.00 -70.00   0.50    0.51    --  -63.72 -15.00 150.00   66
 24  ω    -65.00 -25.00   0.50    0.51    --  -63.72 125.00 -30.00   80
 25  ω    -53.00 -25.00   0.50    0.51    --  -63.72 125.00 -90.00   56
 26  ω   -102.00 -76.00   0.50    0.51    --  -81.49 125.00-180.00   52
 27  ω   -102.00 -76.00   0.50    0.51    --  -81.49 125.00 -60.00   52
 28  ω   -102.00 -46.00   0.50    0.51    --  -81.49 125.00 -90.00  112
 29  ω   -102.00 -75.00   0.50    0.51    --  -81.49 125.00 -30.00   54
 30  ω   -101.00 -52.00   0.50    0.51    --  -81.49 125.00   0.00   98
 31  ω   -102.00 -48.00   0.50    0.51    --  -81.49 125.00  30.00  108
 32  ω   -102.00 -52.00   0.50    0.51    --  -81.49 125.00  60.00  100
 33  ω   -102.00 -60.00   0.50    0.51    --  -81.49 125.00  90.00   84
 34  ω   -100.00 -50.00   0.50    0.51    --  -81.49 125.00 150.00  100
 35  ω    -52.00 -27.00   0.50    0.51    --  -63.72 125.00 150.00   50
 36  ω    -73.00 -34.00   0.50    0.51    --  -76.43 125.00  90.00   78
 37  ω   -102.00 -42.00   0.50    0.51    --  -81.49 125.00-150.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0008712000
_diffrn_orient_matrix_UB_12      0.0765668000
_diffrn_orient_matrix_UB_13      0.0280419000
_diffrn_orient_matrix_UB_21      0.0232327000
_diffrn_orient_matrix_UB_22      -0.0393472000
_diffrn_orient_matrix_UB_23      0.0724778000
_diffrn_orient_matrix_UB_31      0.1361611000
_diffrn_orient_matrix_UB_32      -0.0041017000
_diffrn_orient_matrix_UB_33      -0.0236121000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10143
_reflns_number_total             13584
_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       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1077
_refine_ls_number_reflns         13584
_refine_ls_number_restraints     204
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0573
_refine_ls_restrained_S_all      1.144
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0851P)²+0.5967P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1682
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C95-C97 \\sim C95-C97A
 with sigma of 0.02
 C95-C98 \\sim C95-C98A
 with sigma of 0.02
 C47-C49 \\sim C47-C49A
 with sigma of 0.02
 C95-C96 \\sim C95-C96A
 with sigma of 0.02
 C47-C50 \\sim C47-C50A
 with sigma of 0.02
 C47-C48 \\sim C47-C48A
 with sigma of 0.02
 C99-C101 \\sim C99-C3
 with sigma of 0.02
 C99-C102 \\sim C99-C1B
 with sigma of 0.02
 C99-C100 \\sim C99-C1A
 with sigma of 0.02
 C43-C46 \\sim C43-C46A
 with sigma of 0.02
 C43-C44 \\sim C43-C44A
 with sigma of 0.02
 C43-C45 \\sim C43-C45A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1A) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C101)
\\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C96A) \\sim Ueq,
Uanis(C98) \\sim Ueq, Uanis(C98A) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C97A)
\\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C48A) \\sim Ueq, Uanis(C48) \\sim Ueq,
Uanis(C49A) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50A) \\sim Ueq, Uanis(C50)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C30) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C31)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C35) \\sim Ueq,
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C46A) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C44A)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C45A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C45) \\sim Ueq, Uanis(C44A) \\sim Ueq, Uanis(C45A) \\sim Ueq, Uanis(C46A)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C46) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Sof(C98A)=Sof(H98D)=Sof(H98E)=Sof(H98F)=Sof(C96A)=Sof(H96D)=Sof(H96E)=
 Sof(H96F)=Sof(C97A)=Sof(H97D)=Sof(H97E)=Sof(H97F)=1-FVAR(1)
 Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(H97C)=Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(H98C)=
 Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(H96C)=FVAR(1)
 Sof(C50A)=Sof(H50D)=Sof(H50E)=Sof(H50F)=Sof(C49A)=Sof(H49D)=Sof(H49E)=
 Sof(H49F)=Sof(C48A)=Sof(H48D)=Sof(H48E)=Sof(H48F)=1-FVAR(2)
 Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=
 Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(2)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=1-FVAR(3)
 Sof(C100)=Sof(H10G)=Sof(H10H)=Sof(H10I)=Sof(C101)=Sof(H10J)=Sof(H10K)=
 Sof(H10L)=Sof(C102)=Sof(H10M)=Sof(H10N)=Sof(H10O)=FVAR(3)
 Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C44A)=Sof(H44D)=Sof(H44E)=
 Sof(H44F)=Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(4)
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(4)
5.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C57(H57), C55(H55), C91(H91), C17(H17), C6(H6), C8(H8),
 C22(H22), C28(H28), C63(H63), C74(H74), C94(H94), C61(H61), C82(H82), C87(H87),
  C77(H77), C92(H92), C20(H20), C18(H18), C27(H27), C25(H25), C72(H72),
 C35(H35), C93(H93), C86(H86), C39(H39), C19(H19), C69(H69), C84(H84), C26(H26),
  C85(H85), C71(H71), C80(H80), C30(H30), C78(H78), C70(H70), C42(H42),
 C40(H40), C41(H41), C79(H79), C34(H34), C32(H32), C33(H33)
5.b Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C51(H51A,H51B,H51C), C104(H10A,H10B,H10C), C46(H46A,H46B,
 H46C), C103(H10D,H10E,H10F), C100(H10G,H10H,H10I), C101(H10J,H10K,H10L),
 C102(H10M,H10N,H10O), C97(H97A,H97B,H97C), C48(H48A,H48B,H48C), C49(H49A,H49B,
 H49C), C98(H98A,H98B,H98C), C50(H50A,H50B,H50C), C45(H45A,H45B,H45C), C44(H44A,
 H44B,H44C), C96(H96A,H96B,H96C), C98A(H98D,H98E,H98F), C96A(H96D,H96E,H96F),
 C97A(H97D,H97E,H97F), C50A(H50D,H50E,H50F), C49A(H49D,H49E,H49F), C48A(H48D,
 H48E,H48F), C3(H3A,H3B,H3C), C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC),
 C46A(H46D,H46E,H46F), C44A(H44D,H44E,H44F), C45A(H45D,H45E,H45F)
;
_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
O3 O 0.58258(11) 0.67864(7) 0.58082(6) 0.0518(3) Uani 1 1 d . . . . .
O66 O 0.86051(11) 0.16333(6) 0.87671(7) 0.0499(3) Uani 1 1 d . . . . .
C2 C 0.64458(15) 0.61125(9) 0.56300(9) 0.0418(4) Uani 1 1 d . . . . .
C1 C 0.67782(14) 0.56337(9) 0.62025(9) 0.0412(4) Uani 1 1 d . . . . .
C11 C 0.67237(15) 0.59186(10) 0.49427(9) 0.0427(4) Uani 1 1 d . . . . .
C15 C 0.64511(15) 0.58662(9) 0.69373(9) 0.0418(4) Uani 1 1 d . . . . .
C4 C 0.53847(15) 0.72836(10) 0.52913(9) 0.0448(4) Uani 1 1 d . . . . .
C67 C 0.72720(15) 0.23558(10) 0.98521(9) 0.0438(4) Uani 1 1 d . . . . .
C53 C 0.80971(14) 0.11613(9) 0.92968(9) 0.0429(4) Uani 1 1 d . . . . .
C54 C 0.74276(15) 0.15174(10) 0.98639(10) 0.0451(4) Uani 1 1 d . . . . .
C13 C 0.77124(15) 0.47111(10) 0.53895(9) 0.0450(4) Uani 1 1 d . . . . .
C89 C 0.94018(15) 0.26828(10) 0.77789(9) 0.0450(4) Uani 1 1 d . . . . .
C65 C 0.92429(15) 0.13393(10) 0.81720(9) 0.0442(4) Uani 1 1 d . . . . .
C90 C 0.82191(15) 0.30469(10) 0.77885(9) 0.0457(4) Uani 1 1 d . . . . .
C81 C 0.79612(16) 0.38184(10) 0.79123(9) 0.0477(4) Uani 1 1 d . . . . .
C12 C 0.73548(15) 0.52130(10) 0.48422(9) 0.0465(4) Uani 1 1 d . . . . .
H12 H 0.754673 0.507073 0.438471 0.056 Uiso 1 1 calc R U . . .
C24 C 0.73346(15) 0.60431(10) 0.73036(9) 0.0450(4) Uani 1 1 d . . . . .
C64 C 0.96694(15) 0.18751(10) 0.76562(10) 0.0472(4) Uani 1 1 d . . . . .
C88 C 1.03189(16) 0.30773(11) 0.79030(10) 0.0486(4) Uani 1 1 d . . . . .
C14 C 0.74107(15) 0.49402(10) 0.60690(9) 0.0457(4) Uani 1 1 d . . . . .
H14 H 0.764217 0.461599 0.644603 0.055 Uiso 1 1 calc R U . . .
C58 C 0.82367(15) 0.03925(10) 0.92700(10) 0.0453(4) Uani 1 1 d . . . . .
C16 C 0.52534(15) 0.58800(9) 0.72685(9) 0.0443(4) Uani 1 1 d . . . . .
C5 C 0.47124(16) 0.79293(10) 0.55422(10) 0.0485(4) Uani 1 1 d . . . . .
C76 C 0.82511(16) 0.27319(10) 0.99034(9) 0.0461(4) Uani 1 1 d . . . . .
C9 C 0.55992(16) 0.71613(10) 0.45860(10) 0.0474(4) Uani 1 1 d . . . . .
C56 C 0.70240(16) 0.02922(10) 1.04305(10) 0.0508(4) Uani 1 1 d . . . . .
C23 C 0.70303(17) 0.62069(11) 0.80284(10) 0.0518(4) Uani 1 1 d . . . . .
C37 C 0.45606(17) 0.80154(10) 0.63124(10) 0.0500(4) Uani 1 1 d . . . . .
C57 C 0.76834(16) -0.00220(10) 0.98513(10) 0.0507(4) Uani 1 1 d . . . . .
H57 H 0.776626 -0.053921 0.984568 0.061 Uiso 1 1 calc R U . . .
C60 C 0.94498(15) 0.05828(10) 0.80853(10) 0.0478(4) Uani 1 1 d . . . . .
C10 C 0.63963(17) 0.64656(11) 0.43205(10) 0.0513(4) Uani 1 1 d . . . . .
C21 C 0.49572(17) 0.60528(11) 0.79892(10) 0.0513(4) Uani 1 1 d . . . . .
C73 C 0.60206(18) 0.35728(11) 0.97134(10) 0.0533(5) Uani 1 1 d . . . . .
C68 C 0.61481(16) 0.27696(10) 0.97668(10) 0.0483(4) Uani 1 1 d . . . . .
C55 C 0.69065(16) 0.10699(10) 1.04240(10) 0.0503(4) Uani 1 1 d . . . . .
H55 H 0.646322 0.129687 1.080862 0.060 Uiso 1 1 calc R U . . .
C75 C 0.81086(18) 0.35336(11) 0.98556(10) 0.0541(5) Uani 1 1 d . . . . .
C91 C 0.67511(17) 0.41726(11) 0.79333(11) 0.0572(5) Uani 1 1 d . . . . .
H91 H 0.657123 0.467342 0.802220 0.069 Uiso 1 1 calc R U . . .
C17 C 0.43186(16) 0.57187(11) 0.69229(11) 0.0532(5) Uani 1 1 d . . . . .
H17 H 0.449078 0.560253 0.645656 0.064 Uiso 1 1 calc R U . . .
C59 C 0.89624(16) 0.00098(10) 0.86519(11) 0.0531(5) Uani 1 1 d . . . . .
C6 C 0.42332(17) 0.84627(10) 0.50559(11) 0.0544(5) Uani 1 1 d . . . . .
H6 H 0.378112 0.889658 0.521491 0.065 Uiso 1 1 calc R U . . .
C7 C 0.44052(17) 0.83712(11) 0.43381(11) 0.0536(5) Uani 1 1 d . . . . .
C38 C 0.34460(18) 0.79514(10) 0.67315(11) 0.0551(5) Uani 1 1 d . . . . .
C83 C 1.00532(17) 0.38601(11) 0.80003(10) 0.0539(5) Uani 1 1 d . . . . .
C47 C 0.84081(17) 0.39385(10) 0.52532(10) 0.0540(5) Uani 1 1 d D . . . .
C8 C 0.50908(17) 0.77193(11) 0.41206(10) 0.0532(5) Uani 1 1 d . . . . .
H8 H 0.521884 0.764964 0.364228 0.064 Uiso 1 1 calc R U . . .
C22 C 0.58509(18) 0.62046(12) 0.83486(10) 0.0579(5) Uani 1 1 d . . . . .
H22 H 0.565512 0.630793 0.881791 0.070 Uiso 1 1 calc R U . . .
C36 C 0.55736(19) 0.80952(10) 0.66198(12) 0.0576(5) Uani 1 1 d . . . . .
C28 C 0.85488(17) 0.60729(11) 0.69882(11) 0.0553(5) Uani 1 1 d . . . . .
H28 H 0.876966 0.597883 0.651780 0.066 Uiso 1 1 calc R U . . .
C63 C 1.03244(17) 0.16292(12) 0.70371(11) 0.0568(5) Uani 1 1 d . . . . .
H63 H 1.061216 0.198055 0.668885 0.068 Uiso 1 1 calc R U . . .
C74 C 0.70022(19) 0.39286(11) 0.97522(11) 0.0589(5) Uani 1 1 d . . . . .
H74 H 0.691826 0.444861 0.970747 0.071 Uiso 1 1 calc R U . . .
C94 C 0.72506(17) 0.26723(11) 0.76827(11) 0.0565(5) Uani 1 1 d . . . . .
H94 H 0.739685 0.216932 0.759931 0.068 Uiso 1 1 calc R U . . .
C61 C 1.01145(17) 0.03708(11) 0.74534(11) 0.0569(5) Uani 1 1 d . . . . .
H61 H 1.026507 -0.013600 0.738514 0.068 Uiso 1 1 calc R U . . .
C82 C 0.88839(18) 0.42060(11) 0.80038(11) 0.0565(5) Uani 1 1 d . . . . .
H82 H 0.871377 0.471298 0.806963 0.068 Uiso 1 1 calc R U . . .
C87 C 1.15116(17) 0.27258(13) 0.79566(11) 0.0589(5) Uani 1 1 d . . . . .
H87 H 1.170191 0.221518 0.791240 0.071 Uiso 1 1 calc R U . . .
C62 C 1.05655(18) 0.08750(12) 0.69192(11) 0.0606(5) Uani 1 1 d . . . . .
C77 C 0.94033(18) 0.23481(13) 1.00027(12) 0.0642(5) Uani 1 1 d . . . . .
H77 H 0.952362 0.182815 1.002857 0.077 Uiso 1 1 calc R U . . .
C92 C 0.58686(18) 0.37952(13) 0.78268(12) 0.0635(6) Uani 1 1 d . . . . .
H92 H 0.508926 0.403749 0.783611 0.076 Uiso 1 1 calc R U . . .
C95 C 0.64232(18) -0.01827(12) 1.10578(11) 0.0610(5) Uani 1 1 d D . . . .
C20 C 0.37441(19) 0.60548(13) 0.83148(12) 0.0653(6) Uani 1 1 d . . . . .
H20 H 0.354091 0.616541 0.878182 0.078 Uiso 1 1 calc R U . . .
C18 C 0.31787(18) 0.57299(13) 0.72562(13) 0.0656(6) Uani 1 1 d . . . . .
H18 H 0.258204 0.562368 0.701559 0.079 Uiso 1 1 calc R U . . .
C29 C 0.3373(2) 0.79586(12) 0.74872(12) 0.0668(6) Uani 1 1 d . U . . .
C43 C 0.38072(19) 0.89608(12) 0.38272(12) 0.0644(5) Uani 1 1 d D U . . .
C27 C 0.93862(18) 0.62352(12) 0.73593(13) 0.0650(6) Uani 1 1 d . . . . .
H27 H 1.016817 0.625566 0.713881 0.078 Uiso 1 1 calc R U . . .
C25 C 0.7949(2) 0.63638(13) 0.83952(12) 0.0667(6) Uani 1 1 d . . . . .
H25 H 0.776037 0.646196 0.886609 0.080 Uiso 1 1 calc R U . . .
C72 C 0.4884(2) 0.39794(13) 0.96149(12) 0.0688(6) Uani 1 1 d . . . . .
H72 H 0.479956 0.449949 0.957287 0.083 Uiso 1 1 calc R U . . .
C35 C 0.67085(19) 0.81748(12) 0.62143(14) 0.0700(6) Uani 1 1 d . U . . .
H35 H 0.677789 0.820072 0.572530 0.084 Uiso 1 1 calc R U . . .
C93 C 0.61217(18) 0.30345(13) 0.77013(12) 0.0658(6) Uani 1 1 d . . . . .
H93 H 0.550525 0.277724 0.763020 0.079 Uiso 1 1 calc R U . . .
C86 C 1.23705(19) 0.31287(15) 0.80712(12) 0.0724(6) Uani 1 1 d . . . . .
H86 H 1.313937 0.288824 0.811022 0.087 Uiso 1 1 calc R U . . .
C39 C 0.24007(19) 0.78621(12) 0.64480(14) 0.0679(6) Uani 1 1 d . . . . .
H39 H 0.243736 0.784064 0.596486 0.081 Uiso 1 1 calc R U . . .
C19 C 0.28890(19) 0.59009(14) 0.79631(13) 0.0715(6) Uani 1 1 d . . . . .
H19 H 0.210397 0.590707 0.818665 0.086 Uiso 1 1 calc R U . . .
C69 C 0.51197(18) 0.24285(13) 0.97090(12) 0.0657(6) Uani 1 1 d . . . . .
H69 H 0.517881 0.190991 0.972922 0.079 Uiso 1 1 calc R U . . .
C84 C 1.0999(2) 0.42554(14) 0.81003(13) 0.0716(6) Uani 1 1 d . . . . .
H84 H 1.084135 0.476715 0.814454 0.086 Uiso 1 1 calc R U . . .
C26 C 0.9087(2) 0.63732(14) 0.80749(13) 0.0717(6) Uani 1 1 d . . . . .
H26 H 0.967488 0.647095 0.832675 0.086 Uiso 1 1 calc R U . . .
C31 C 0.5494(2) 0.80755(13) 0.73681(13) 0.0689(6) Uani 1 1 d . U . . .
C85 C 1.2118(2) 0.39058(15) 0.81322(14) 0.0776(7) Uani 1 1 d . . . . .
H85 H 1.272387 0.417606 0.819455 0.093 Uiso 1 1 calc R U . . .
C99 C 1.1315(2) 0.06092(16) 0.62373(13) 0.0807(7) Uani 1 1 d D . . . .
C71 C 0.3932(2) 0.36343(16) 0.95811(13) 0.0797(7) Uani 1 1 d . . . . .
H71 H 0.319376 0.391328 0.952895 0.096 Uiso 1 1 calc R U . . .
C80 C 0.9116(2) 0.38969(14) 0.99153(13) 0.0763(7) Uani 1 1 d . . . . .
H80 H 0.903404 0.441665 0.988445 0.092 Uiso 1 1 calc R U . . .
C30 C 0.4400(2) 0.80027(14) 0.77715(14) 0.0784(7) Uani 1 1 d . U . . .
H30 H 0.435225 0.798234 0.825933 0.094 Uiso 1 1 calc R U . . .
C52 C 0.7566(2) 0.67174(14) 0.39062(13) 0.0823(8) Uani 1 1 d . . . . .
H52A H 0.737711 0.707215 0.351947 0.124 Uiso 1 1 calc R U . . .
H52B H 0.807783 0.629066 0.372865 0.124 Uiso 1 1 calc R U . . .
H52C H 0.796977 0.694581 0.421334 0.124 Uiso 1 1 calc R U . . .
C78 C 1.0327(2) 0.27201(16) 1.00603(15) 0.0824(7) Uani 1 1 d . . . . .
H78 H 1.106678 0.245362 1.013044 0.099 Uiso 1 1 calc R U . . .
C51 C 0.5756(3) 0.60843(14) 0.38443(13) 0.0860(8) Uani 1 1 d . . . . .
H51A H 0.507643 0.588517 0.411824 0.129 Uiso 1 1 calc R U . . .
H51B H 0.629776 0.568545 0.363725 0.129 Uiso 1 1 calc R U . . .
H51C H 0.548996 0.644264 0.347812 0.129 Uiso 1 1 calc R U . . .
C70 C 0.4053(2) 0.28478(16) 0.96247(14) 0.0790(7) Uani 1 1 d . . . . .
H70 H 0.339155 0.261095 0.959525 0.095 Uiso 1 1 calc R U . . .
C42 C 0.2237(3) 0.79046(15) 0.79025(16) 0.0897(8) Uani 1 1 d . . . . .
H42 H 0.216937 0.791448 0.838871 0.108 Uiso 1 1 calc R U . . .
C40 C 0.1341(2) 0.78072(14) 0.68780(17) 0.0848(8) Uani 1 1 d . . . . .
H40 H 0.066215 0.774757 0.668529 0.102 Uiso 1 1 calc R U . . .
C41 C 0.1265(3) 0.78402(15) 0.76140(18) 0.0950(9) Uani 1 1 d . . . . .
H41 H 0.053267 0.781691 0.789934 0.114 Uiso 1 1 calc R U . . .
C79 C 1.0179(2) 0.35056(17) 1.00151(15) 0.0885(8) Uani 1 1 d . . . . .
H79 H 1.082194 0.375555 1.005452 0.106 Uiso 1 1 calc R U . . .
C34 C 0.7690(2) 0.82139(15) 0.65196(19) 0.0905(8) Uani 1 1 d . U . . .
H34 H 0.841911 0.826434 0.623871 0.109 Uiso 1 1 calc R U . . .
C104 C 0.8163(3) -0.04325(16) 0.83244(15) 0.0973(9) Uani 1 1 d . . . . .
H10A H 0.786123 -0.080594 0.867052 0.146 Uiso 1 1 calc R U . . .
H10B H 0.862414 -0.067040 0.793034 0.146 Uiso 1 1 calc R U . . .
H10C H 0.750372 -0.009766 0.816755 0.146 Uiso 1 1 calc R U . . .
C46 C 0.4274(5) 0.8828(3) 0.3041(3) 0.0709(13) Uani 0.655(12) 1 d D U P A 1
H46A H 0.512774 0.882788 0.295572 0.106 Uiso 0.655(12) 1 calc R U P A 1
H46B H 0.390016 0.922055 0.274055 0.106 Uiso 0.655(12) 1 calc R U P A 1
H46C H 0.408230 0.835497 0.294201 0.106 Uiso 0.655(12) 1 calc R U P A 1
C103 C 1.0011(2) -0.05190(15) 0.89158(16) 0.0960(10) Uani 1 1 d . . . . .
H10D H 1.047826 -0.024167 0.914351 0.144 Uiso 1 1 calc R U . . .
H10E H 1.050702 -0.074116 0.852355 0.144 Uiso 1 1 calc R U . . .
H10F H 0.970543 -0.090481 0.924531 0.144 Uiso 1 1 calc R U . . .
C32 C 0.6559(3) 0.81185(15) 0.76669(17) 0.0940(9) Uani 1 1 d . U . . .
H32 H 0.652300 0.810429 0.815369 0.113 Uiso 1 1 calc R U . . .
C33 C 0.7619(3) 0.81796(17) 0.7250(2) 0.1022(10) Uani 1 1 d . U . . .
H33 H 0.830420 0.819863 0.745287 0.123 Uiso 1 1 calc R U . . .
C100 C 1.0619(8) 0.0057(7) 0.5950(6) 0.129(4) Uani 0.510(9) 1 d D U P B 1
H10G H 1.111581 -0.017496 0.556360 0.194 Uiso 0.510(9) 1 calc R U P B 1
H10H H 0.990443 0.032537 0.579062 0.194 Uiso 0.510(9) 1 calc R U P B 1
H10I H 1.040509 -0.032035 0.631793 0.194 Uiso 0.510(9) 1 calc R U P B 1
C101 C 1.2414(5) 0.0030(5) 0.6476(4) 0.096(2) Uani 0.510(9) 1 d D U P B 1
H10J H 1.211122 -0.039223 0.675333 0.145 Uiso 0.510(9) 1 calc R U P B 1
H10K H 1.285531 0.027181 0.675250 0.145 Uiso 0.510(9) 1 calc R U P B 1
H10L H 1.293260 -0.013653 0.606633 0.145 Uiso 0.510(9) 1 calc R U P B 1
C102 C 1.1782(14) 0.1179(5) 0.5743(6) 0.179(7) Uani 0.510(9) 1 d D U P B 1
H10M H 1.234219 0.095062 0.537836 0.268 Uiso 0.510(9) 1 calc R U P B 1
H10N H 1.217969 0.148865 0.598091 0.268 Uiso 0.510(9) 1 calc R U P B 1
H10O H 1.113560 0.147998 0.553746 0.268 Uiso 0.510(9) 1 calc R U P B 1
C97 C 0.6903(5) -0.0069(3) 1.1716(2) 0.104(2) Uani 0.681(7) 1 d D U P C 1
H97A H 0.775246 -0.022502 1.166217 0.156 Uiso 0.681(7) 1 calc R U P C 1
H97B H 0.651867 -0.035972 1.210876 0.156 Uiso 0.681(7) 1 calc R U P C 1
H97C H 0.674679 0.045100 1.179999 0.156 Uiso 0.681(7) 1 calc R U P C 1
C48 C 0.8693(6) 0.3471(3) 0.5917(2) 0.091(2) Uani 0.592(8) 1 d D U P D 1
H48A H 0.911103 0.299237 0.579764 0.137 Uiso 0.592(8) 1 calc R U P D 1
H48B H 0.796148 0.340131 0.622265 0.137 Uiso 0.592(8) 1 calc R U P D 1
H48C H 0.918810 0.372020 0.615175 0.137 Uiso 0.592(8) 1 calc R U P D 1
C49 C 0.9581(5) 0.4031(3) 0.4773(4) 0.103(3) Uani 0.592(8) 1 d D U P D 1
H49A H 1.007796 0.427910 0.500853 0.155 Uiso 0.592(8) 1 calc R U P D 1
H49B H 0.941423 0.432486 0.434606 0.155 Uiso 0.592(8) 1 calc R U P D 1
H49C H 0.998902 0.354803 0.466286 0.155 Uiso 0.592(8) 1 calc R U P D 1
C98 C 0.6642(6) -0.1012(2) 1.0935(3) 0.115(2) Uani 0.681(7) 1 d D U P C 1
H98A H 0.632550 -0.108494 1.051625 0.172 Uiso 0.681(7) 1 calc R U P C 1
H98B H 0.624912 -0.129334 1.133147 0.172 Uiso 0.681(7) 1 calc R U P C 1
H98C H 0.748721 -0.117934 1.087979 0.172 Uiso 0.681(7) 1 calc R U P C 1
C50 C 0.7657(5) 0.3503(3) 0.4890(4) 0.109(3) Uani 0.592(8) 1 d D U P D 1
H50A H 0.807216 0.301060 0.482417 0.163 Uiso 0.592(8) 1 calc R U P D 1
H50B H 0.752934 0.375966 0.443992 0.163 Uiso 0.592(8) 1 calc R U P D 1
H50C H 0.689758 0.346554 0.517743 0.163 Uiso 0.592(8) 1 calc R U P D 1
C45 C 0.4083(6) 0.9749(2) 0.3946(3) 0.0814(15) Uani 0.655(12) 1 d D U P A 1
H45A H 0.376564 0.986168 0.441964 0.122 Uiso 0.655(12) 1 calc R U P A 1
H45B H 0.371808 1.011625 0.361953 0.122 Uiso 0.655(12) 1 calc R U P A 1
H45C H 0.493444 0.975733 0.387336 0.122 Uiso 0.655(12) 1 calc R U P A 1
C44 C 0.2494(4) 0.8956(4) 0.3957(3) 0.0908(17) Uani 0.655(12) 1 d D U P A 1
H44A H 0.230822 0.847887 0.386619 0.136 Uiso 0.655(12) 1 calc R U P A 1
H44B H 0.211828 0.934173 0.365120 0.136 Uiso 0.655(12) 1 calc R U P A 1
H44C H 0.220265 0.904604 0.443941 0.136 Uiso 0.655(12) 1 calc R U P A 1
C96 C 0.5085(3) 0.0069(4) 1.1144(3) 0.109(2) Uani 0.681(7) 1 d D U P C 1
H96A H 0.493449 0.058980 1.122412 0.163 Uiso 0.681(7) 1 calc R U P C 1
H96B H 0.469815 -0.021803 1.153804 0.163 Uiso 0.681(7) 1 calc R U P C 1
H96C H 0.477504 -0.000512 1.072343 0.163 Uiso 0.681(7) 1 calc R U P C 1
C98A C 0.7357(8) -0.0795(7) 1.1340(7) 0.109(5) Uani 0.319(7) 1 d D U P C 2
H98D H 0.774193 -0.109065 1.096443 0.163 Uiso 0.319(7) 1 calc R U P C 2
H98E H 0.696590 -0.110875 1.171017 0.163 Uiso 0.319(7) 1 calc R U P C 2
H98F H 0.794559 -0.056629 1.151987 0.163 Uiso 0.319(7) 1 calc R U P C 2
C96A C 0.5468(10) -0.0569(7) 1.0821(5) 0.102(4) Uani 0.319(7) 1 d D U P C 2
H96D H 0.489564 -0.020098 1.061677 0.153 Uiso 0.319(7) 1 calc R U P C 2
H96E H 0.506659 -0.084260 1.122025 0.153 Uiso 0.319(7) 1 calc R U P C 2
H96F H 0.583779 -0.090815 1.047729 0.153 Uiso 0.319(7) 1 calc R U P C 2
C97A C 0.5825(14) 0.0270(5) 1.1669(5) 0.113(5) Uani 0.319(7) 1 d D U P C 2
H97D H 0.640714 0.052324 1.182664 0.170 Uiso 0.319(7) 1 calc R U P C 2
H97E H 0.549712 -0.006021 1.204948 0.170 Uiso 0.319(7) 1 calc R U P C 2
H97F H 0.519280 0.063059 1.151490 0.170 Uiso 0.319(7) 1 calc R U P C 2
C50A C 0.8759(10) 0.3836(4) 0.4473(4) 0.103(4) Uani 0.408(8) 1 d D U P D 2
H50D H 0.922644 0.422081 0.425590 0.154 Uiso 0.408(8) 1 calc R U P D 2
H50E H 0.804920 0.386621 0.425302 0.154 Uiso 0.408(8) 1 calc R U P D 2
H50F H 0.922429 0.335496 0.441711 0.154 Uiso 0.408(8) 1 calc R U P D 2
C49A C 0.9531(8) 0.3846(5) 0.5617(7) 0.122(4) Uani 0.408(8) 1 d D U P D 2
H49D H 0.930399 0.392414 0.610659 0.182 Uiso 0.408(8) 1 calc R U P D 2
H49E H 1.004635 0.420523 0.539882 0.182 Uiso 0.408(8) 1 calc R U P D 2
H49F H 0.994658 0.334998 0.557281 0.182 Uiso 0.408(8) 1 calc R U P D 2
C48A C 0.7637(8) 0.3345(4) 0.5580(6) 0.108(4) Uani 0.408(8) 1 d D U P D 2
H48D H 0.808272 0.285851 0.552189 0.162 Uiso 0.408(8) 1 calc R U P D 2
H48E H 0.693283 0.339281 0.535142 0.162 Uiso 0.408(8) 1 calc R U P D 2
H48F H 0.740600 0.340484 0.607271 0.162 Uiso 0.408(8) 1 calc R U P D 2
C3 C 1.1141(14) -0.0132(6) 0.6056(7) 0.167(7) Uani 0.490(9) 1 d D U P B 2
H3A H 1.029918 -0.016999 0.610770 0.250 Uiso 0.490(9) 1 calc R U P B 2
H3B H 1.152064 -0.051245 0.636440 0.250 Uiso 0.490(9) 1 calc R U P B 2
H3C H 1.149053 -0.019579 0.557663 0.250 Uiso 0.490(9) 1 calc R U P B 2
C1A C 1.0867(7) 0.1145(5) 0.5598(3) 0.101(3) Uani 0.490(9) 1 d D U P B 2
H1AA H 1.130799 0.098447 0.516240 0.151 Uiso 0.490(9) 1 calc R U P B 2
H1AB H 1.099453 0.164835 0.564562 0.151 Uiso 0.490(9) 1 calc R U P B 2
H1AC H 1.002821 0.112730 0.559731 0.151 Uiso 0.490(9) 1 calc R U P B 2
C1B C 1.2578(5) 0.0744(9) 0.6215(5) 0.149(5) Uani 0.490(9) 1 d D U P B 2
H1BA H 1.293179 0.042783 0.658058 0.224 Uiso 0.490(9) 1 calc R U P B 2
H1BB H 1.259703 0.125877 0.628480 0.224 Uiso 0.490(9) 1 calc R U P B 2
H1BC H 1.302099 0.063424 0.576463 0.224 Uiso 0.490(9) 1 calc R U P B 2
C46A C 0.2543(7) 0.8650(6) 0.3755(5) 0.070(3) Uani 0.345(12) 1 d D U P A 2
H46D H 0.271761 0.816845 0.357112 0.105 Uiso 0.345(12) 1 calc R U P A 2
H46E H 0.210768 0.899354 0.344091 0.105 Uiso 0.345(12) 1 calc R U P A 2
H46F H 0.206839 0.860669 0.421033 0.105 Uiso 0.345(12) 1 calc R U P A 2
C44A C 0.3455(13) 0.9710(5) 0.4093(6) 0.094(3) Uani 0.345(12) 1 d D U P A 2
H44D H 0.275473 0.969900 0.443942 0.141 Uiso 0.345(12) 1 calc R U P A 2
H44E H 0.328350 1.007200 0.370858 0.141 Uiso 0.345(12) 1 calc R U P A 2
H44F H 0.409995 0.984268 0.430302 0.141 Uiso 0.345(12) 1 calc R U P A 2
C45A C 0.4533(9) 0.9004(6) 0.3125(5) 0.075(3) Uani 0.345(12) 1 d D U P A 2
H45D H 0.532122 0.910731 0.316957 0.113 Uiso 0.345(12) 1 calc R U P A 2
H45E H 0.415888 0.939635 0.282516 0.113 Uiso 0.345(12) 1 calc R U P A 2
H45F H 0.459207 0.853586 0.292327 0.113 Uiso 0.345(12) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O3 C2 1.370(2) . ?
O3 C4 1.374(2) . ?
O66 C53 1.373(2) . ?
O66 C65 1.375(2) . ?
C2 C1 1.393(2) . ?
C2 C11 1.384(2) . ?
C1 C15 1.497(2) . ?
C1 C14 1.385(2) . ?
C11 C12 1.392(2) . ?
C11 C10 1.528(2) . ?
C15 C24 1.403(2) . ?
C15 C16 1.412(2) . ?
C4 C5 1.393(2) . ?
C4 C9 1.379(3) . ?
C67 C54 1.503(2) . ?
C67 C76 1.408(2) . ?
C67 C68 1.410(3) . ?
C53 C54 1.395(2) . ?
C53 C58 1.386(2) . ?
C54 C55 1.389(2) . ?
C13 C12 1.387(2) . ?
C13 C14 1.394(2) . ?
C13 C47 1.535(2) . ?
C89 C90 1.410(2) . ?
C89 C64 1.489(2) . ?
C89 C88 1.408(3) . ?
C65 C64 1.396(2) . ?
C65 C60 1.382(2) . ?
C90 C81 1.426(3) . ?
C90 C94 1.424(3) . ?
C81 C91 1.430(3) . ?
C81 C82 1.386(3) . ?
C24 C23 1.439(3) . ?
C24 C28 1.429(3) . ?
C64 C63 1.387(3) . ?
C88 C83 1.434(3) . ?
C88 C87 1.428(3) . ?
C58 C57 1.399(2) . ?
C58 C59 1.515(3) . ?
C16 C21 1.435(3) . ?
C16 C17 1.416(3) . ?
C5 C37 1.490(3) . ?
C5 C6 1.386(3) . ?
C76 C75 1.434(3) . ?
C76 C77 1.423(3) . ?
C9 C10 1.531(3) . ?
C9 C8 1.399(3) . ?
C56 C57 1.375(3) . ?
C56 C55 1.396(3) . ?
C56 C95 1.538(3) . ?
C23 C22 1.390(3) . ?
C23 C25 1.423(3) . ?
C37 C38 1.409(3) . ?
C37 C36 1.405(3) . ?
C60 C59 1.522(3) . ?
C60 C61 1.392(3) . ?
C10 C52 1.546(3) . ?
C10 C51 1.527(3) . ?
C21 C22 1.387(3) . ?
C21 C20 1.427(3) . ?
C73 C68 1.437(3) . ?
C73 C74 1.382(3) . ?
C73 C72 1.423(3) . ?
C68 C69 1.423(3) . ?
C75 C74 1.387(3) . ?
C75 C80 1.426(3) . ?
C91 C92 1.345(3) . ?
C17 C18 1.356(3) . ?
C59 C104 1.536(3) . ?
C59 C103 1.534(3) . ?
C6 C7 1.391(3) . ?
C7 C8 1.387(3) . ?
C7 C43 1.531(3) . ?
C38 C29 1.447(3) . ?
C38 C39 1.418(3) . ?
C83 C82 1.387(3) . ?
C83 C84 1.423(3) . ?
C47 C48 1.508(5) . ?
C47 C49 1.523(5) . ?
C47 C50 1.528(5) . ?
C47 C50A 1.520(7) . ?
C47 C49A 1.528(7) . ?
C47 C48A 1.511(7) . ?
C36 C35 1.422(3) . ?
C36 C31 1.427(3) . ?
C28 C27 1.356(3) . ?
C63 C62 1.392(3) . ?
C94 C93 1.354(3) . ?
C61 C62 1.390(3) . ?
C87 C86 1.357(3) . ?
C62 C99 1.537(3) . ?
C77 C78 1.351(3) . ?
C92 C93 1.407(3) . ?
C95 C97 1.500(5) . ?
C95 C98 1.526(5) . ?
C95 C96 1.515(5) . ?
C95 C98A 1.537(8) . ?
C95 C96A 1.523(8) . ?
C95 C97A 1.524(9) . ?
C20 C19 1.342(3) . ?
C18 C19 1.408(3) . ?
C29 C30 1.379(3) . ?
C29 C42 1.424(3) . ?
C43 C46 1.559(5) . ?
C43 C45 1.554(5) . ?
C43 C44 1.478(5) . ?
C43 C46A 1.648(8) . ?
C43 C44A 1.482(9) . ?
C43 C45A 1.475(10) . ?
C27 C26 1.409(3) . ?
C25 C26 1.349(3) . ?
C72 C71 1.339(3) . ?
C35 C34 1.352(3) . ?
C86 C85 1.411(4) . ?
C39 C40 1.366(3) . ?
C69 C70 1.359(3) . ?
C84 C85 1.345(3) . ?
C31 C30 1.379(3) . ?
C31 C32 1.434(4) . ?
C99 C100 1.554(10) . ?
C99 C101 1.604(7) . ?
C99 C102 1.432(8) . ?
C99 C3 1.470(11) . ?
C99 C1A 1.586(7) . ?
C99 C1B 1.486(8) . ?
C71 C70 1.408(4) . ?
C80 C79 1.341(4) . ?
C78 C79 1.405(4) . ?
C42 C41 1.335(4) . ?
C40 C41 1.414(4) . ?
C34 C33 1.392(4) . ?
C32 C33 1.356(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 O3 C4 119.21(14) . . ?
C53 O66 C65 119.11(13) . . ?
O3 C2 C1 114.16(15) . . ?
O3 C2 C11 123.37(15) . . ?
C11 C2 C1 122.47(16) . . ?
C2 C1 C15 120.57(15) . . ?
C14 C1 C2 117.93(16) . . ?
C14 C1 C15 121.50(15) . . ?
C2 C11 C12 116.94(16) . . ?
C2 C11 C10 121.53(15) . . ?
C12 C11 C10 121.48(16) . . ?
C24 C15 C1 120.30(15) . . ?
C24 C15 C16 120.18(16) . . ?
C16 C15 C1 119.49(15) . . ?
O3 C4 C5 113.92(16) . . ?
O3 C4 C9 123.20(16) . . ?
C9 C4 C5 122.87(17) . . ?
C76 C67 C54 120.39(15) . . ?
C76 C67 C68 119.77(16) . . ?
C68 C67 C54 119.81(16) . . ?
O66 C53 C54 114.67(15) . . ?
O66 C53 C58 122.66(16) . . ?
C58 C53 C54 122.67(16) . . ?
C53 C54 C67 120.29(15) . . ?
C55 C54 C67 122.15(16) . . ?
C55 C54 C53 117.56(16) . . ?
C12 C13 C14 116.97(16) . . ?
C12 C13 C47 121.53(16) . . ?
C14 C13 C47 121.49(17) . . ?
C90 C89 C64 119.69(16) . . ?
C88 C89 C90 120.06(17) . . ?
C88 C89 C64 120.22(15) . . ?
O66 C65 C64 114.00(15) . . ?
O66 C65 C60 123.56(16) . . ?
C60 C65 C64 122.44(17) . . ?
C89 C90 C81 119.68(16) . . ?
C89 C90 C94 122.55(17) . . ?
C94 C90 C81 117.76(16) . . ?
C90 C81 C91 118.73(17) . . ?
C82 C81 C90 119.47(16) . . ?
C82 C81 C91 121.81(18) . . ?
C13 C12 C11 123.37(16) . . ?
C15 C24 C23 119.88(16) . . ?
C15 C24 C28 122.87(17) . . ?
C28 C24 C23 117.25(17) . . ?
C65 C64 C89 119.76(16) . . ?
C63 C64 C89 122.22(17) . . ?
C63 C64 C65 118.01(17) . . ?
C89 C88 C83 119.50(16) . . ?
C89 C88 C87 122.68(18) . . ?
C87 C88 C83 117.80(18) . . ?
C1 C14 C13 122.31(17) . . ?
C53 C58 C57 116.60(17) . . ?
C53 C58 C59 122.40(16) . . ?
C57 C58 C59 120.99(16) . . ?
C15 C16 C21 119.43(16) . . ?
C15 C16 C17 122.81(17) . . ?
C17 C16 C21 117.75(16) . . ?
C4 C5 C37 118.62(16) . . ?
C6 C5 C4 117.80(18) . . ?
C6 C5 C37 123.57(17) . . ?
C67 C76 C75 119.97(16) . . ?
C67 C76 C77 122.64(18) . . ?
C77 C76 C75 117.39(17) . . ?
C4 C9 C10 121.77(16) . . ?
C4 C9 C8 116.69(17) . . ?
C8 C9 C10 121.50(17) . . ?
C57 C56 C55 117.03(17) . . ?
C57 C56 C95 122.15(17) . . ?
C55 C56 C95 120.82(18) . . ?
C22 C23 C24 119.02(17) . . ?
C22 C23 C25 122.11(19) . . ?
C25 C23 C24 118.87(18) . . ?
C38 C37 C5 120.38(17) . . ?
C36 C37 C5 118.57(17) . . ?
C36 C37 C38 120.81(19) . . ?
C56 C57 C58 123.71(17) . . ?
C65 C60 C59 121.47(16) . . ?
C65 C60 C61 116.86(17) . . ?
C61 C60 C59 121.67(17) . . ?
C11 C10 C9 110.22(15) . . ?
C11 C10 C52 108.20(16) . . ?
C9 C10 C52 107.90(16) . . ?
C51 C10 C11 109.90(17) . . ?
C51 C10 C9 110.35(16) . . ?
C51 C10 C52 110.2(2) . . ?
C22 C21 C16 119.48(17) . . ?
C22 C21 C20 122.11(19) . . ?
C20 C21 C16 118.40(18) . . ?
C74 C73 C68 119.39(17) . . ?
C74 C73 C72 121.9(2) . . ?
C72 C73 C68 118.73(19) . . ?
C67 C68 C73 119.66(17) . . ?
C67 C68 C69 122.94(18) . . ?
C69 C68 C73 117.38(18) . . ?
C54 C55 C56 122.42(17) . . ?
C74 C75 C76 119.15(17) . . ?
C74 C75 C80 122.3(2) . . ?
C80 C75 C76 118.54(19) . . ?
C92 C91 C81 121.2(2) . . ?
C18 C17 C16 121.52(19) . . ?
C58 C59 C60 110.73(15) . . ?
C58 C59 C104 109.74(16) . . ?
C58 C59 C103 108.71(18) . . ?
C60 C59 C104 108.12(19) . . ?
C60 C59 C103 109.35(16) . . ?
C103 C59 C104 110.2(2) . . ?
C5 C6 C7 122.25(18) . . ?
C6 C7 C43 120.14(18) . . ?
C8 C7 C6 117.21(17) . . ?
C8 C7 C43 122.61(19) . . ?
C37 C38 C29 118.43(19) . . ?
C37 C38 C39 123.0(2) . . ?
C39 C38 C29 118.55(19) . . ?
C82 C83 C88 119.24(17) . . ?
C82 C83 C84 122.0(2) . . ?
C84 C83 C88 118.73(19) . . ?
C48 C47 C13 113.5(2) . . ?
C48 C47 C49 108.4(4) . . ?
C48 C47 C50 107.1(4) . . ?
C49 C47 C13 109.6(2) . . ?
C49 C47 C50 108.9(4) . . ?
C50 C47 C13 109.2(2) . . ?
C50A C47 C13 112.8(3) . . ?
C50A C47 C49A 109.9(6) . . ?
C49A C47 C13 107.9(3) . . ?
C48A C47 C13 108.9(3) . . ?
C48A C47 C50A 108.7(6) . . ?
C48A C47 C49A 108.7(6) . . ?
C7 C8 C9 123.18(19) . . ?
C21 C22 C23 121.96(18) . . ?
C37 C36 C35 122.5(2) . . ?
C37 C36 C31 119.9(2) . . ?
C35 C36 C31 117.5(2) . . ?
C27 C28 C24 121.5(2) . . ?
C64 C63 C62 122.27(19) . . ?
C73 C74 C75 122.02(18) . . ?
C93 C94 C90 121.3(2) . . ?
C62 C61 C60 123.61(18) . . ?
C81 C82 C83 121.95(18) . . ?
C86 C87 C88 120.7(2) . . ?
C63 C62 C99 121.7(2) . . ?
C61 C62 C63 116.81(18) . . ?
C61 C62 C99 121.5(2) . . ?
C78 C77 C76 121.7(2) . . ?
C91 C92 C93 120.14(19) . . ?
C97 C95 C56 109.6(2) . . ?
C97 C95 C98 109.5(4) . . ?
C97 C95 C96 109.3(4) . . ?
C98 C95 C56 111.3(2) . . ?
C96 C95 C56 108.5(2) . . ?
C96 C95 C98 108.6(4) . . ?
C98A C95 C56 110.0(4) . . ?
C96A C95 C56 109.9(4) . . ?
C96A C95 C98A 107.6(7) . . ?
C96A C95 C97A 107.7(7) . . ?
C97A C95 C56 113.5(4) . . ?
C97A C95 C98A 107.9(8) . . ?
C19 C20 C21 121.6(2) . . ?
C17 C18 C19 120.7(2) . . ?
C30 C29 C38 119.0(2) . . ?
C30 C29 C42 123.2(3) . . ?
C42 C29 C38 117.7(2) . . ?
C7 C43 C46 112.3(2) . . ?
C7 C43 C45 109.7(2) . . ?
C7 C43 C46A 104.2(3) . . ?
C45 C43 C46 107.2(3) . . ?
C44 C43 C7 109.6(2) . . ?
C44 C43 C46 109.3(3) . . ?
C44 C43 C45 108.5(3) . . ?
C44A C43 C7 114.7(4) . . ?
C44A C43 C46A 105.7(5) . . ?
C45A C43 C7 111.4(4) . . ?
C45A C43 C46A 108.4(5) . . ?
C45A C43 C44A 111.7(6) . . ?
C28 C27 C26 120.8(2) . . ?
C26 C25 C23 121.5(2) . . ?
C71 C72 C73 121.8(2) . . ?
C34 C35 C36 121.9(3) . . ?
C94 C93 C92 120.9(2) . . ?
C87 C86 C85 121.2(2) . . ?
C40 C39 C38 120.6(2) . . ?
C20 C19 C18 120.11(19) . . ?
C70 C69 C68 121.1(2) . . ?
C85 C84 C83 121.5(2) . . ?
C25 C26 C27 120.1(2) . . ?
C36 C31 C32 118.5(2) . . ?
C30 C31 C36 118.5(2) . . ?
C30 C31 C32 123.0(3) . . ?
C84 C85 C86 120.0(2) . . ?
C62 C99 C100 107.6(4) . . ?
C62 C99 C101 106.2(3) . . ?
C62 C99 C1A 107.6(3) . . ?
C100 C99 C101 99.3(5) . . ?
C102 C99 C62 116.2(4) . . ?
C102 C99 C100 117.0(8) . . ?
C102 C99 C101 108.8(6) . . ?
C3 C99 C62 115.9(5) . . ?
C3 C99 C1A 102.3(7) . . ?
C3 C99 C1B 116.1(7) . . ?
C1B C99 C62 109.7(4) . . ?
C1B C99 C1A 103.8(6) . . ?
C72 C71 C70 119.8(2) . . ?
C79 C80 C75 121.5(2) . . ?
C29 C30 C31 123.2(2) . . ?
C77 C78 C79 120.6(2) . . ?
C69 C70 C71 121.1(2) . . ?
C41 C42 C29 121.9(3) . . ?
C39 C40 C41 120.6(3) . . ?
C42 C41 C40 120.6(2) . . ?
C80 C79 C78 120.3(2) . . ?
C35 C34 C33 120.7(3) . . ?
C33 C32 C31 120.9(3) . . ?
C32 C33 C34 120.5(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.287
_oxdiff_exptl_absorpt_empirical_full_min 0.374
####################################################################### 
# 
# 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_t
_database_code_depnum_ccdc_archive 'CCDC 2180355'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2022-06-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2019-11-15
_audit_creation_method           
; 
Olex2 1.2 
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) 
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C51 H46 O, C H2 Cl2'
_chemical_formula_sum            'C52 H48 Cl2 O'
_chemical_formula_weight         759.80
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.819(3)
_cell_length_b                   13.093(3)
_cell_length_c                   14.822(3)
_cell_angle_alpha                93.696(5)
_cell_angle_beta                 114.031(4)
_cell_angle_gamma                108.413(5)
_cell_volume                     2101.6(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4142
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      26.65
_cell_measurement_theta_min      2.21
_shelx_estimated_absorpt_T_max   0.996
_shelx_estimated_absorpt_T_min   0.981
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Bruker,2008)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1221
_diffrn_reflns_av_unetI/netI     0.0988
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29916
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.543
_diffrn_ambient_temperature      290(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3306
_reflns_number_total             7408
_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 v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7408
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.1634
_refine_ls_R_factor_gt           0.0812
_refine_ls_restrained_S_all      1.117
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2050
_refine_ls_wR_factor_ref         0.2373
_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. Restrained distances 
 Cl2-C1S' = Cl1'-C1S' 
 1.73 with sigma of 0.01 
 Cl2-C1S' \\sim Cl2'-C1S 
 with sigma of 0.02 
 Cl1'-C1S' \\sim Cl1-C1S 
 with sigma of 0.02 
 Cl2-Cl1' \\sim Cl2'-Cl1 
 with sigma of 0.04 
 Cl1'-C1S' \\sim Cl1-C1S \\sim Cl2-C1S' \\sim Cl2'-C1S 
 with sigma of 0.01 
 Cl2'-Cl1 \\sim Cl1'-Cl2 
 with sigma of 0.01 
3. Uiso/Uaniso restraints and constraints 
Uanis(Cl1) \\sim Ueq, Uanis(C1S) \\sim Ueq, Uanis(Cl2') \\sim Ueq, Uanis(C1S') 
\\sim Ueq, Uanis(Cl1') \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C15) \\sim Ueq: 
with sigma of 0.01 and sigma for terminal atoms of 0.02 
4. Others 
 Sof(C1S)=Sof(H1SC)=Sof(H1SD)=Sof(Cl1)=Sof(Cl2')=1-FVAR(1) 
 Sof(C1S')=Sof(H1SA)=Sof(H1SB)=Sof(Cl1')=Sof(Cl2)=FVAR(1) 
5.a Secondary CH2 refined with riding coordinates: 
 C1S'(H1SA,H1SB), C1S(H1SC,H1SD) 
5.b Aromatic/amide H refined with riding coordinates: 
 C2(H2), C6(H6), C11(H11), C13(H13), C26(H26), C27(H27), C28(H28), C29(H29), 
 C31(H31), C34(H34), C35(H35), C36(H36), C37(H37), C40(H40), C41(H41), C42(H42), 
  C43(H43), C45(H45), C48(H48), C49(H49), C50(H50), C51(H51) 
5.c Idealised Me refined as rotating group: 
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B, 
 H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A, 
 H23B,H23C) 
;
_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
C1 C 0.4985(3) 0.1699(3) 0.1870(3) 0.0349(9) Uani 1 1 d . . . . .
C2 C 0.4945(3) 0.2515(3) 0.2490(3) 0.0351(9) Uani 1 1 d . . . . .
H2 H 0.4384 0.2312 0.2755 0.042 Uiso 1 1 calc R . . . .
C3 C 0.5707(3) 0.3623(3) 0.2731(2) 0.0289(8) Uani 1 1 d . . . . .
C4 C 0.6541(3) 0.3906(2) 0.2338(2) 0.0297(8) Uani 1 1 d . . . . .
C5 C 0.6622(3) 0.3120(3) 0.1716(3) 0.0324(8) Uani 1 1 d . . . . .
C6 C 0.5839(3) 0.2032(3) 0.1499(3) 0.0368(9) Uani 1 1 d . . . . .
H6 H 0.5890 0.1503 0.1086 0.044 Uiso 1 1 calc R . . . .
C7 C 0.5605(3) 0.4468(3) 0.3409(3) 0.0301(8) Uani 1 1 d . . . . .
C8 C 0.6527(3) 0.5612(3) 0.3564(2) 0.0291(8) Uani 1 1 d . . . . .
C9 C 0.7331(3) 0.5804(3) 0.3136(2) 0.0304(8) Uani 1 1 d . . . . .
C10 C 0.8184(3) 0.6851(3) 0.3292(3) 0.0326(8) Uani 1 1 d . . . . .
C11 C 0.8213(3) 0.7727(3) 0.3900(3) 0.0381(9) Uani 1 1 d . . . . .
H11 H 0.8779 0.8431 0.4009 0.046 Uiso 1 1 calc R . . . .
C12 C 0.7430(3) 0.7590(3) 0.4349(3) 0.0344(9) Uani 1 1 d . . . . .
C13 C 0.6601(3) 0.6522(3) 0.4166(3) 0.0356(9) Uani 1 1 d . . . . .
H13 H 0.6069 0.6408 0.4461 0.043 Uiso 1 1 calc R . . . .
C14 C 0.4137(4) 0.0487(3) 0.1644(3) 0.0486(10) Uani 1 1 d . . . . .
C15 C 0.4516(7) 0.0054(4) 0.2574(5) 0.152(3) Uani 1 1 d . U . . .
H15A H 0.5327 0.0049 0.2773 0.228 Uiso 1 1 calc GR . . . .
H15B H 0.3945 -0.0684 0.2445 0.228 Uiso 1 1 calc GR . . . .
H15C H 0.4523 0.0517 0.3108 0.228 Uiso 1 1 calc GR . . . .
C16 C 0.2800(5) 0.0399(4) 0.1325(6) 0.122(2) Uani 1 1 d . . . . .
H16A H 0.2763 0.0787 0.1876 0.183 Uiso 1 1 calc GR . . . .
H16B H 0.2270 -0.0364 0.1154 0.183 Uiso 1 1 calc GR . . . .
H16C H 0.2536 0.0718 0.0748 0.183 Uiso 1 1 calc GR . . . .
C17 C 0.4098(6) -0.0219(4) 0.0800(5) 0.121(3) Uani 1 1 d . . . . .
H17A H 0.3842 0.0072 0.0203 0.181 Uiso 1 1 calc GR . . . .
H17B H 0.3524 -0.0956 0.0670 0.181 Uiso 1 1 calc GR . . . .
H17C H 0.4903 -0.0230 0.0981 0.181 Uiso 1 1 calc GR . . . .
C18 C 0.5894(4) 0.4162(3) 0.4450(3) 0.0453(10) Uani 1 1 d . . . . .
H18A H 0.5318 0.3439 0.4361 0.068 Uiso 1 1 calc GR . . . .
H18B H 0.5827 0.4690 0.4883 0.068 Uiso 1 1 calc GR . . . .
H18C H 0.6716 0.4167 0.4753 0.068 Uiso 1 1 calc GR . . . .
C19 C 0.4295(3) 0.4466(3) 0.2921(3) 0.0441(10) Uani 1 1 d . . . . .
H19A H 0.4126 0.4671 0.2281 0.066 Uiso 1 1 calc GR . . . .
H19B H 0.4224 0.4985 0.3359 0.066 Uiso 1 1 calc GR . . . .
H19C H 0.3715 0.3740 0.2818 0.066 Uiso 1 1 calc GR . . . .
C20 C 0.7465(4) 0.8549(3) 0.5021(3) 0.0476(10) Uani 1 1 d . . . . .
C21 C 0.7641(6) 0.8262(4) 0.6045(4) 0.104(2) Uani 1 1 d . . . . .
H21A H 0.6987 0.7585 0.5941 0.157 Uiso 1 1 calc GR . . . .
H21B H 0.7631 0.8845 0.6465 0.157 Uiso 1 1 calc GR . . . .
H21C H 0.8417 0.8177 0.6371 0.157 Uiso 1 1 calc GR . . . .
C22 C 0.6244(5) 0.8682(5) 0.4563(5) 0.125(3) Uani 1 1 d . . . . .
H22A H 0.6134 0.8944 0.3953 0.187 Uiso 1 1 calc GR . . . .
H22B H 0.6225 0.9204 0.5036 0.187 Uiso 1 1 calc GR . . . .
H22C H 0.5592 0.7983 0.4407 0.187 Uiso 1 1 calc GR . . . .
C23 C 0.8478(6) 0.9610(4) 0.5200(5) 0.120(3) Uani 1 1 d . . . . .
H23A H 0.9257 0.9533 0.5539 0.179 Uiso 1 1 calc GR . . . .
H23B H 0.8447 1.0184 0.5613 0.179 Uiso 1 1 calc GR . . . .
H23C H 0.8382 0.9796 0.4562 0.179 Uiso 1 1 calc GR . . . .
C24 C 0.7513(3) 0.3430(3) 0.1277(3) 0.0335(9) Uani 1 1 d . . . . .
C25 C 0.7076(3) 0.3375(3) 0.0231(3) 0.0352(9) Uani 1 1 d . . . . .
C26 C 0.5810(4) 0.3101(3) -0.0445(3) 0.0489(10) Uani 1 1 d . . . . .
H26 H 0.5239 0.2957 -0.0188 0.059 Uiso 1 1 calc R . . . .
C27 C 0.5414(4) 0.3042(3) -0.1456(3) 0.0594(12) Uani 1 1 d . . . . .
H27 H 0.4583 0.2864 -0.1882 0.071 Uiso 1 1 calc R . . . .
C28 C 0.6278(5) 0.3253(4) -0.1859(4) 0.0651(13) Uani 1 1 d . . . . .
H28 H 0.6005 0.3202 -0.2552 0.078 Uiso 1 1 calc R . . . .
C29 C 0.7465(5) 0.3521(3) -0.1259(3) 0.0579(12) Uani 1 1 d . . . . .
H29 H 0.8010 0.3662 -0.1542 0.069 Uiso 1 1 calc R . . . .
C30 C 0.7938(4) 0.3601(3) -0.0192(3) 0.0438(10) Uani 1 1 d . . . . .
C31 C 0.9172(4) 0.3866(3) 0.0436(3) 0.0490(11) Uani 1 1 d . . . . .
H31 H 0.9719 0.4004 0.0156 0.059 Uiso 1 1 calc R . . . .
C32 C 0.9624(4) 0.3933(3) 0.1468(3) 0.0466(10) Uani 1 1 d . . . . .
C33 C 0.8779(3) 0.3719(3) 0.1913(3) 0.0394(9) Uani 1 1 d . . . . .
C34 C 0.9287(4) 0.3793(3) 0.2975(3) 0.0550(11) Uani 1 1 d . . . . .
H34 H 0.8766 0.3662 0.3281 0.066 Uiso 1 1 calc R . . . .
C35 C 1.0497(4) 0.4047(4) 0.3549(4) 0.0727(14) Uani 1 1 d . . . . .
H35 H 1.0802 0.4102 0.4245 0.087 Uiso 1 1 calc R . . . .
C36 C 1.1311(4) 0.4233(4) 0.3107(4) 0.0819(16) Uani 1 1 d . . . . .
H36 H 1.2144 0.4391 0.3511 0.098 Uiso 1 1 calc R . . . .
C37 C 1.0891(4) 0.4182(4) 0.2110(4) 0.0671(13) Uani 1 1 d . . . . .
H37 H 1.1441 0.4313 0.1832 0.080 Uiso 1 1 calc R . . . .
C38 C 0.9083(3) 0.7063(2) 0.2859(3) 0.0342(9) Uani 1 1 d . . . . .
C39 C 1.0341(3) 0.7344(3) 0.3501(3) 0.0373(9) Uani 1 1 d . . . . .
C40 C 1.0810(4) 0.7332(3) 0.4553(3) 0.0507(11) Uani 1 1 d . . . . .
H40 H 1.0260 0.7117 0.4828 0.061 Uiso 1 1 calc R . . . .
C41 C 1.2032(4) 0.7624(3) 0.5165(3) 0.0605(12) Uani 1 1 d . . . . .
H41 H 1.2309 0.7609 0.5848 0.073 Uiso 1 1 calc R . . . .
C42 C 1.2879(4) 0.7951(4) 0.4762(4) 0.0637(13) Uani 1 1 d . . . . .
H42 H 1.3718 0.8165 0.5183 0.076 Uiso 1 1 calc R . . . .
C43 C 1.2485(4) 0.7957(3) 0.3777(4) 0.0561(11) Uani 1 1 d . . . . .
H43 H 1.3057 0.8156 0.3522 0.067 Uiso 1 1 calc R . . . .
C44 C 1.1215(3) 0.7665(3) 0.3109(3) 0.0411(10) Uani 1 1 d . . . . .
C45 C 1.0798(4) 0.7698(3) 0.2091(3) 0.0479(10) Uani 1 1 d . . . . .
H45 H 1.1370 0.7932 0.1840 0.057 Uiso 1 1 calc R . . . .
C46 C 0.9567(4) 0.7397(3) 0.1441(3) 0.0446(10) Uani 1 1 d . . . . .
C47 C 0.8675(3) 0.7055(3) 0.1816(3) 0.0386(9) Uani 1 1 d . . . . .
C48 C 0.7405(4) 0.6744(3) 0.1108(3) 0.0551(11) Uani 1 1 d . . . . .
H48 H 0.6805 0.6514 0.1332 0.066 Uiso 1 1 calc R . . . .
C49 C 0.7061(4) 0.6779(4) 0.0125(3) 0.0695(14) Uani 1 1 d . . . . .
H49 H 0.6229 0.6564 -0.0321 0.083 Uiso 1 1 calc R . . . .
C50 C 0.7948(5) 0.7137(4) -0.0235(3) 0.0722(14) Uani 1 1 d . . . . .
H50 H 0.7699 0.7169 -0.0912 0.087 Uiso 1 1 calc R . . . .
C51 C 0.9143(5) 0.7430(4) 0.0393(4) 0.0644(13) Uani 1 1 d . . . . .
H51 H 0.9716 0.7661 0.0142 0.077 Uiso 1 1 calc R . . . .
O1 O 0.7341(2) 0.49724(17) 0.25222(18) 0.0404(7) Uani 1 1 d . . . . .
C1S' C 0.8876(12) -0.0139(7) 0.1779(9) 0.128(5) Uani 0.605(11) 1 d D U P A 1
H1SA H 0.8253 -0.0732 0.1199 0.153 Uiso 0.605(11) 1 calc R . P A 1
H1SB H 0.9450 -0.0416 0.2248 0.153 Uiso 0.605(11) 1 calc R . P A 1
Cl1' Cl 0.8212(8) 0.0499(9) 0.2377(8) 0.255(4) Uani 0.605(11) 1 d D U P A 1
Cl2 Cl 0.9643(6) 0.1025(5) 0.1408(4) 0.240(6) Uani 0.605(11) 1 d D U P A 1
C1S C 0.8885(12) 0.0969(9) 0.1846(13) 0.095(5) Uani 0.395(11) 1 d D U P A 2
H1SC H 0.8394 0.1271 0.1331 0.114 Uiso 0.395(11) 1 calc R . P A 2
H1SD H 0.9436 0.1538 0.2461 0.114 Uiso 0.395(11) 1 calc R . P A 2
Cl1 Cl 0.7942(12) -0.0244(10) 0.2071(10) 0.214(5) Uani 0.395(11) 1 d D U P A 2
Cl2' Cl 0.9700(8) 0.0323(8) 0.1405(7) 0.212(8) Uani 0.395(11) 1 d D U P A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.391(4) . ?
C1 C6 1.383(4) . ?
C1 C14 1.534(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.393(4) . ?
C3 C4 1.380(4) . ?
C3 C7 1.519(4) . ?
C4 C5 1.394(4) . ?
C4 O1 1.377(4) . ?
C5 C6 1.383(4) . ?
C5 C24 1.496(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.519(4) . ?
C7 C18 1.545(5) . ?
C7 C19 1.533(5) . ?
C8 C9 1.384(4) . ?
C8 C13 1.395(4) . ?
C9 C10 1.392(4) . ?
C9 O1 1.381(4) . ?
C10 C11 1.394(4) . ?
C10 C38 1.496(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.389(4) . ?
C12 C13 1.392(4) . ?
C12 C20 1.529(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.479(6) . ?
C14 C16 1.543(7) . ?
C14 C17 1.480(6) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.530(6) . ?
C20 C22 1.504(6) . ?
C20 C23 1.490(6) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C25 1.406(5) . ?
C24 C33 1.409(5) . ?
C25 C26 1.424(5) . ?
C25 C30 1.443(5) . ?
C26 H26 0.9300 . ?
C26 C27 1.361(5) . ?
C27 H27 0.9300 . ?
C27 C28 1.424(6) . ?
C28 H28 0.9300 . ?
C28 C29 1.323(6) . ?
C29 H29 0.9300 . ?
C29 C30 1.427(6) . ?
C30 C31 1.379(5) . ?
C31 H31 0.9300 . ?
C31 C32 1.382(5) . ?
C32 C33 1.450(5) . ?
C32 C37 1.420(6) . ?
C33 C34 1.420(5) . ?
C34 H34 0.9300 . ?
C34 C35 1.343(5) . ?
C35 H35 0.9300 . ?
C35 C36 1.413(6) . ?
C36 H36 0.9300 . ?
C36 C37 1.340(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.404(5) . ?
C38 C47 1.414(5) . ?
C39 C40 1.428(5) . ?
C39 C44 1.425(5) . ?
C40 H40 0.9300 . ?
C40 C41 1.358(5) . ?
C41 H41 0.9300 . ?
C41 C42 1.411(6) . ?
C42 H42 0.9300 . ?
C42 C43 1.337(6) . ?
C43 H43 0.9300 . ?
C43 C44 1.422(5) . ?
C44 C45 1.390(5) . ?
C45 H45 0.9300 . ?
C45 C46 1.376(5) . ?
C46 C47 1.430(5) . ?
C46 C51 1.430(6) . ?
C47 C48 1.433(5) . ?
C48 H48 0.9300 . ?
C48 C49 1.349(5) . ?
C49 H49 0.9300 . ?
C49 C50 1.409(6) . ?
C50 H50 0.9300 . ?
C50 C51 1.335(6) . ?
C51 H51 0.9300 . ?
C1S' H1SA 0.9700 . ?
C1S' H1SB 0.9700 . ?
C1S' Cl1' 1.783(6) . ?
C1S' Cl2 1.787(6) . ?
C1S H1SC 0.9700 . ?
C1S H1SD 0.9700 . ?
C1S Cl1 1.811(8) . ?
C1S Cl2' 1.810(8) . ?

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
C2 C1 C14 120.7(3) . . ?
C6 C1 C2 116.8(3) . . ?
C6 C1 C14 122.5(3) . . ?
C1 C2 H2 118.5 . . ?
C1 C2 C3 122.9(3) . . ?
C3 C2 H2 118.5 . . ?
C2 C3 C7 119.9(3) . . ?
C4 C3 C2 117.6(3) . . ?
C4 C3 C7 122.4(3) . . ?
C3 C4 C5 121.8(3) . . ?
O1 C4 C3 123.0(3) . . ?
O1 C4 C5 115.3(3) . . ?
C4 C5 C24 121.7(3) . . ?
C6 C5 C4 118.1(3) . . ?
C6 C5 C24 120.2(3) . . ?
C1 C6 C5 122.8(3) . . ?
C1 C6 H6 118.6 . . ?
C5 C6 H6 118.6 . . ?
C3 C7 C18 108.9(3) . . ?
C3 C7 C19 109.5(3) . . ?
C8 C7 C3 110.2(3) . . ?
C8 C7 C18 108.7(3) . . ?
C8 C7 C19 109.7(3) . . ?
C19 C7 C18 109.8(3) . . ?
C9 C8 C7 122.6(3) . . ?
C9 C8 C13 117.1(3) . . ?
C13 C8 C7 120.3(3) . . ?
C8 C9 C10 122.4(3) . . ?
O1 C9 C8 122.5(3) . . ?
O1 C9 C10 115.1(3) . . ?
C9 C10 C11 117.8(3) . . ?
C9 C10 C38 122.9(3) . . ?
C11 C10 C38 119.3(3) . . ?
C10 C11 H11 118.7 . . ?
C12 C11 C10 122.6(3) . . ?
C12 C11 H11 118.7 . . ?
C11 C12 C13 116.7(3) . . ?
C11 C12 C20 122.7(3) . . ?
C13 C12 C20 120.6(3) . . ?
C8 C13 H13 118.3 . . ?
C12 C13 C8 123.4(3) . . ?
C12 C13 H13 118.3 . . ?
C1 C14 C16 110.1(3) . . ?
C15 C14 C1 109.6(4) . . ?
C15 C14 C16 106.8(5) . . ?
C15 C14 C17 110.8(5) . . ?
C17 C14 C1 113.0(3) . . ?
C17 C14 C16 106.2(4) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C7 C18 H18A 109.5 . . ?
C7 C18 H18B 109.5 . . ?
C7 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C7 C19 H19A 109.5 . . ?
C7 C19 H19B 109.5 . . ?
C7 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C12 C20 C21 108.7(3) . . ?
C22 C20 C12 109.9(3) . . ?
C22 C20 C21 106.5(4) . . ?
C23 C20 C12 112.9(3) . . ?
C23 C20 C21 108.6(4) . . ?
C23 C20 C22 110.1(4) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C5 119.9(3) . . ?
C25 C24 C33 120.7(3) . . ?
C33 C24 C5 119.3(3) . . ?
C24 C25 C26 123.1(3) . . ?
C24 C25 C30 119.2(3) . . ?
C26 C25 C30 117.7(4) . . ?
C25 C26 H26 119.2 . . ?
C27 C26 C25 121.7(4) . . ?
C27 C26 H26 119.2 . . ?
C26 C27 H27 120.1 . . ?
C26 C27 C28 119.7(4) . . ?
C28 C27 H27 120.1 . . ?
C27 C28 H28 119.6 . . ?
C29 C28 C27 120.7(4) . . ?
C29 C28 H28 119.6 . . ?
C28 C29 H29 118.9 . . ?
C28 C29 C30 122.2(4) . . ?
C30 C29 H29 118.9 . . ?
C29 C30 C25 118.0(4) . . ?
C31 C30 C25 119.4(4) . . ?
C31 C30 C29 122.6(4) . . ?
C30 C31 H31 118.8 . . ?
C30 C31 C32 122.4(4) . . ?
C32 C31 H31 118.8 . . ?
C31 C32 C33 119.3(4) . . ?
C31 C32 C37 122.2(4) . . ?
C37 C32 C33 118.5(4) . . ?
C24 C33 C32 118.9(3) . . ?
C24 C33 C34 123.9(3) . . ?
C34 C33 C32 117.2(4) . . ?
C33 C34 H34 119.1 . . ?
C35 C34 C33 121.9(4) . . ?
C35 C34 H34 119.1 . . ?
C34 C35 H35 119.7 . . ?
C34 C35 C36 120.6(5) . . ?
C36 C35 H35 119.7 . . ?
C35 C36 H36 119.8 . . ?
C37 C36 C35 120.4(4) . . ?
C37 C36 H36 119.8 . . ?
C32 C37 H37 119.3 . . ?
C36 C37 C32 121.4(4) . . ?
C36 C37 H37 119.3 . . ?
C39 C38 C10 119.9(3) . . ?
C39 C38 C47 120.1(3) . . ?
C47 C38 C10 119.8(3) . . ?
C38 C39 C40 123.0(3) . . ?
C38 C39 C44 120.0(4) . . ?
C44 C39 C40 117.1(4) . . ?
C39 C40 H40 118.9 . . ?
C41 C40 C39 122.1(4) . . ?
C41 C40 H40 118.9 . . ?
C40 C41 H41 120.1 . . ?
C40 C41 C42 119.7(4) . . ?
C42 C41 H41 120.1 . . ?
C41 C42 H42 119.8 . . ?
C43 C42 C41 120.5(4) . . ?
C43 C42 H42 119.8 . . ?
C42 C43 H43 119.1 . . ?
C42 C43 C44 121.7(4) . . ?
C44 C43 H43 119.1 . . ?
C43 C44 C39 118.9(4) . . ?
C45 C44 C39 118.8(4) . . ?
C45 C44 C43 122.3(4) . . ?
C44 C45 H45 118.9 . . ?
C46 C45 C44 122.3(3) . . ?
C46 C45 H45 118.9 . . ?
C45 C46 C47 119.7(4) . . ?
C45 C46 C51 122.0(4) . . ?
C47 C46 C51 118.3(4) . . ?
C38 C47 C46 119.0(3) . . ?
C38 C47 C48 123.4(3) . . ?
C46 C47 C48 117.6(4) . . ?
C47 C48 H48 119.3 . . ?
C49 C48 C47 121.3(4) . . ?
C49 C48 H48 119.3 . . ?
C48 C49 H49 119.6 . . ?
C48 C49 C50 120.7(4) . . ?
C50 C49 H49 119.6 . . ?
C49 C50 H50 119.9 . . ?
C51 C50 C49 120.3(4) . . ?
C51 C50 H50 119.9 . . ?
C46 C51 H51 119.1 . . ?
C50 C51 C46 121.7(4) . . ?
C50 C51 H51 119.1 . . ?
C4 O1 C9 119.3(2) . . ?
H1SA C1S' H1SB 109.6 . . ?
Cl1' C1S' H1SA 112.0 . . ?
Cl1' C1S' H1SB 112.0 . . ?
Cl1' C1S' Cl2 99.1(5) . . ?
Cl2 C1S' H1SA 112.0 . . ?
Cl2 C1S' H1SB 112.0 . . ?
H1SC C1S H1SD 109.8 . . ?
Cl1 C1S H1SC 112.2 . . ?
Cl1 C1S H1SD 112.2 . . ?
Cl2' C1S H1SC 112.2 . . ?
Cl2' C1S H1SD 112.2 . . ?
Cl2' C1S Cl1 97.9(6) . . ?

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 C2 C3 C4 -0.6(5) . . . . ?
C1 C2 C3 C7 179.7(3) . . . . ?
C2 C1 C6 C5 -0.4(5) . . . . ?
C2 C1 C14 C15 -68.9(6) . . . . ?
C2 C1 C14 C16 48.3(5) . . . . ?
C2 C1 C14 C17 166.9(4) . . . . ?
C2 C3 C4 C5 0.3(5) . . . . ?
C2 C3 C4 O1 179.9(3) . . . . ?
C2 C3 C7 C8 179.9(3) . . . . ?
C2 C3 C7 C18 60.7(4) . . . . ?
C2 C3 C7 C19 -59.3(4) . . . . ?
C3 C4 C5 C6 -0.1(5) . . . . ?
C3 C4 C5 C24 179.1(3) . . . . ?
C3 C4 O1 C9 0.8(5) . . . . ?
C3 C7 C8 C9 -0.6(4) . . . . ?
C3 C7 C8 C13 -179.8(3) . . . . ?
C4 C3 C7 C8 0.2(4) . . . . ?
C4 C3 C7 C18 -119.0(3) . . . . ?
C4 C3 C7 C19 120.9(3) . . . . ?
C4 C5 C6 C1 0.2(5) . . . . ?
C4 C5 C24 C25 -110.3(4) . . . . ?
C4 C5 C24 C33 73.1(4) . . . . ?
C5 C4 O1 C9 -179.5(3) . . . . ?
C5 C24 C25 C26 4.1(5) . . . . ?
C5 C24 C25 C30 -175.6(3) . . . . ?
C5 C24 C33 C32 175.1(3) . . . . ?
C5 C24 C33 C34 -3.5(5) . . . . ?
C6 C1 C2 C3 0.6(5) . . . . ?
C6 C1 C14 C15 109.4(5) . . . . ?
C6 C1 C14 C16 -133.4(4) . . . . ?
C6 C1 C14 C17 -14.8(6) . . . . ?
C6 C5 C24 C25 68.9(4) . . . . ?
C6 C5 C24 C33 -107.8(4) . . . . ?
C7 C3 C4 C5 -179.9(3) . . . . ?
C7 C3 C4 O1 -0.3(5) . . . . ?
C7 C8 C9 C10 -179.1(3) . . . . ?
C7 C8 C9 O1 1.1(5) . . . . ?
C7 C8 C13 C12 179.4(3) . . . . ?
C8 C9 C10 C11 -0.2(5) . . . . ?
C8 C9 C10 C38 178.1(3) . . . . ?
C8 C9 O1 C4 -1.2(5) . . . . ?
C9 C8 C13 C12 0.1(5) . . . . ?
C9 C10 C11 C12 0.1(5) . . . . ?
C9 C10 C38 C39 -109.3(4) . . . . ?
C9 C10 C38 C47 75.0(4) . . . . ?
C10 C9 O1 C4 179.0(3) . . . . ?
C10 C11 C12 C13 0.2(5) . . . . ?
C10 C11 C12 C20 179.6(3) . . . . ?
C10 C38 C39 C40 6.6(5) . . . . ?
C10 C38 C39 C44 -173.1(3) . . . . ?
C10 C38 C47 C46 172.0(3) . . . . ?
C10 C38 C47 C48 -6.3(5) . . . . ?
C11 C10 C38 C39 69.0(4) . . . . ?
C11 C10 C38 C47 -106.6(4) . . . . ?
C11 C12 C13 C8 -0.2(5) . . . . ?
C11 C12 C20 C21 -124.9(4) . . . . ?
C11 C12 C20 C22 119.0(5) . . . . ?
C11 C12 C20 C23 -4.3(6) . . . . ?
C13 C8 C9 C10 0.1(5) . . . . ?
C13 C8 C9 O1 -179.6(3) . . . . ?
C13 C12 C20 C21 54.6(5) . . . . ?
C13 C12 C20 C22 -61.5(5) . . . . ?
C13 C12 C20 C23 175.2(4) . . . . ?
C14 C1 C2 C3 179.0(3) . . . . ?
C14 C1 C6 C5 -178.7(4) . . . . ?
C18 C7 C8 C9 118.7(3) . . . . ?
C18 C7 C8 C13 -60.5(4) . . . . ?
C19 C7 C8 C9 -121.2(4) . . . . ?
C19 C7 C8 C13 59.6(4) . . . . ?
C20 C12 C13 C8 -179.7(3) . . . . ?
C24 C5 C6 C1 -179.0(3) . . . . ?
C24 C25 C26 C27 -179.2(3) . . . . ?
C24 C25 C30 C29 179.0(3) . . . . ?
C24 C25 C30 C31 0.0(5) . . . . ?
C24 C33 C34 C35 178.4(4) . . . . ?
C25 C24 C33 C32 -1.5(5) . . . . ?
C25 C24 C33 C34 179.9(3) . . . . ?
C25 C26 C27 C28 0.3(6) . . . . ?
C25 C30 C31 C32 -0.5(5) . . . . ?
C26 C25 C30 C29 -0.8(5) . . . . ?
C26 C25 C30 C31 -179.7(3) . . . . ?
C26 C27 C28 C29 -0.9(6) . . . . ?
C27 C28 C29 C30 0.6(7) . . . . ?
C28 C29 C30 C25 0.2(6) . . . . ?
C28 C29 C30 C31 179.1(4) . . . . ?
C29 C30 C31 C32 -179.4(4) . . . . ?
C30 C25 C26 C27 0.5(5) . . . . ?
C30 C31 C32 C33 0.0(6) . . . . ?
C30 C31 C32 C37 178.6(4) . . . . ?
C31 C32 C33 C24 1.0(5) . . . . ?
C31 C32 C33 C34 179.7(4) . . . . ?
C31 C32 C37 C36 -179.3(4) . . . . ?
C32 C33 C34 C35 -0.1(6) . . . . ?
C33 C24 C25 C26 -179.2(3) . . . . ?
C33 C24 C25 C30 1.0(5) . . . . ?
C33 C32 C37 C36 -0.7(6) . . . . ?
C33 C34 C35 C36 -1.1(7) . . . . ?
C34 C35 C36 C37 1.5(8) . . . . ?
C35 C36 C37 C32 -0.6(8) . . . . ?
C37 C32 C33 C24 -177.6(3) . . . . ?
C37 C32 C33 C34 1.0(5) . . . . ?
C38 C10 C11 C12 -178.3(3) . . . . ?
C38 C39 C40 C41 -178.9(4) . . . . ?
C38 C39 C44 C43 179.4(3) . . . . ?
C38 C39 C44 C45 0.3(5) . . . . ?
C38 C47 C48 C49 178.1(4) . . . . ?
C39 C38 C47 C46 -3.7(5) . . . . ?
C39 C38 C47 C48 178.0(3) . . . . ?
C39 C40 C41 C42 -0.1(6) . . . . ?
C39 C44 C45 C46 -2.2(6) . . . . ?
C40 C39 C44 C43 -0.4(5) . . . . ?
C40 C39 C44 C45 -179.4(3) . . . . ?
C40 C41 C42 C43 -1.2(7) . . . . ?
C41 C42 C43 C44 1.7(7) . . . . ?
C42 C43 C44 C39 -0.9(6) . . . . ?
C42 C43 C44 C45 178.1(4) . . . . ?
C43 C44 C45 C46 178.8(4) . . . . ?
C44 C39 C40 C41 0.8(5) . . . . ?
C44 C45 C46 C47 1.1(6) . . . . ?
C44 C45 C46 C51 -179.8(4) . . . . ?
C45 C46 C47 C38 1.9(5) . . . . ?
C45 C46 C47 C48 -179.7(3) . . . . ?
C45 C46 C51 C50 180.0(4) . . . . ?
C46 C47 C48 C49 -0.3(6) . . . . ?
C47 C38 C39 C40 -177.7(3) . . . . ?
C47 C38 C39 C44 2.6(5) . . . . ?
C47 C46 C51 C50 -0.9(6) . . . . ?
C47 C48 C49 C50 -0.8(7) . . . . ?
C48 C49 C50 C51 1.1(8) . . . . ?
C49 C50 C51 C46 -0.3(7) . . . . ?
C51 C46 C47 C38 -177.3(3) . . . . ?
C51 C46 C47 C48 1.1(5) . . . . ?
O1 C4 C5 C6 -179.8(3) . . . . ?
O1 C4 C5 C24 -0.6(5) . . . . ?
O1 C9 C10 C11 179.6(3) . . . . ?
O1 C9 C10 C38 -2.1(5) . . . . ?

_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_mo_210428d_0m
_database_code_depnum_ccdc_archive 'CCDC 2180360'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2022-06-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2022-06-10
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C51 H46 O, C0.313 H2.938 I0.313 O, 0.63(C H3 I)'
_chemical_formula_sum            'C52 H51 I O2'
_chemical_formula_weight         834.83
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.074(4)
_cell_length_b                   13.147(4)
_cell_length_c                   14.493(5)
_cell_angle_alpha                69.147(7)
_cell_angle_beta                 66.505(7)
_cell_angle_gamma                89.161(8)
_cell_volume                     2111.4(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5712
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.67
_cell_measurement_theta_min      2.20
_shelx_estimated_absorpt_T_max   0.924
_shelx_estimated_absorpt_T_min   0.924
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6120
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0975 before and 0.0525 after correction. The Ratio of minimum to maximum transmission is 0.8219. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24340
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        20.919
_diffrn_reflns_theta_max         20.919
_diffrn_reflns_theta_min         1.658
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           45.0
_diffrn_source_power             2.25
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3158
_reflns_number_total             4432
_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 V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         4432
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0845
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          1.970
_refine_ls_shift/su_mean         0.033
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1332P)²+6.1808P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2268
_refine_ls_wR_factor_ref         0.2664
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1T) \\sim Ueq, Uanis(C1U) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
3. Others
 Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(I0AA)=FVAR(1)
 Sof(C1T)=Sof(H1TA)=Sof(H1TB)=Sof(H1TC)=Sof(I1AA)=FVAR(2)
 Sof(C1U)=Sof(H1UA)=Sof(H1UB)=Sof(H1UC)=Sof(I)=FVAR(3)
4.a Free rotating group:
 O1W(H1WA,H1WB)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18),
 C20(H20), C24(H24), C30(H30), C33(H33), C35(H35), C36(H36), C38(H38), C40(H40),
  C41(H41), C42(H42), C43(H43), C50(H50), C51(H51), C52(H52)
4.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C1S(H1SA,H1SB,H1SC), C1T(H1TA,H1TB,H1TC), C1U(H1UA,H1UB,H1UC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
C1 C 0.7421(6) 0.6781(6) 0.0663(8) 0.063(2) Uani 1 1 d . . . . .
H1 H 0.819930 0.683537 0.030094 0.075 Uiso 1 1 calc R U . . .
C3 C 0.5618(6) 0.6878(5) 0.0603(6) 0.0472(18) Uani 1 1 d . . . . .
H3 H 0.518509 0.698512 0.020886 0.057 Uiso 1 1 calc R U . . .
C4 C 0.5067(5) 0.6658(4) 0.1732(5) 0.0349(16) Uani 1 1 d . . . . .
C5 C 0.3897(5) 0.6599(4) 0.2297(5) 0.0261(14) Uani 1 1 d . . . . .
C6 C 0.3195(5) 0.6893(5) 0.1675(5) 0.0347(16) Uani 1 1 d . . . . .
C7 C 0.2420(5) 0.6117(5) 0.1748(4) 0.0289(15) Uani 1 1 d . . . . .
C8 C 0.1626(5) 0.4234(5) 0.2553(5) 0.0295(15) Uani 1 1 d . . . . .
C9 C 0.1614(5) 0.3195(5) 0.3271(5) 0.0325(15) Uani 1 1 d . . . . .
C10 C 0.2316(5) 0.2992(4) 0.3893(5) 0.0303(15) Uani 1 1 d . . . . .
C11 C 0.1799(5) 0.2681(4) 0.5030(5) 0.0322(15) Uani 1 1 d . . . . .
C12 C 0.0623(6) 0.2620(5) 0.5631(6) 0.0444(17) Uani 1 1 d . . . . .
H12 H 0.016492 0.280658 0.526116 0.053 Uiso 1 1 calc R U . . .
C13 C 0.0148(7) 0.2299(6) 0.6729(6) 0.056(2) Uani 1 1 d . . . . .
H13 H -0.062520 0.226499 0.710348 0.068 Uiso 1 1 calc R U . . .
C14 C 0.0837(7) 0.2015(6) 0.7303(6) 0.055(2) Uani 1 1 d . . . . .
H14 H 0.050910 0.178493 0.805720 0.066 Uiso 1 1 calc R U . . .
C15 C 0.5832(7) 0.3118(9) 0.2321(8) 0.086(3) Uani 1 1 d . . . . .
H15 H 0.660237 0.311188 0.197568 0.103 Uiso 1 1 calc R U . . .
C16 C 0.5334(6) 0.2818(7) 0.3402(7) 0.073(2) Uani 1 1 d . . . . .
H16 H 0.576916 0.262777 0.379530 0.087 Uiso 1 1 calc R U . . .
C17 C 0.4152(6) 0.2784(6) 0.3965(6) 0.0484(18) Uani 1 1 d . . . . .
C18 C 0.3629(6) 0.2445(6) 0.5085(6) 0.0501(19) Uani 1 1 d . . . . .
H18 H 0.406144 0.223968 0.548009 0.060 Uiso 1 1 calc R U . . .
C19 C 0.2478(6) 0.2404(5) 0.5634(5) 0.0408(17) Uani 1 1 d . . . . .
C20 C 0.1937(7) 0.2072(6) 0.6783(6) 0.0531(19) Uani 1 1 d . . . . .
H20 H 0.236928 0.189038 0.717996 0.064 Uiso 1 1 calc R U . . .
C21 C 0.1808(5) 0.6400(5) 0.1135(5) 0.0292(15) Uani 1 1 d . . . . .
C22 C 0.0988(5) 0.5550(4) 0.1181(5) 0.0297(15) Uani 1 1 d . . . . .
C23 C 0.0973(5) 0.4426(5) 0.1974(5) 0.0299(15) Uani 1 1 d . . . . .
C24 C 0.0284(5) 0.3507(5) 0.2144(5) 0.0381(16) Uani 1 1 d . . . . .
H24 H -0.016095 0.361536 0.176126 0.046 Uiso 1 1 calc R U . . .
C25 C 0.0229(5) 0.2443(5) 0.2856(5) 0.0323(15) Uani 1 1 d . . . . .
C26 C -0.0533(6) 0.1491(5) 0.2985(5) 0.0431(17) Uani 1 1 d . . . . .
C27 C -0.1734(7) 0.1764(7) 0.3261(8) 0.085(3) Uani 1 1 d . . . . .
H27A H -0.199725 0.191889 0.391081 0.128 Uiso 1 1 calc R U . . .
H27B H -0.222035 0.114903 0.337605 0.128 Uiso 1 1 calc R U . . .
H27C H -0.173782 0.239715 0.267042 0.128 Uiso 1 1 calc R U . . .
C28 C -0.0127(9) 0.1323(8) 0.1925(8) 0.103(3) Uani 1 1 d . . . . .
H28A H -0.011929 0.198942 0.136028 0.154 Uiso 1 1 calc R U . . .
H28B H -0.062383 0.073873 0.200179 0.154 Uiso 1 1 calc R U . . .
H28C H 0.062164 0.113435 0.173989 0.154 Uiso 1 1 calc R U . . .
C29 C -0.0617(8) 0.0436(6) 0.3886(8) 0.085(3) Uani 1 1 d . . . . .
H29A H 0.011230 0.020351 0.372817 0.127 Uiso 1 1 calc R U . . .
H29B H -0.113756 -0.011906 0.395015 0.127 Uiso 1 1 calc R U . . .
H29C H -0.087813 0.054841 0.455775 0.127 Uiso 1 1 calc R U . . .
C30 C 0.0898(5) 0.2320(5) 0.3412(5) 0.0377(16) Uani 1 1 d . . . . .
H30 H 0.087127 0.162305 0.390354 0.045 Uiso 1 1 calc R U . . .
C31 C -0.0186(5) 0.5866(5) 0.1524(5) 0.0457(18) Uani 1 1 d . . . . .
H31A H -0.042667 0.590930 0.222583 0.069 Uiso 1 1 calc R U . . .
H31B H -0.069876 0.532085 0.156299 0.069 Uiso 1 1 calc R U . . .
H31C H -0.017685 0.656836 0.100153 0.069 Uiso 1 1 calc R U . . .
C32 C 0.1389(6) 0.5516(5) 0.0040(5) 0.0483(18) Uani 1 1 d . . . . .
H32A H 0.140198 0.622856 -0.047063 0.072 Uiso 1 1 calc R U . . .
H32B H 0.088198 0.498231 0.005681 0.072 Uiso 1 1 calc R U . . .
H32C H 0.213350 0.531742 -0.017807 0.072 Uiso 1 1 calc R U . . .
C33 C 0.1955(5) 0.7503(5) 0.0455(5) 0.0352(16) Uani 1 1 d . . . . .
H33 H 0.153956 0.770198 0.004200 0.042 Uiso 1 1 calc R U . . .
C34 C 0.2695(5) 0.8318(5) 0.0368(5) 0.0361(16) Uani 1 1 d . . . . .
C35 C 0.3303(5) 0.7980(5) 0.0982(5) 0.0393(17) Uani 1 1 d . . . . .
H35 H 0.381242 0.850478 0.093298 0.047 Uiso 1 1 calc R U . . .
C36 C 0.6954(6) 0.6560(6) 0.1716(7) 0.053(2) Uani 1 1 d . . . . .
H36 H 0.741326 0.645467 0.208382 0.064 Uiso 1 1 calc R U . . .
C37 C 0.5776(6) 0.6477(5) 0.2306(6) 0.0426(17) Uani 1 1 d . . . . .
C38 C 0.5270(6) 0.6260(5) 0.3413(6) 0.0505(19) Uani 1 1 d . . . . .
H38 H 0.572984 0.618459 0.377772 0.061 Uiso 1 1 calc R U . . .
C39 C 0.4125(6) 0.6150(5) 0.3997(6) 0.0454(18) Uani 1 1 d . . . . .
C40 C 0.3622(7) 0.5919(6) 0.5129(6) 0.061(2) Uani 1 1 d . . . . .
H40 H 0.407974 0.582223 0.549862 0.073 Uiso 1 1 calc R U . . .
C41 C 0.2522(8) 0.5838(7) 0.5674(7) 0.073(2) Uani 1 1 d . . . . .
H41 H 0.222040 0.569703 0.641467 0.088 Uiso 1 1 calc R U . . .
C42 C 0.1792(7) 0.5963(7) 0.5144(7) 0.068(2) Uani 1 1 d . . . . .
H42 H 0.101669 0.588038 0.554121 0.081 Uiso 1 1 calc R U . . .
C43 C 0.2230(6) 0.6202(6) 0.4056(6) 0.0529(19) Uani 1 1 d . . . . .
H43 H 0.174213 0.629909 0.371820 0.063 Uiso 1 1 calc R U . . .
C44 C 0.3408(5) 0.6310(5) 0.3415(5) 0.0393(17) Uani 1 1 d . . . . .
C45 C 0.2829(6) 0.9506(5) -0.0410(6) 0.0463(18) Uani 1 1 d . . . . .
C46 C 0.3219(8) 0.9538(6) -0.1586(7) 0.082(3) Uani 1 1 d . . . . .
H46A H 0.389699 0.921341 -0.177682 0.123 Uiso 1 1 calc R U . . .
H46B H 0.336141 1.028770 -0.208757 0.123 Uiso 1 1 calc R U . . .
H46C H 0.263917 0.913222 -0.162020 0.123 Uiso 1 1 calc R U . . .
C47 C 0.3733(9) 1.0256(6) -0.0473(9) 0.097(3) Uani 1 1 d . . . . .
H47A H 0.354395 1.027105 0.023361 0.146 Uiso 1 1 calc R U . . .
H47B H 0.378971 1.098600 -0.097889 0.146 Uiso 1 1 calc R U . . .
H47C H 0.444140 0.999057 -0.071254 0.146 Uiso 1 1 calc R U . . .
C48 C 0.1715(7) 0.9916(7) -0.0126(8) 0.090(3) Uani 1 1 d . . . . .
H48A H 0.119581 0.946796 -0.019326 0.135 Uiso 1 1 calc R U . . .
H48B H 0.180963 1.066512 -0.061272 0.135 Uiso 1 1 calc R U . . .
H48C H 0.142415 0.987810 0.060851 0.135 Uiso 1 1 calc R U . . .
C49 C 0.3494(5) 0.3076(5) 0.3351(5) 0.0382(16) Uani 1 1 d . . . . .
C50 C 0.4081(6) 0.3411(6) 0.2201(6) 0.0529(19) Uani 1 1 d . . . . .
H50 H 0.367495 0.361448 0.177911 0.064 Uiso 1 1 calc R U . . .
C51 C 0.5198(7) 0.3441(7) 0.1705(6) 0.071(2) Uani 1 1 d . . . . .
H51 H 0.555435 0.367703 0.095128 0.085 Uiso 1 1 calc R U . . .
C52 C 0.6746(7) 0.6939(6) 0.0075(6) 0.060(2) Uani 1 1 d . . . . .
H52 H 0.707733 0.708206 -0.066597 0.072 Uiso 1 1 calc R U . . .
O1 O 0.2348(3) 0.5061(3) 0.2449(3) 0.0382(11) Uani 1 1 d . . . . .
C1S C 0.365(2) 1.024(3) 0.365(3) 0.070(10) Uani 0.313(15) 1 d . . P A 2
H1SA H 0.408786 1.095560 0.319269 0.105 Uiso 0.313(15) 1 calc R U P A 2
H1SB H 0.413130 0.971534 0.380582 0.105 Uiso 0.313(15) 1 calc R U P A 2
H1SC H 0.309091 1.026255 0.431211 0.105 Uiso 0.313(15) 1 calc R U P A 2
I0AA I 0.2888(11) 0.980(3) 0.2877(15) 0.199(11) Uani 0.313(15) 1 d . . P A 2
C1T C 0.365(5) 0.925(3) 0.361(4) 0.08(2) Uani 0.373(11) 1 d . U P B 3
H1TA H 0.324300 0.900229 0.438166 0.122 Uiso 0.373(11) 1 calc R U P B 3
H1TB H 0.390232 1.002927 0.330735 0.122 Uiso 0.373(11) 1 calc R U P B 3
H1TC H 0.428766 0.887179 0.342972 0.122 Uiso 0.373(11) 1 calc R U P B 3
I1AA I 0.3064(11) 0.9076(5) 0.3241(5) 0.145(3) Uani 0.373(11) 1 d . . P B 3
C1U C 0.369(3) 0.882(3) 0.359(4) 0.014(9) Uani 0.258(12) 1 d . U P C 1
H1UA H 0.409037 0.856248 0.301997 0.021 Uiso 0.258(12) 1 calc R U P C 1
H1UB H 0.300432 0.831767 0.410197 0.021 Uiso 0.258(12) 1 calc R U P C 1
H1UC H 0.414734 0.885967 0.395603 0.021 Uiso 0.258(12) 1 calc R U P C 1
I I 0.3256(6) 1.0512(5) 0.2868(12) 0.155(6) Uani 0.258(12) 1 d . . P C 1
O1W O 0.4706(12) 0.9891(11) 0.4452(9) 0.194(5) Uani 1 1 d G . . . .
H1WA H 0.424648 1.026800 0.423571 0.291 Uiso 1 1 d G U . . .
H1WB H 0.535938 0.971117 0.421439 0.291 Uiso 1 1 d G 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
C1 H1 0.9300 . ?
C1 C36 1.316(10) . ?
C1 C52 1.419(11) . ?
C3 H3 0.9300 . ?
C3 C4 1.417(9) . ?
C3 C52 1.352(10) . ?
C4 C5 1.406(8) . ?
C4 C37 1.441(9) . ?
C5 C6 1.486(8) . ?
C5 C44 1.386(8) . ?
C6 C7 1.395(8) . ?
C6 C35 1.393(8) . ?
C7 C21 1.375(8) . ?
C7 O1 1.375(7) . ?
C8 C9 1.387(8) . ?
C8 C23 1.382(8) . ?
C8 O1 1.378(7) . ?
C9 C10 1.487(8) . ?
C9 C30 1.396(8) . ?
C10 C11 1.407(8) . ?
C10 C49 1.407(8) . ?
C11 C12 1.419(9) . ?
C11 C19 1.439(8) . ?
C12 H12 0.9300 . ?
C12 C13 1.355(9) . ?
C13 H13 0.9300 . ?
C13 C14 1.418(10) . ?
C14 H14 0.9300 . ?
C14 C20 1.319(10) . ?
C15 H15 0.9300 . ?
C15 C16 1.337(11) . ?
C15 C51 1.406(11) . ?
C16 H16 0.9300 . ?
C16 C17 1.423(10) . ?
C17 C18 1.382(9) . ?
C17 C49 1.428(9) . ?
C18 H18 0.9300 . ?
C18 C19 1.384(9) . ?
C19 C20 1.421(9) . ?
C20 H20 0.9300 . ?
C21 C22 1.527(8) . ?
C21 C33 1.397(8) . ?
C22 C23 1.510(8) . ?
C22 C31 1.515(8) . ?
C22 C32 1.540(9) . ?
C23 C24 1.405(8) . ?
C24 H24 0.9300 . ?
C24 C25 1.394(8) . ?
C25 C26 1.522(8) . ?
C25 C30 1.381(8) . ?
C26 C27 1.530(10) . ?
C26 C28 1.509(11) . ?
C26 C29 1.497(10) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30 0.9300 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33 0.9300 . ?
C33 C34 1.392(8) . ?
C34 C35 1.377(8) . ?
C34 C45 1.529(9) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C36 C37 1.415(10) . ?
C37 C38 1.388(10) . ?
C38 H38 0.9300 . ?
C38 C39 1.374(10) . ?
C39 C40 1.417(10) . ?
C39 C44 1.461(9) . ?
C40 H40 0.9300 . ?
C40 C41 1.321(11) . ?
C41 H41 0.9300 . ?
C41 C42 1.420(11) . ?
C42 H42 0.9300 . ?
C42 C43 1.358(10) . ?
C43 H43 0.9300 . ?
C43 C44 1.424(9) . ?
C45 C46 1.557(11) . ?
C45 C47 1.504(10) . ?
C45 C48 1.496(10) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 C50 1.424(9) . ?
C50 H50 0.9300 . ?
C50 C51 1.339(10) . ?
C51 H51 0.9300 . ?
C52 H52 0.9300 . ?
C1S H1SA 0.9600 . ?
C1S H1SB 0.9600 . ?
C1S H1SC 0.9600 . ?
C1S I0AA 1.98(4) . ?
C1T H1TA 0.9600 . ?
C1T H1TB 0.9600 . ?
C1T H1TC 0.9600 . ?
C1T I1AA 1.15(6) . ?
C1U H1UA 0.9600 . ?
C1U H1UB 0.9600 . ?
C1U H1UC 0.9600 . ?
C1U I 2.27(3) . ?
O1W H1WA 0.8579 . ?
O1W H1WB 0.8497 . ?

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
C36 C1 H1 119.8 . . ?
C36 C1 C52 120.5(7) . . ?
C52 C1 H1 119.8 . . ?
C4 C3 H3 118.6 . . ?
C52 C3 H3 118.6 . . ?
C52 C3 C4 122.8(7) . . ?
C3 C4 C37 116.2(6) . . ?
C5 C4 C3 123.8(6) . . ?
C5 C4 C37 119.9(6) . . ?
C4 C5 C6 119.1(5) . . ?
C44 C5 C4 120.6(5) . . ?
C44 C5 C6 120.3(5) . . ?
C7 C6 C5 122.5(5) . . ?
C35 C6 C5 119.8(5) . . ?
C35 C6 C7 117.7(5) . . ?
C21 C7 C6 121.5(5) . . ?
C21 C7 O1 123.6(5) . . ?
O1 C7 C6 114.9(5) . . ?
C23 C8 C9 122.7(5) . . ?
O1 C8 C9 115.0(5) . . ?
O1 C8 C23 122.3(5) . . ?
C8 C9 C10 122.5(5) . . ?
C8 C9 C30 117.8(5) . . ?
C30 C9 C10 119.7(5) . . ?
C11 C10 C9 119.9(5) . . ?
C49 C10 C9 120.0(5) . . ?
C49 C10 C11 120.0(5) . . ?
C10 C11 C12 123.4(6) . . ?
C10 C11 C19 119.4(6) . . ?
C12 C11 C19 117.2(6) . . ?
C11 C12 H12 119.0 . . ?
C13 C12 C11 122.0(6) . . ?
C13 C12 H12 119.0 . . ?
C12 C13 H13 120.2 . . ?
C12 C13 C14 119.6(7) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 H14 119.5 . . ?
C20 C14 C13 121.0(7) . . ?
C20 C14 H14 119.5 . . ?
C16 C15 H15 119.9 . . ?
C16 C15 C51 120.3(7) . . ?
C51 C15 H15 119.9 . . ?
C15 C16 H16 119.2 . . ?
C15 C16 C17 121.6(7) . . ?
C17 C16 H16 119.2 . . ?
C16 C17 C49 118.6(7) . . ?
C18 C17 C16 121.7(6) . . ?
C18 C17 C49 119.7(6) . . ?
C17 C18 H18 119.1 . . ?
C17 C18 C19 121.8(6) . . ?
C19 C18 H18 119.1 . . ?
C18 C19 C11 119.4(6) . . ?
C18 C19 C20 122.1(6) . . ?
C20 C19 C11 118.5(6) . . ?
C14 C20 C19 121.8(7) . . ?
C14 C20 H20 119.1 . . ?
C19 C20 H20 119.1 . . ?
C7 C21 C22 121.9(5) . . ?
C7 C21 C33 118.1(5) . . ?
C33 C21 C22 120.0(5) . . ?
C21 C22 C32 108.5(5) . . ?
C23 C22 C21 110.0(5) . . ?
C23 C22 C31 109.9(5) . . ?
C23 C22 C32 108.9(5) . . ?
C31 C22 C21 110.0(5) . . ?
C31 C22 C32 109.5(5) . . ?
C8 C23 C22 123.2(5) . . ?
C8 C23 C24 116.6(5) . . ?
C24 C23 C22 120.2(5) . . ?
C23 C24 H24 118.2 . . ?
C25 C24 C23 123.6(5) . . ?
C25 C24 H24 118.2 . . ?
C24 C25 C26 120.3(5) . . ?
C30 C25 C24 116.3(5) . . ?
C30 C25 C26 123.4(5) . . ?
C25 C26 C27 109.6(5) . . ?
C28 C26 C25 109.7(6) . . ?
C28 C26 C27 107.7(7) . . ?
C29 C26 C25 113.5(5) . . ?
C29 C26 C27 106.2(7) . . ?
C29 C26 C28 109.9(7) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C9 C30 H30 118.5 . . ?
C25 C30 C9 123.0(5) . . ?
C25 C30 H30 118.5 . . ?
C22 C31 H31A 109.5 . . ?
C22 C31 H31B 109.5 . . ?
C22 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C22 C32 H32A 109.5 . . ?
C22 C32 H32B 109.5 . . ?
C22 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C21 C33 H33 118.5 . . ?
C34 C33 C21 122.9(5) . . ?
C34 C33 H33 118.5 . . ?
C33 C34 C45 120.1(5) . . ?
C35 C34 C33 116.3(5) . . ?
C35 C34 C45 123.6(5) . . ?
C6 C35 H35 118.3 . . ?
C34 C35 C6 123.4(6) . . ?
C34 C35 H35 118.3 . . ?
C1 C36 H36 118.9 . . ?
C1 C36 C37 122.2(7) . . ?
C37 C36 H36 118.9 . . ?
C36 C37 C4 118.9(7) . . ?
C38 C37 C4 118.1(6) . . ?
C38 C37 C36 123.0(6) . . ?
C37 C38 H38 118.3 . . ?
C39 C38 C37 123.4(6) . . ?
C39 C38 H38 118.3 . . ?
C38 C39 C40 122.6(7) . . ?
C38 C39 C44 118.2(6) . . ?
C40 C39 C44 119.1(7) . . ?
C39 C40 H40 119.1 . . ?
C41 C40 C39 121.8(7) . . ?
C41 C40 H40 119.1 . . ?
C40 C41 H41 119.6 . . ?
C40 C41 C42 120.9(7) . . ?
C42 C41 H41 119.6 . . ?
C41 C42 H42 120.1 . . ?
C43 C42 C41 119.9(8) . . ?
C43 C42 H42 120.1 . . ?
C42 C43 H43 118.8 . . ?
C42 C43 C44 122.4(7) . . ?
C44 C43 H43 118.8 . . ?
C5 C44 C39 119.6(6) . . ?
C5 C44 C43 124.4(6) . . ?
C43 C44 C39 116.0(6) . . ?
C34 C45 C46 109.0(6) . . ?
C47 C45 C34 112.9(6) . . ?
C47 C45 C46 105.2(7) . . ?
C48 C45 C34 110.1(6) . . ?
C48 C45 C46 106.6(7) . . ?
C48 C45 C47 112.6(7) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C10 C49 C17 119.7(6) . . ?
C10 C49 C50 123.3(6) . . ?
C50 C49 C17 117.0(6) . . ?
C49 C50 H50 118.9 . . ?
C51 C50 C49 122.3(7) . . ?
C51 C50 H50 118.9 . . ?
C15 C51 H51 119.9 . . ?
C50 C51 C15 120.3(7) . . ?
C50 C51 H51 119.9 . . ?
C1 C52 H52 120.3 . . ?
C3 C52 C1 119.4(7) . . ?
C3 C52 H52 120.3 . . ?
C7 O1 C8 119.0(4) . . ?
H1SA C1S H1SB 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
I0AA C1S H1SA 109.5 . . ?
I0AA C1S H1SB 109.4 . . ?
I0AA C1S H1SC 109.5 . . ?
H1TA C1T H1TB 109.5 . . ?
H1TA C1T H1TC 109.5 . . ?
H1TB C1T H1TC 109.5 . . ?
I1AA C1T H1TA 109.5 . . ?
I1AA C1T H1TB 109.4 . . ?
I1AA C1T H1TC 109.5 . . ?
H1UA C1U H1UB 109.5 . . ?
H1UA C1U H1UC 109.5 . . ?
H1UB C1U H1UC 109.5 . . ?
I C1U H1UA 109.4 . . ?
I C1U H1UB 109.5 . . ?
I C1U H1UC 109.6 . . ?
H1WA O1W H1WB 141.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C36 C37 C4 -1.0(10) . . . . ?
C1 C36 C37 C38 -179.0(7) . . . . ?
C3 C4 C5 C6 -6.6(8) . . . . ?
C3 C4 C5 C44 175.8(6) . . . . ?
C3 C4 C37 C36 1.8(8) . . . . ?
C3 C4 C37 C38 179.9(6) . . . . ?
C4 C3 C52 C1 -0.2(11) . . . . ?
C4 C5 C6 C7 111.6(6) . . . . ?
C4 C5 C6 C35 -68.1(7) . . . . ?
C4 C5 C44 C39 4.8(8) . . . . ?
C4 C5 C44 C43 -178.3(6) . . . . ?
C4 C37 C38 C39 3.7(10) . . . . ?
C5 C4 C37 C36 -178.9(5) . . . . ?
C5 C4 C37 C38 -0.8(8) . . . . ?
C5 C6 C7 C21 -177.6(6) . . . . ?
C5 C6 C7 O1 0.6(8) . . . . ?
C5 C6 C35 C34 179.2(6) . . . . ?
C6 C5 C44 C39 -172.7(5) . . . . ?
C6 C5 C44 C43 4.2(9) . . . . ?
C6 C7 C21 C22 177.9(5) . . . . ?
C6 C7 C21 C33 -2.1(9) . . . . ?
C6 C7 O1 C8 -178.3(5) . . . . ?
C7 C6 C35 C34 -0.6(9) . . . . ?
C7 C21 C22 C23 0.3(7) . . . . ?
C7 C21 C22 C31 121.5(6) . . . . ?
C7 C21 C22 C32 -118.7(6) . . . . ?
C7 C21 C33 C34 0.5(9) . . . . ?
C8 C9 C10 C11 111.8(6) . . . . ?
C8 C9 C10 C49 -70.3(8) . . . . ?
C8 C9 C30 C25 1.4(9) . . . . ?
C8 C23 C24 C25 0.3(9) . . . . ?
C9 C8 C23 C22 -179.3(5) . . . . ?
C9 C8 C23 C24 -0.1(9) . . . . ?
C9 C8 O1 C7 179.5(5) . . . . ?
C9 C10 C11 C12 -4.7(8) . . . . ?
C9 C10 C11 C19 175.1(5) . . . . ?
C9 C10 C49 C17 -174.3(6) . . . . ?
C9 C10 C49 C50 3.6(9) . . . . ?
C10 C9 C30 C25 -179.4(6) . . . . ?
C10 C11 C12 C13 178.8(6) . . . . ?
C10 C11 C19 C18 -0.2(9) . . . . ?
C10 C11 C19 C20 -178.8(5) . . . . ?
C10 C49 C50 C51 -177.2(7) . . . . ?
C11 C10 C49 C17 3.6(9) . . . . ?
C11 C10 C49 C50 -178.5(6) . . . . ?
C11 C12 C13 C14 0.1(10) . . . . ?
C11 C19 C20 C14 -0.1(10) . . . . ?
C12 C11 C19 C18 179.7(6) . . . . ?
C12 C11 C19 C20 1.0(8) . . . . ?
C12 C13 C14 C20 0.9(11) . . . . ?
C13 C14 C20 C19 -0.9(11) . . . . ?
C15 C16 C17 C18 178.2(8) . . . . ?
C15 C16 C17 C49 0.1(12) . . . . ?
C16 C15 C51 C50 -2.6(14) . . . . ?
C16 C17 C18 C19 -179.5(7) . . . . ?
C16 C17 C49 C10 176.6(6) . . . . ?
C16 C17 C49 C50 -1.4(10) . . . . ?
C17 C18 C19 C11 2.3(10) . . . . ?
C17 C18 C19 C20 -179.1(6) . . . . ?
C17 C49 C50 C51 0.8(10) . . . . ?
C18 C17 C49 C10 -1.5(10) . . . . ?
C18 C17 C49 C50 -179.5(6) . . . . ?
C18 C19 C20 C14 -178.7(7) . . . . ?
C19 C11 C12 C13 -1.0(9) . . . . ?
C21 C7 O1 C8 -0.1(8) . . . . ?
C21 C22 C23 C8 -0.2(8) . . . . ?
C21 C22 C23 C24 -179.4(5) . . . . ?
C21 C33 C34 C35 1.0(9) . . . . ?
C21 C33 C34 C45 178.9(6) . . . . ?
C22 C21 C33 C34 -179.5(5) . . . . ?
C22 C23 C24 C25 179.5(5) . . . . ?
C23 C8 C9 C10 -179.9(6) . . . . ?
C23 C8 C9 C30 -0.7(9) . . . . ?
C23 C8 O1 C7 0.2(8) . . . . ?
C23 C24 C25 C26 -179.4(6) . . . . ?
C23 C24 C25 C30 0.3(9) . . . . ?
C24 C25 C26 C27 -53.5(8) . . . . ?
C24 C25 C26 C28 64.6(8) . . . . ?
C24 C25 C26 C29 -172.0(7) . . . . ?
C24 C25 C30 C9 -1.2(9) . . . . ?
C26 C25 C30 C9 178.5(6) . . . . ?
C30 C9 C10 C11 -67.3(7) . . . . ?
C30 C9 C10 C49 110.6(6) . . . . ?
C30 C25 C26 C27 126.8(7) . . . . ?
C30 C25 C26 C28 -115.1(8) . . . . ?
C30 C25 C26 C29 8.3(10) . . . . ?
C31 C22 C23 C8 -121.5(6) . . . . ?
C31 C22 C23 C24 59.3(7) . . . . ?
C32 C22 C23 C8 118.6(6) . . . . ?
C32 C22 C23 C24 -60.6(7) . . . . ?
C33 C21 C22 C23 -179.7(5) . . . . ?
C33 C21 C22 C31 -58.5(7) . . . . ?
C33 C21 C22 C32 61.3(7) . . . . ?
C33 C34 C35 C6 -0.9(9) . . . . ?
C33 C34 C45 C46 -58.5(8) . . . . ?
C33 C34 C45 C47 -175.0(7) . . . . ?
C33 C34 C45 C48 58.1(9) . . . . ?
C35 C6 C7 C21 2.2(9) . . . . ?
C35 C6 C7 O1 -179.6(5) . . . . ?
C35 C34 C45 C46 119.2(7) . . . . ?
C35 C34 C45 C47 2.7(10) . . . . ?
C35 C34 C45 C48 -124.2(7) . . . . ?
C36 C1 C52 C3 1.1(11) . . . . ?
C36 C37 C38 C39 -178.3(6) . . . . ?
C37 C4 C5 C6 174.2(5) . . . . ?
C37 C4 C5 C44 -3.4(8) . . . . ?
C37 C38 C39 C40 179.4(6) . . . . ?
C37 C38 C39 C44 -2.3(10) . . . . ?
C38 C39 C40 C41 178.7(7) . . . . ?
C38 C39 C44 C5 -2.0(9) . . . . ?
C38 C39 C44 C43 -179.2(6) . . . . ?
C39 C40 C41 C42 1.0(13) . . . . ?
C40 C39 C44 C5 176.3(6) . . . . ?
C40 C39 C44 C43 -0.8(9) . . . . ?
C40 C41 C42 C43 -2.0(13) . . . . ?
C41 C42 C43 C44 1.6(12) . . . . ?
C42 C43 C44 C5 -177.2(7) . . . . ?
C42 C43 C44 C39 -0.2(10) . . . . ?
C44 C5 C6 C7 -70.8(8) . . . . ?
C44 C5 C6 C35 109.4(7) . . . . ?
C44 C39 C40 C41 0.4(11) . . . . ?
C45 C34 C35 C6 -178.7(6) . . . . ?
C49 C10 C11 C12 177.4(5) . . . . ?
C49 C10 C11 C19 -2.8(8) . . . . ?
C49 C17 C18 C19 -1.5(10) . . . . ?
C49 C50 C51 C15 1.2(13) . . . . ?
C51 C15 C16 C17 1.9(15) . . . . ?
C52 C1 C36 C37 -0.5(11) . . . . ?
C52 C3 C4 C5 179.5(6) . . . . ?
C52 C3 C4 C37 -1.2(9) . . . . ?
O1 C7 C21 C22 -0.2(9) . . . . ?
O1 C7 C21 C33 179.8(5) . . . . ?
O1 C8 C9 C10 0.8(8) . . . . ?
O1 C8 C9 C30 180.0(5) . . . . ?
O1 C8 C23 C22 0.0(9) . . . . ?
O1 C8 C23 C24 179.2(5) . . . . ?


_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_20220506-lqy288k
_database_code_depnum_ccdc_archive 'CCDC 2180361'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2022-06-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2022-05-31
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H4 Cl2, C51 H46 O'
_chemical_formula_sum            'C53 H50 Cl2 O'
_chemical_formula_weight         773.83
_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'
Cl Cl 0.3639 0.7018 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.8218(2)
_cell_length_b                   13.0029(2)
_cell_length_c                   15.1355(2)
_cell_angle_alpha                93.8330(10)
_cell_angle_beta                 114.4340(10)
_cell_angle_gamma                108.3690(10)
_cell_volume                     2122.79(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17127
_cell_measurement_temperature    288.00(10)
_cell_measurement_theta_max      66.5350
_cell_measurement_theta_min      3.2770
_shelx_estimated_absorpt_T_max   0.852
_shelx_estimated_absorpt_T_min   0.789
_exptl_absorpt_coefficient_mu    1.656
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24572
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         3.294
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      288.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     31.00  94.00   0.50    0.40    --   72.93-125.00 -30.00  126
  2  ω     47.00  98.00   0.50    0.40    --   76.75-125.00 -90.00  102
  3  ω     29.00  59.00   0.50    0.40    --   62.89-125.00-150.00   60
  4  ω     31.00  57.00   0.50    0.40    --   72.93-125.00  60.00   52
  5  ω     54.00  98.00   0.50    0.40    --   76.75-125.00  60.00   88
  6  ω     35.00  98.00   0.50    0.40    --   76.75-125.00 120.00  126
  7  ω     35.00  76.00   0.50    0.40    --   76.75-125.00 150.00   82
  8  ω     57.00  97.00   0.50    0.40    --   76.75-125.00-150.00   80
  9  ω    -69.00 -28.00   0.50    0.40    --  -63.72 125.00 -90.00   82
 10  ω    -72.00 -36.00   0.50    0.40    --  -76.43 125.00-150.00   72
 11  ω   -102.00 -76.00   0.50    0.40    --  -81.49 125.00-180.00   52
 12  ω   -102.00 -63.00   0.50    0.40    --  -81.49 125.00-120.00   78
 13  ω   -102.00 -44.00   0.50    0.40    --  -81.49 125.00   0.00  116
 14  ω   -102.00 -59.00   0.50    0.40    --  -81.49 125.00 -90.00   86
 15  ω    -69.00 -44.00   0.50    0.40    --  -81.49 125.00  60.00   50
 16  ω    -56.00 -31.00   0.50    0.40    --  -71.74 125.00 150.00   50
 17  ω   -102.00 -43.00   0.50    0.40    --  -81.49 125.00 150.00  118
 18  ω   -102.00 -77.00   0.50    0.40    --  -81.49 125.00 120.00   50
 19  ω   -102.00 -76.00   0.50    0.40    --  -81.49 125.00  60.00   52
 20  ω   -102.00 -76.00   0.50    0.40    --  -81.49 125.00  30.00   52
 21  ω   -101.00 -44.00   0.50    0.40    --  -81.49 125.00  90.00  114
 22  ω   -102.00 -43.00   0.50    0.40    --  -81.49 125.00 -60.00  118
 23  ω    -70.00 -45.00   0.50    0.40    --  -81.49 125.00-180.00   50
 24  ω   -102.00 -77.00   0.50    0.40    --  -81.49 125.00-150.00   50
 25  ω   -123.00 -80.00   0.50    0.40    --  -81.49 -15.00-180.00   86
 26  ω    -83.00 -54.00   0.50    0.40    --  -63.72 -15.00-150.00   58
 27  ω   -101.00 -68.00   0.50    0.40    --  -63.72 -15.00 -60.00   66
 28  ω    -99.00 -63.00   0.50    0.40    --  -63.72 -15.00 -30.00   72
 29  ω    -97.00 -57.00   0.50    0.40    --  -63.72 -15.00   0.00   80
 30  ω   -104.00 -56.00   0.50    0.40    --  -63.72 -15.00  60.00   96
 31  ω   -108.00 -74.00   0.50    0.40    --  -76.43 -15.00 120.00   68
 32  ω   -114.00 -75.00   0.50    0.40    --  -71.74 -15.00 150.00   78
 33  ω   -111.00 -74.00   0.50    0.40    --  -71.74 -15.00  90.00   74
 34  ω   -124.00 -73.00   0.50    0.40    --  -81.49 -15.00  30.00  102
 35  ω   -125.00 -91.00   0.50    0.40    --  -81.49 -15.00 -60.00   68
 36  ω   -119.00 -69.00   0.50    0.40    --  -76.43 -15.00-120.00  100
 37  ω   -115.00 -85.00   0.50    0.40    --  -71.74 -15.00-150.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0463399000
_diffrn_orient_matrix_UB_12      0.0746303000
_diffrn_orient_matrix_UB_13      -0.0614265000
_diffrn_orient_matrix_UB_21      0.0889413000
_diffrn_orient_matrix_UB_22      -0.0591219000
_diffrn_orient_matrix_UB_23      0.0062615000
_diffrn_orient_matrix_UB_31      -0.1012450000
_diffrn_orient_matrix_UB_32      -0.0858851000
_diffrn_orient_matrix_UB_33      -0.0968151000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6625
_reflns_number_total             7435
_reflns_odcompleteness_completeness 98.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         7435
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0653
_refine_ls_restrained_S_all      1.110
_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)+(0.1069P)²+0.8116P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1942
_refine_ls_wR_factor_ref         0.1982
_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. Restrained distances
 C53-Cl2
 1.78 with sigma of 0.02
 C52-Cl1
 1.78 with sigma of 0.02
 C52-C53
 1.54 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C53(H53A,H53B)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C5(H5), C3(H3), C10(H10), C29(H29), C34(H34), C20(H20), C25(H25),
 C32(H32), C39(H39), C15(H15), C22(H22), C31(H31), C30(H30), C36(H36), C23(H23),
  C24(H24), C18(H18), C16(H16), C17(H17), C37(H37), C38(H38)
3.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C42(H42A,H42B,H42C), C47(H47A,H47B,H47C), C51(H51A,H51B,
 H51C), C45(H45A,H45B,H45C), C50(H50A,H50B,H50C), C46(H46A,H46B,H46C), C49(H49A,
 H49B,H49C)
;
_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
Cl1 Cl 0.97955(10) 0.90478(14) 0.37640(8) 0.1417(5) Uani 1 1 d D . . . .
O32 O 0.26540(12) 0.50375(10) 0.24497(10) 0.0431(3) Uani 1 1 d . . . . .
Cl2 Cl 1.23441(15) 1.00348(19) 0.25936(14) 0.1905(9) Uani 1 1 d D . . . .
C6 C 0.34912(16) 0.44046(14) 0.14392(13) 0.0353(4) Uani 1 1 d . . . . .
C8 C 0.51045(16) 0.75270(14) 0.25625(13) 0.0375(4) Uani 1 1 d . . . . .
H8 H 0.567795 0.773976 0.231786 0.045 Uiso 1 1 calc R U . . .
C5 C 0.34167(17) 0.34978(14) 0.08413(13) 0.0378(4) Uani 1 1 d . . . . .
H5 H 0.396101 0.361599 0.056645 0.045 Uiso 1 1 calc R U . . .
C1 C 0.26719(16) 0.42136(14) 0.18431(13) 0.0360(4) Uani 1 1 d . . . . .
C2 C 0.17966(17) 0.31537(14) 0.16597(14) 0.0382(4) Uani 1 1 d . . . . .
C11 C 0.33896(17) 0.68917(14) 0.32805(14) 0.0370(4) Uani 1 1 d . . . . .
C7 C 0.43324(16) 0.64090(14) 0.22972(13) 0.0349(4) Uani 1 1 d . . . . .
C12 C 0.34746(16) 0.61099(14) 0.26637(13) 0.0357(4) Uani 1 1 d . . . . .
C9 C 0.50595(17) 0.83386(14) 0.31740(14) 0.0377(4) Uani 1 1 d . . . . .
C27 C 0.24673(17) 0.65658(14) 0.36753(14) 0.0380(4) Uani 1 1 d . . . . .
C13 C 0.09003(17) 0.29369(14) 0.20814(14) 0.0388(4) Uani 1 1 d . . . . .
C3 C 0.17659(17) 0.22759(14) 0.10536(14) 0.0409(4) Uani 1 1 d . . . . .
H3 H 0.118698 0.156658 0.092557 0.049 Uiso 1 1 calc R U . . .
C10 C 0.41882(17) 0.79950(14) 0.35233(14) 0.0394(4) Uani 1 1 d . . . . .
H10 H 0.413760 0.852203 0.393414 0.047 Uiso 1 1 calc R U . . .
C40 C 0.11965(18) 0.62695(15) 0.30277(15) 0.0419(4) Uani 1 1 d . . . . .
C26 C -0.03690(18) 0.26427(14) 0.14349(15) 0.0411(4) Uani 1 1 d . . . . .
C4 C 0.25695(17) 0.24231(14) 0.06337(14) 0.0385(4) Uani 1 1 d . . . . .
C28 C 0.28773(18) 0.66065(14) 0.47021(14) 0.0400(4) Uani 1 1 d . . . . .
C41 C 0.44369(16) 0.55640(13) 0.16207(13) 0.0350(4) Uani 1 1 d . . . . .
C14 C 0.13096(18) 0.29650(15) 0.31063(15) 0.0434(4) Uani 1 1 d . . . . .
C21 C -0.12472(19) 0.23207(16) 0.18204(17) 0.0472(5) Uani 1 1 d . . . . .
C43 C 0.57453(18) 0.55542(16) 0.21079(17) 0.0483(5) Uani 1 1 d . . . . .
H43A H 0.580834 0.502301 0.168010 0.072 Uiso 1 1 calc R U . . .
H43B H 0.591152 0.535249 0.273701 0.072 Uiso 1 1 calc R U . . .
H43C H 0.633557 0.628109 0.221179 0.072 Uiso 1 1 calc R U . . .
C29 C 0.4143(2) 0.68852(17) 0.53923(16) 0.0513(5) Uani 1 1 d . . . . .
H29 H 0.473186 0.703241 0.516174 0.062 Uiso 1 1 calc R U . . .
C33 C 0.1990(2) 0.63578(15) 0.50836(16) 0.0462(5) Uani 1 1 d . . . . .
C35 C 0.03292(19) 0.60307(17) 0.34251(17) 0.0485(5) Uani 1 1 d . . . . .
C44 C 0.25501(19) 0.14670(15) -0.00313(15) 0.0448(5) Uani 1 1 d . . . . .
C48 C 0.59313(18) 0.95572(14) 0.34224(15) 0.0443(5) Uani 1 1 d . . . . .
C19 C 0.0415(2) 0.26301(17) 0.34767(16) 0.0490(5) Uani 1 1 d . . . . .
C34 C 0.0748(2) 0.60841(18) 0.44383(17) 0.0521(5) Uani 1 1 d . . . . .
H34 H 0.018123 0.593235 0.469178 0.063 Uiso 1 1 calc R U . . .
C20 C -0.0831(2) 0.23121(18) 0.28222(17) 0.0529(5) Uani 1 1 d . . . . .
H20 H -0.140675 0.208573 0.306370 0.063 Uiso 1 1 calc R U . . .
C25 C -0.0843(2) 0.26312(17) 0.03958(17) 0.0525(5) Uani 1 1 d . . . . .
H25 H -0.029514 0.284353 0.012706 0.063 Uiso 1 1 calc R U . . .
C42 C 0.4173(2) 0.58946(16) 0.06145(15) 0.0477(5) Uani 1 1 d . . . . .
H42A H 0.475968 0.662486 0.072249 0.072 Uiso 1 1 calc R U . . .
H42B H 0.335126 0.589527 0.030717 0.072 Uiso 1 1 calc R U . . .
H42C H 0.424343 0.536973 0.018657 0.072 Uiso 1 1 calc R U . . .
C32 C 0.2422(2) 0.64273(19) 0.61304(18) 0.0568(6) Uani 1 1 d . . . . .
H32 H 0.185612 0.627253 0.638505 0.068 Uiso 1 1 calc R U . . .
C39 C 0.0724(2) 0.62141(19) 0.19833(17) 0.0542(5) Uani 1 1 d . . . . .
H39 H 0.126544 0.635725 0.170493 0.065 Uiso 1 1 calc R U . . .
C15 C 0.2580(2) 0.3284(2) 0.38043(17) 0.0565(5) Uani 1 1 d . . . . .
H15 H 0.317911 0.350232 0.358630 0.068 Uiso 1 1 calc R U . . .
C22 C -0.2532(2) 0.19980(19) 0.1156(2) 0.0604(6) Uani 1 1 d . . . . .
H22 H -0.310549 0.178720 0.140090 0.072 Uiso 1 1 calc R U . . .
C31 C 0.3630(3) 0.6712(2) 0.67527(18) 0.0634(6) Uani 1 1 d . . . . .
H31 H 0.388979 0.675911 0.743110 0.076 Uiso 1 1 calc R U . . .
C30 C 0.4508(2) 0.6940(2) 0.63850(18) 0.0623(6) Uani 1 1 d . . . . .
H30 H 0.533983 0.712957 0.682178 0.075 Uiso 1 1 calc R U . . .
C36 C -0.0947(2) 0.5779(2) 0.2770(2) 0.0659(6) Uani 1 1 d . . . . .
H36 H -0.151207 0.563728 0.302519 0.079 Uiso 1 1 calc R U . . .
C23 C -0.2930(2) 0.1993(2) 0.0177(2) 0.0657(6) Uani 1 1 d . . . . .
H23 H -0.377193 0.177557 -0.024380 0.079 Uiso 1 1 calc R U . . .
C24 C -0.2075(2) 0.2318(2) -0.0209(2) 0.0636(6) Uani 1 1 d . . . . .
H24 H -0.235698 0.231733 -0.088296 0.076 Uiso 1 1 calc R U . . .
C18 C 0.0834(3) 0.2615(2) 0.45033(19) 0.0652(6) Uani 1 1 d . . . . .
H18 H 0.025717 0.238769 0.474354 0.078 Uiso 1 1 calc R U . . .
C47 C 0.1463(3) 0.03914(18) -0.0276(2) 0.0758(8) Uani 1 1 d . . . . .
H47A H 0.070653 0.051997 -0.056973 0.114 Uiso 1 1 calc R U . . .
H47B H 0.155053 0.014087 0.032377 0.114 Uiso 1 1 calc R U . . .
H47C H 0.144522 -0.016588 -0.073732 0.114 Uiso 1 1 calc R U . . .
C51 C 0.5940(3) 1.02728(18) 0.4268(2) 0.0710(7) Uani 1 1 d . . . . .
H51A H 0.615662 0.995899 0.484342 0.106 Uiso 1 1 calc R U . . .
H51B H 0.513353 1.029578 0.406278 0.106 Uiso 1 1 calc R U . . .
H51C H 0.653508 1.101394 0.442911 0.106 Uiso 1 1 calc R U . . .
C45 C 0.2418(3) 0.1765(2) -0.10235(19) 0.0714(7) Uani 1 1 d . . . . .
H45A H 0.238899 0.115887 -0.144401 0.107 Uiso 1 1 calc R U . . .
H45B H 0.311311 0.242119 -0.090291 0.107 Uiso 1 1 calc R U . . .
H45C H 0.166928 0.190017 -0.134586 0.107 Uiso 1 1 calc R U . . .
C16 C 0.2932(3) 0.3276(3) 0.47842(19) 0.0725(7) Uani 1 1 d . . . . .
H16 H 0.376774 0.350516 0.522812 0.087 Uiso 1 1 calc R U . . .
C17 C 0.2040(3) 0.2922(3) 0.5134(2) 0.0752(7) Uani 1 1 d . . . . .
H17 H 0.228988 0.290224 0.580147 0.090 Uiso 1 1 calc R U . . .
C50 C 0.7260(2) 0.9634(2) 0.3753(2) 0.0755(8) Uani 1 1 d . . . . .
H50A H 0.780464 1.040219 0.395190 0.113 Uiso 1 1 calc R U . . .
H50B H 0.730737 0.926098 0.321018 0.113 Uiso 1 1 calc R U . . .
H50C H 0.750200 0.928804 0.430578 0.113 Uiso 1 1 calc R U . . .
C37 C -0.1345(2) 0.5744(3) 0.1789(2) 0.0764(8) Uani 1 1 d . . . . .
H37 H -0.217853 0.557927 0.137488 0.092 Uiso 1 1 calc R U . . .
C38 C -0.0500(2) 0.5956(3) 0.1387(2) 0.0716(7) Uani 1 1 d . . . . .
H38 H -0.078545 0.591932 0.070726 0.086 Uiso 1 1 calc R U . . .
C46 C 0.3757(3) 0.1297(3) 0.0482(2) 0.0886(10) Uani 1 1 d . . . . .
H46A H 0.383216 0.107536 0.109101 0.133 Uiso 1 1 calc R U . . .
H46B H 0.443471 0.198008 0.062788 0.133 Uiso 1 1 calc R U . . .
H46C H 0.376872 0.072788 0.005249 0.133 Uiso 1 1 calc R U . . .
C49 C 0.5515(3) 1.0023(2) 0.2502(2) 0.0831(9) Uani 1 1 d . . . . .
H49A H 0.467846 0.996594 0.228910 0.125 Uiso 1 1 calc R U . . .
H49B H 0.555986 0.960763 0.197840 0.125 Uiso 1 1 calc R U . . .
H49C H 0.604413 1.079000 0.265394 0.125 Uiso 1 1 calc R U . . .
C52 C 1.0898(5) 0.9005(4) 0.3246(4) 0.178(3) Uani 1 1 d D . . . .
H52A H 1.160180 0.886395 0.371349 0.214 Uiso 1 1 calc R U . . .
H52B H 1.049085 0.846964 0.261418 0.214 Uiso 1 1 calc R U . . .
C53 C 1.1208(6) 1.0069(4) 0.3143(3) 0.171(3) Uani 1 1 d D . . . .
H53A H 1.162035 1.060308 0.377604 0.205 Uiso 1 1 calc R U . . .
H53B H 1.050244 1.021046 0.268083 0.205 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C52 1.892(7) . ?
O32 C1 1.376(2) . ?
O32 C12 1.375(2) . ?
Cl2 C53 1.962(7) . ?
C6 C5 1.390(2) . ?
C6 C1 1.388(2) . ?
C6 C41 1.528(2) . ?
C8 H8 0.9300 . ?
C8 C7 1.393(2) . ?
C8 C9 1.388(2) . ?
C5 H5 0.9300 . ?
C5 C4 1.391(2) . ?
C1 C2 1.397(2) . ?
C2 C13 1.495(2) . ?
C2 C3 1.396(2) . ?
C11 C12 1.394(2) . ?
C11 C27 1.496(2) . ?
C11 C10 1.391(2) . ?
C7 C12 1.390(2) . ?
C7 C41 1.526(2) . ?
C9 C10 1.390(3) . ?
C9 C48 1.536(2) . ?
C27 C40 1.413(3) . ?
C27 C28 1.411(3) . ?
C13 C26 1.412(3) . ?
C13 C14 1.411(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.391(3) . ?
C10 H10 0.9300 . ?
C40 C35 1.434(3) . ?
C40 C39 1.427(3) . ?
C26 C21 1.436(3) . ?
C26 C25 1.430(3) . ?
C4 C44 1.533(2) . ?
C28 C29 1.425(3) . ?
C28 C33 1.438(3) . ?
C41 C43 1.533(3) . ?
C41 C42 1.540(3) . ?
C14 C19 1.439(3) . ?
C14 C15 1.426(3) . ?
C21 C20 1.386(3) . ?
C21 C22 1.428(3) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C29 H29 0.9300 . ?
C29 C30 1.365(3) . ?
C33 C34 1.388(3) . ?
C33 C32 1.431(3) . ?
C35 C34 1.388(3) . ?
C35 C36 1.430(3) . ?
C44 C47 1.520(3) . ?
C44 C45 1.530(3) . ?
C44 C46 1.513(3) . ?
C48 C51 1.525(3) . ?
C48 C50 1.531(3) . ?
C48 C49 1.515(3) . ?
C19 C20 1.387(3) . ?
C19 C18 1.422(3) . ?
C34 H34 0.9300 . ?
C20 H20 0.9300 . ?
C25 H25 0.9300 . ?
C25 C24 1.359(3) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C32 H32 0.9300 . ?
C32 C31 1.345(4) . ?
C39 H39 0.9300 . ?
C39 C38 1.359(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.362(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.351(4) . ?
C31 H31 0.9300 . ?
C31 C30 1.412(4) . ?
C30 H30 0.9300 . ?
C36 H36 0.9300 . ?
C36 C37 1.348(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.413(4) . ?
C24 H24 0.9300 . ?
C18 H18 0.9300 . ?
C18 C17 1.342(4) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C16 H16 0.9300 . ?
C16 C17 1.415(4) . ?
C17 H17 0.9300 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C37 H37 0.9300 . ?
C37 C38 1.414(4) . ?
C38 H38 0.9300 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 C53 1.353(7) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?

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
C12 O32 C1 119.00(13) . . ?
C5 C6 C41 120.18(15) . . ?
C1 C6 C5 117.59(15) . . ?
C1 C6 C41 122.22(15) . . ?
C7 C8 H8 118.4 . . ?
C9 C8 H8 118.4 . . ?
C9 C8 C7 123.19(16) . . ?
C6 C5 H5 118.3 . . ?
C6 C5 C4 123.31(16) . . ?
C4 C5 H5 118.3 . . ?
O32 C1 C6 123.30(15) . . ?
O32 C1 C2 114.88(15) . . ?
C6 C1 C2 121.82(15) . . ?
C1 C2 C13 122.44(15) . . ?
C3 C2 C1 117.98(16) . . ?
C3 C2 C13 119.58(15) . . ?
C12 C11 C27 121.50(15) . . ?
C10 C11 C12 118.25(16) . . ?
C10 C11 C27 120.25(15) . . ?
C8 C7 C41 120.16(15) . . ?
C12 C7 C8 117.50(15) . . ?
C12 C7 C41 122.33(14) . . ?
O32 C12 C11 115.18(15) . . ?
O32 C12 C7 123.15(15) . . ?
C7 C12 C11 121.67(15) . . ?
C8 C9 C10 117.02(15) . . ?
C8 C9 C48 120.12(16) . . ?
C10 C9 C48 122.86(16) . . ?
C40 C27 C11 119.91(17) . . ?
C28 C27 C11 119.74(17) . . ?
C28 C27 C40 120.29(16) . . ?
C26 C13 C2 119.31(17) . . ?
C14 C13 C2 120.28(17) . . ?
C14 C13 C26 120.32(16) . . ?
C2 C3 H3 118.8 . . ?
C4 C3 C2 122.42(16) . . ?
C4 C3 H3 118.8 . . ?
C11 C10 H10 118.8 . . ?
C9 C10 C11 122.38(16) . . ?
C9 C10 H10 118.8 . . ?
C27 C40 C35 119.49(18) . . ?
C27 C40 C39 122.96(17) . . ?
C39 C40 C35 117.54(18) . . ?
C13 C26 C21 119.42(18) . . ?
C13 C26 C25 123.29(17) . . ?
C25 C26 C21 117.29(18) . . ?
C5 C4 C3 116.88(16) . . ?
C5 C4 C44 120.07(16) . . ?
C3 C4 C44 123.05(15) . . ?
C27 C28 C29 123.06(17) . . ?
C27 C28 C33 119.27(18) . . ?
C29 C28 C33 117.66(18) . . ?
C6 C41 C43 109.73(14) . . ?
C6 C41 C42 108.94(14) . . ?
C7 C41 C6 109.99(13) . . ?
C7 C41 C43 109.69(15) . . ?
C7 C41 C42 108.99(14) . . ?
C43 C41 C42 109.48(15) . . ?
C13 C14 C19 119.36(18) . . ?
C13 C14 C15 123.20(17) . . ?
C15 C14 C19 117.42(19) . . ?
C20 C21 C26 119.36(19) . . ?
C20 C21 C22 121.60(19) . . ?
C22 C21 C26 119.0(2) . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C28 C29 H29 119.3 . . ?
C30 C29 C28 121.4(2) . . ?
C30 C29 H29 119.3 . . ?
C34 C33 C28 119.61(18) . . ?
C34 C33 C32 121.65(19) . . ?
C32 C33 C28 118.7(2) . . ?
C34 C35 C40 119.55(19) . . ?
C34 C35 C36 121.42(19) . . ?
C36 C35 C40 119.0(2) . . ?
C47 C44 C4 112.19(16) . . ?
C47 C44 C45 106.88(19) . . ?
C45 C44 C4 109.58(16) . . ?
C46 C44 C4 109.13(18) . . ?
C46 C44 C47 110.3(2) . . ?
C46 C44 C45 108.7(2) . . ?
C51 C48 C9 112.13(16) . . ?
C51 C48 C50 107.2(2) . . ?
C50 C48 C9 110.24(16) . . ?
C49 C48 C9 108.86(17) . . ?
C49 C48 C51 108.9(2) . . ?
C49 C48 C50 109.5(2) . . ?
C20 C19 C14 119.28(19) . . ?
C20 C19 C18 121.82(19) . . ?
C18 C19 C14 118.9(2) . . ?
C33 C34 H34 119.1 . . ?
C35 C34 C33 121.78(18) . . ?
C35 C34 H34 119.1 . . ?
C21 C20 C19 122.16(18) . . ?
C21 C20 H20 118.9 . . ?
C19 C20 H20 118.9 . . ?
C26 C25 H25 119.2 . . ?
C24 C25 C26 121.7(2) . . ?
C24 C25 H25 119.2 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C33 C32 H32 119.4 . . ?
C31 C32 C33 121.2(2) . . ?
C31 C32 H32 119.4 . . ?
C40 C39 H39 119.3 . . ?
C38 C39 C40 121.4(2) . . ?
C38 C39 H39 119.3 . . ?
C14 C15 H15 119.4 . . ?
C16 C15 C14 121.3(2) . . ?
C16 C15 H15 119.4 . . ?
C21 C22 H22 119.4 . . ?
C23 C22 C21 121.2(2) . . ?
C23 C22 H22 119.4 . . ?
C32 C31 H31 119.7 . . ?
C32 C31 C30 120.6(2) . . ?
C30 C31 H31 119.7 . . ?
C29 C30 C31 120.4(2) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C35 C36 H36 119.4 . . ?
C37 C36 C35 121.1(2) . . ?
C37 C36 H36 119.4 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.3(2) . . ?
C24 C23 H23 119.8 . . ?
C25 C24 C23 120.5(2) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C19 C18 H18 119.2 . . ?
C17 C18 C19 121.6(2) . . ?
C17 C18 H18 119.2 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C48 C51 H51A 109.5 . . ?
C48 C51 H51B 109.5 . . ?
C48 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C15 C16 H16 119.6 . . ?
C15 C16 C17 120.7(2) . . ?
C17 C16 H16 119.6 . . ?
C18 C17 C16 120.1(2) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C36 C37 H37 119.9 . . ?
C36 C37 C38 120.3(2) . . ?
C38 C37 H37 119.9 . . ?
C39 C38 C37 120.7(2) . . ?
C39 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
Cl1 C52 H52A 112.5 . . ?
Cl1 C52 H52B 112.5 . . ?
H52A C52 H52B 110.0 . . ?
C53 C52 Cl1 96.5(4) . . ?
C53 C52 H52A 112.5 . . ?
C53 C52 H52B 112.5 . . ?
Cl2 C53 H53A 112.3 . . ?
Cl2 C53 H53B 112.4 . . ?
C52 C53 Cl2 97.0(4) . . ?
C52 C53 H53A 112.4 . . ?
C52 C53 H53B 112.4 . . ?
H53A C53 H53B 109.9 . . ?

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
Cl1 C52 C53 Cl2 -179.52(18) . . . . ?
O32 C1 C2 C13 0.7(3) . . . . ?
O32 C1 C2 C3 -179.70(16) . . . . ?
C6 C5 C4 C3 0.2(3) . . . . ?
C6 C5 C4 C44 -179.82(17) . . . . ?
C6 C1 C2 C13 -179.41(18) . . . . ?
C6 C1 C2 C3 0.2(3) . . . . ?
C8 C7 C12 O32 179.41(16) . . . . ?
C8 C7 C12 C11 -0.5(3) . . . . ?
C8 C7 C41 C6 -179.77(16) . . . . ?
C8 C7 C41 C43 59.5(2) . . . . ?
C8 C7 C41 C42 -60.4(2) . . . . ?
C8 C9 C10 C11 0.1(3) . . . . ?
C8 C9 C48 C51 -167.8(2) . . . . ?
C8 C9 C48 C50 -48.4(3) . . . . ?
C8 C9 C48 C49 71.7(3) . . . . ?
C5 C6 C1 O32 179.68(17) . . . . ?
C5 C6 C1 C2 -0.2(3) . . . . ?
C5 C6 C41 C7 180.00(16) . . . . ?
C5 C6 C41 C43 -59.2(2) . . . . ?
C5 C6 C41 C42 60.6(2) . . . . ?
C5 C4 C44 C47 -172.8(2) . . . . ?
C5 C4 C44 C45 -54.3(3) . . . . ?
C5 C4 C44 C46 64.6(3) . . . . ?
C1 O32 C12 C11 179.78(16) . . . . ?
C1 O32 C12 C7 -0.1(3) . . . . ?
C1 C6 C5 C4 0.0(3) . . . . ?
C1 C6 C41 C7 0.9(2) . . . . ?
C1 C6 C41 C43 121.67(19) . . . . ?
C1 C6 C41 C42 -118.48(19) . . . . ?
C1 C2 C13 C26 111.3(2) . . . . ?
C1 C2 C13 C14 -72.2(2) . . . . ?
C1 C2 C3 C4 0.0(3) . . . . ?
C2 C13 C26 C21 173.52(15) . . . . ?
C2 C13 C26 C25 -5.6(3) . . . . ?
C2 C13 C14 C19 -172.93(16) . . . . ?
C2 C13 C14 C15 5.3(3) . . . . ?
C2 C3 C4 C5 -0.2(3) . . . . ?
C2 C3 C4 C44 179.82(18) . . . . ?
C11 C27 C40 C35 -175.85(16) . . . . ?
C11 C27 C40 C39 3.0(3) . . . . ?
C11 C27 C28 C29 -3.8(3) . . . . ?
C11 C27 C28 C33 176.19(15) . . . . ?
C7 C8 C9 C10 -0.3(3) . . . . ?
C7 C8 C9 C48 -179.24(17) . . . . ?
C12 O32 C1 C6 0.8(3) . . . . ?
C12 O32 C1 C2 -179.37(16) . . . . ?
C12 C11 C27 C40 -71.7(2) . . . . ?
C12 C11 C27 C28 111.3(2) . . . . ?
C12 C11 C10 C9 0.0(3) . . . . ?
C12 C7 C41 C6 -0.3(2) . . . . ?
C12 C7 C41 C43 -121.10(19) . . . . ?
C12 C7 C41 C42 119.05(19) . . . . ?
C9 C8 C7 C12 0.5(3) . . . . ?
C9 C8 C7 C41 180.00(17) . . . . ?
C27 C11 C12 O32 0.2(3) . . . . ?
C27 C11 C12 C7 -179.85(17) . . . . ?
C27 C11 C10 C9 -179.92(17) . . . . ?
C27 C40 C35 C34 -0.6(3) . . . . ?
C27 C40 C35 C36 177.31(19) . . . . ?
C27 C40 C39 C38 -178.1(2) . . . . ?
C27 C28 C29 C30 178.50(18) . . . . ?
C27 C28 C33 C34 -0.1(3) . . . . ?
C27 C28 C33 C32 -178.57(16) . . . . ?
C13 C2 C3 C4 179.64(18) . . . . ?
C13 C26 C21 C20 0.4(3) . . . . ?
C13 C26 C21 C22 -178.47(17) . . . . ?
C13 C26 C25 C24 178.43(19) . . . . ?
C13 C14 C19 C20 -1.6(3) . . . . ?
C13 C14 C19 C18 177.30(19) . . . . ?
C13 C14 C15 C16 -178.5(2) . . . . ?
C3 C2 C13 C26 -68.3(2) . . . . ?
C3 C2 C13 C14 108.2(2) . . . . ?
C3 C4 C44 C47 7.1(3) . . . . ?
C3 C4 C44 C45 125.7(2) . . . . ?
C3 C4 C44 C46 -115.5(2) . . . . ?
C10 C11 C12 O32 -179.66(16) . . . . ?
C10 C11 C12 C7 0.2(3) . . . . ?
C10 C11 C27 C40 108.2(2) . . . . ?
C10 C11 C27 C28 -68.8(2) . . . . ?
C10 C9 C48 C51 13.4(3) . . . . ?
C10 C9 C48 C50 132.7(2) . . . . ?
C10 C9 C48 C49 -107.2(2) . . . . ?
C40 C27 C28 C29 179.18(16) . . . . ?
C40 C27 C28 C33 -0.8(2) . . . . ?
C40 C35 C34 C33 -0.4(3) . . . . ?
C40 C35 C36 C37 1.2(4) . . . . ?
C40 C39 C38 C37 0.6(4) . . . . ?
C26 C13 C14 C19 3.5(3) . . . . ?
C26 C13 C14 C15 -178.22(18) . . . . ?
C26 C21 C20 C19 1.5(3) . . . . ?
C26 C21 C22 C23 -0.1(3) . . . . ?
C26 C25 C24 C23 0.1(4) . . . . ?
C28 C27 C40 C35 1.1(3) . . . . ?
C28 C27 C40 C39 179.96(17) . . . . ?
C28 C29 C30 C31 0.5(3) . . . . ?
C28 C33 C34 C35 0.7(3) . . . . ?
C28 C33 C32 C31 -0.4(3) . . . . ?
C41 C6 C5 C4 -179.15(17) . . . . ?
C41 C6 C1 O32 -1.2(3) . . . . ?
C41 C6 C1 C2 178.92(17) . . . . ?
C41 C7 C12 O32 -0.1(3) . . . . ?
C41 C7 C12 C11 -179.95(16) . . . . ?
C14 C13 C26 C21 -3.0(3) . . . . ?
C14 C13 C26 C25 177.95(17) . . . . ?
C14 C19 C20 C21 -1.0(3) . . . . ?
C14 C19 C18 C17 1.1(4) . . . . ?
C14 C15 C16 C17 1.6(4) . . . . ?
C21 C26 C25 C24 -0.7(3) . . . . ?
C21 C22 C23 C24 -0.4(4) . . . . ?
C29 C28 C33 C34 179.89(17) . . . . ?
C29 C28 C33 C32 1.4(3) . . . . ?
C33 C28 C29 C30 -1.5(3) . . . . ?
C33 C32 C31 C30 -0.6(3) . . . . ?
C35 C40 C39 C38 0.7(3) . . . . ?
C35 C36 C37 C38 0.0(5) . . . . ?
C48 C9 C10 C11 178.94(18) . . . . ?
C19 C14 C15 C16 -0.2(3) . . . . ?
C19 C18 C17 C16 0.3(4) . . . . ?
C34 C33 C32 C31 -178.8(2) . . . . ?
C34 C35 C36 C37 179.1(2) . . . . ?
C20 C21 C22 C23 -179.0(2) . . . . ?
C20 C19 C18 C17 179.9(2) . . . . ?
C25 C26 C21 C20 179.59(17) . . . . ?
C25 C26 C21 C22 0.7(3) . . . . ?
C32 C33 C34 C35 179.12(19) . . . . ?
C32 C31 C30 C29 0.6(4) . . . . ?
C39 C40 C35 C34 -179.43(19) . . . . ?
C39 C40 C35 C36 -1.6(3) . . . . ?
C15 C14 C19 C20 -179.94(19) . . . . ?
C15 C14 C19 C18 -1.1(3) . . . . ?
C15 C16 C17 C18 -1.6(5) . . . . ?
C22 C21 C20 C19 -179.6(2) . . . . ?
C22 C23 C24 C25 0.4(4) . . . . ?
C36 C35 C34 C33 -178.2(2) . . . . ?
C36 C37 C38 C39 -1.0(5) . . . . ?
C18 C19 C20 C21 -179.8(2) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.656
_oxdiff_exptl_absorpt_empirical_full_min 0.389
####################################################################### 
# 
# 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_Y
_database_code_depnum_ccdc_archive 'CCDC 2180337'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2022-06-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2022-06-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_chemical_formula_moiety         'C37 H38 O'
_chemical_formula_sum            'C37 H38 O'
_chemical_formula_weight         498.713
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x+1/2,-y+1/2,-z
3 -x,y+1/2,-z+1/2
4 -x+1/2,-y,z+1/2
5 -x,-y,-z
6 -x-1/2,y-1/2,z
7 x,-y-1/2,z-1/2
8 x-1/2,y,-z-1/2

_symmetry_Int_Tables_number      61
_cell_length_a                   13.254(3)
_cell_length_b                   11.5590(16)
_cell_length_c                   38.103(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5837.6(18)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5740
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      2.40
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6181
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0775 before and 0.0510 after correction.
The Ratio of minimum to maximum transmission is 0.8292.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             2144.855
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.9996
_diffrn_reflns_Laue_measured_fraction_max 0.9996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            44149
_diffrn_reflns_point_group_measured_fraction_full 0.9996
_diffrn_reflns_point_group_measured_fraction_max 0.9996
_diffrn_reflns_theta_full        24.9997
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.87
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              45
_reflns_limit_l_min              0
_reflns_number_gt                3355
_reflns_number_total             5126
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.2772
_refine_diff_density_min         -0.2432
_refine_diff_density_rms         0.0612
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             10.8802
_refine_ls_goodness_of_fit_ref   1.0934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    86
_refine_ls_number_parameters     413
_refine_ls_number_reflns         5126
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0580
_refine_ls_restrained_S_all      1.0885
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0539P)²+1.9776P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1495
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C30-C31 \\sim C30-C31a
 with sigma of 0.02
 C30-C32 \\sim C30-C32a
 with sigma of 0.02
 C30-C33 \\sim C30-C33a
 with sigma of 0.02
3. Rigid bond restraints
 C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C32) \\sim Ueq, Uanis(C32a) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C33) \\sim Ueq, Uanis(C33a) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C31) \\sim Ueq, Uanis(C31a) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(C35a)=Sof(H35d)=Sof(H35e)=Sof(H35f)=Sof(C36a)=Sof(H36d)=Sof(H36e)=
 Sof(H36f)=Sof(C37a)=Sof(H37d)=Sof(H37e)=Sof(H37f)=Sof(H35d)=Sof(H35e)=
 Sof(H35f)=Sof(H36d)=Sof(H36e)=Sof(H36f)=Sof(H37d)=Sof(H37e)=Sof(H37f)=1-FVAR(1)
 Sof(C35)=Sof(H35a)=Sof(H35b)=Sof(H35c)=Sof(C36)=Sof(H36a)=Sof(H36b)=Sof(H36c)=
 Sof(C37)=Sof(H37a)=Sof(H37b)=Sof(H37c)=Sof(H35a)=Sof(H35b)=Sof(H35c)=Sof(H36a)=
 Sof(H36b)=Sof(H36c)=Sof(H37a)=Sof(H37b)=Sof(H37c)=FVAR(1)
 Sof(C31a)=Sof(C32a)=Sof(C33a)=Sof(H31d)=Sof(H31e)=Sof(H31f)=Sof(H32d)=
 Sof(H32e)=Sof(H32f)=Sof(H33d)=Sof(H33e)=Sof(H33f)=1-FVAR(2)
 Sof(C31)=Sof(C32)=Sof(C33)=Sof(H31a)=Sof(H31b)=Sof(H31c)=Sof(H32a)=Sof(H32b)=
 Sof(H32c)=Sof(H33a)=Sof(H33b)=Sof(H33c)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C12(H12), C11(H11), C9(H9), C26(H26), C17(H17), C16(H16),
 C15(H15), C14(H14), C21(H21), C22(H22), C23(H23), C24(H24)
6.b Idealised Me refined as rotating group:
 C28(H28a,H28b,H28c), C29(H29a,H29b,H29c), C31(H31a,H31b,H31c), C32(H32a,H32b,
 H32c), C33(H33a,H33b,H33c), C35(H35a,H35b,H35c), C35a(H35d,H35e,H35f),
 C36(H36a,H36b,H36c), C36a(H36d,H36e,H36f), C37(H37a,H37b,H37c), C37a(H37d,H37e,
 H37f), C31a(H31d,H31e,H31f), C32a(H32d,H32e,H32f), C33a(H33d,H33e,H33f)
;
_atom_sites_special_details      
;
The structure was solved using Direct Methods (ShelXS). RE = 0.3, Nqual =  -1, Ralpha = 0.065
;
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_disorder_group
O1 O 0.49277(10) 0.54210(14) 0.14574(3) 0.0475(4) Uani 1.000000 . . .
C1 C 0.52303(15) 0.57767(19) 0.11288(5) 0.0386(5) Uani 1.000000 . . .
C2 C 0.46093(16) 0.6598(2) 0.09711(6) 0.0445(6) Uani 1.000000 . . .
C3 C 0.48730(18) 0.6998(2) 0.06424(6) 0.0519(6) Uani 1.000000 . . .
C4 C 0.57243(17) 0.6622(2) 0.04641(5) 0.0464(6) Uani 1.000000 . . .
C5 C 0.63077(16) 0.5801(2) 0.06311(5) 0.0434(6) Uani 1.000000 . . .
C6 C 0.60840(15) 0.53557(19) 0.09631(5) 0.0370(5) Uani 1.000000 . . .
C7 C 0.55244(15) 0.46452(18) 0.16378(5) 0.0371(5) Uani 1.000000 . . .
C8 C 0.63854(15) 0.41587(18) 0.14990(5) 0.0356(5) Uani 1.000000 . . .
C9 C 0.69050(16) 0.33804(18) 0.17148(5) 0.0416(5) Uani 1.000000 . . .
C10 C 0.66006(17) 0.30872(18) 0.20516(5) 0.0405(5) Uani 1.000000 . . .
C11 C 0.57281(17) 0.3612(2) 0.21762(6) 0.0466(6) Uani 1.000000 . . .
C12 C 0.51919(17) 0.4376(2) 0.19722(5) 0.0450(6) Uani 1.000000 . . .
C13 C 0.1848(2) 0.7156(4) 0.11966(8) 0.0802(11) Uani 1.000000 . . .
C14 C 0.0886(2) 0.6650(5) 0.11065(10) 0.1120(16) Uani 1.000000 . . .
C15 C 0.0818(3) 0.5739(5) 0.08917(11) 0.1224(18) Uani 1.000000 . . .
C16 C 0.1684(2) 0.5228(3) 0.07538(8) 0.0934(11) Uani 1.000000 . . .
C17 C 0.2610(2) 0.5659(3) 0.08304(7) 0.0716(9) Uani 1.000000 . . .
C18 C 0.27354(18) 0.6628(3) 0.10557(7) 0.0593(7) Uani 1.000000 . . .
C19 C 0.36876(17) 0.7067(2) 0.11482(6) 0.0502(6) Uani 1.000000 . . .
C20 C 0.3779(2) 0.7989(2) 0.13868(6) 0.0578(7) Uani 1.000000 . . .
C21 C 0.4723(2) 0.8412(3) 0.15055(7) 0.0700(8) Uani 1.000000 . . .
C22 C 0.4785(3) 0.9319(3) 0.17282(8) 0.0940(11) Uani 1.000000 . . .
C23 C 0.3910(4) 0.9897(3) 0.18426(10) 0.1098(13) Uani 1.000000 . . .
C24 C 0.2996(4) 0.9521(4) 0.17376(10) 0.1023(13) Uani 1.000000 . . .
C25 C 0.2883(2) 0.8544(3) 0.15155(8) 0.0754(9) Uani 1.000000 . . .
C26 C 0.1945(3) 0.8098(4) 0.14156(9) 0.0924(12) Uani 1.000000 . . .
C27 C 0.67562(16) 0.44393(19) 0.11296(5) 0.0410(5) Uani 1.000000 . . .
C28 C 0.78445(17) 0.4892(3) 0.11443(7) 0.0633(8) Uani 1.000000 . . .
C29 C 0.6724(2) 0.3334(2) 0.09034(6) 0.0679(8) Uani 1.000000 . . .
C30 C 0.5972(2) 0.7115(2) 0.01008(6) 0.0586(7) Uani 1.000000 D . .
C31 C 0.5177(3) 0.6754(4) -0.01589(8) 0.0967(17) Uani 0.861(6) D U 1
C32 C 0.6003(4) 0.8450(3) 0.01273(9) 0.0913(16) Uani 0.861(6) D U 1
C33 C 0.7005(3) 0.6745(4) -0.00272(9) 0.0917(16) Uani 0.861(6) D U 1
C34 C 0.72083(19) 0.2248(2) 0.22797(6) 0.0514(6) Uani 1.000000 . U .
C35 C 0.7568(8) 0.1257(6) 0.20693(14) 0.112(4) Uani 0.720(15) . . 1
C35a C 0.8346(13) 0.202(2) 0.2113(4) 0.111(9) Uani 0.280(15) . . 2
C36 C 0.8072(5) 0.2904(5) 0.2441(2) 0.096(3) Uani 0.720(15) . . 1
C36a C 0.744(2) 0.2673(18) 0.2622(4) 0.133(14) Uani 0.280(15) . . 2
C37 C 0.6562(4) 0.1778(6) 0.25871(16) 0.094(3) Uani 0.720(15) . . 1
C37a C 0.6746(19) 0.1070(13) 0.2273(7) 0.146(14) Uani 0.280(15) . . 2
C31a C 0.518(2) 0.797(2) -0.0036(7) 0.100(10) Uani 0.139(6) D U 2
C32a C 0.695(2) 0.777(3) 0.0090(10) 0.133(13) Uani 0.139(6) D U 2
C33a C 0.601(3) 0.606(2) -0.0173(7) 0.120(12) Uani 0.139(6) D U 2
H5 H 0.68806(16) 0.5530(2) 0.05167(5) 0.0521(7) Uiso 1.000000 R . .
H3 H 0.44607(18) 0.7545(2) 0.05355(6) 0.0623(8) Uiso 1.000000 R . .
H12 H 0.46054(17) 0.4713(2) 0.20590(5) 0.0540(7) Uiso 1.000000 R . .
H11 H 0.55028(17) 0.3443(2) 0.24016(6) 0.0560(7) Uiso 1.000000 R . .
H9 H 0.74887(16) 0.30397(18) 0.16272(5) 0.0499(6) Uiso 1.000000 R . .
H26 H 0.1363(3) 0.8452(4) 0.15004(9) 0.1109(15) Uiso 1.000000 R . .
H17 H 0.3177(2) 0.5311(3) 0.07330(7) 0.0859(10) Uiso 1.000000 R . .
H16 H 0.1626(2) 0.4586(3) 0.06081(8) 0.1121(14) Uiso 1.000000 R . .
H15 H 0.0187(3) 0.5443(5) 0.08338(11) 0.147(2) Uiso 1.000000 R . .
H14 H 0.0299(2) 0.6966(5) 0.12001(10) 0.1344(19) Uiso 1.000000 R . .
H21 H 0.5312(2) 0.8058(3) 0.14284(7) 0.0840(9) Uiso 1.000000 R . .
H22 H 0.5413(3) 0.9565(3) 0.18068(8) 0.1128(13) Uiso 1.000000 R . .
H23 H 0.3963(4) 1.0535(3) 0.19900(10) 0.1317(16) Uiso 1.000000 R . .
H24 H 0.2422(4) 0.9913(4) 0.18129(10) 0.1228(16) Uiso 1.000000 R . .
H28a H 0.8077(5) 0.5053(15) 0.09107(7) 0.0950(12) Uiso 1.000000 GR . .
H28b H 0.7866(3) 0.5588(9) 0.1282(4) 0.0950(12) Uiso 1.000000 GR . .
H28c H 0.8271(3) 0.4318(7) 0.1250(4) 0.0950(12) Uiso 1.000000 GR . .
H29a H 0.6044(3) 0.3048(9) 0.0894(4) 0.1018(12) Uiso 1.000000 GR . .
H29b H 0.6953(13) 0.3509(4) 0.06704(15) 0.1018(12) Uiso 1.000000 GR . .
H29c H 0.7153(11) 0.2756(6) 0.1006(3) 0.1018(12) Uiso 1.000000 GR . .
H31a H 0.5185(16) 0.5928(5) -0.0184(6) 0.145(3) Uiso 0.861(6) GR . 1
H31b H 0.4526(4) 0.700(2) -0.0077(4) 0.145(3) Uiso 0.861(6) GR . 1
H31c H 0.5312(13) 0.711(2) -0.0382(2) 0.145(3) Uiso 0.861(6) GR . 1
H32a H 0.5344(6) 0.8735(4) 0.0186(8) 0.137(2) Uiso 0.861(6) GR . 1
H32b H 0.6473(17) 0.8674(3) 0.0306(5) 0.137(2) Uiso 0.861(6) GR . 1
H32c H 0.621(2) 0.8769(3) -0.0094(2) 0.137(2) Uiso 0.861(6) GR . 1
H33a H 0.7500(4) 0.692(2) 0.0149(3) 0.138(2) Uiso 0.861(6) GR . 1
H33b H 0.7003(7) 0.5929(7) -0.0073(7) 0.138(2) Uiso 0.861(6) GR . 1
H33c H 0.7168(10) 0.716(2) -0.0239(4) 0.138(2) Uiso 0.861(6) GR . 1
H35a H 0.7001(8) 0.086(2) 0.1968(10) 0.168(6) Uiso 0.720(15) GR . 1
H35b H 0.800(3) 0.1531(7) 0.1886(8) 0.168(6) Uiso 0.720(15) GR . 1
H35c H 0.793(3) 0.073(2) 0.2218(3) 0.168(6) Uiso 0.720(15) GR . 1
H35d H 0.8284(13) 0.174(9) 0.1878(11) 0.166(14) Uiso 0.280(15) GR . 2
H35e H 0.872(3) 0.274(3) 0.211(3) 0.166(14) Uiso 0.280(15) GR . 2
H35f H 0.870(4) 0.146(8) 0.2254(17) 0.166(14) Uiso 0.280(15) GR . 2
H36a H 0.8503(17) 0.319(3) 0.2259(2) 0.145(5) Uiso 0.720(15) GR . 1
H36b H 0.7813(5) 0.354(2) 0.2576(9) 0.145(5) Uiso 0.720(15) GR . 1
H36c H 0.8450(19) 0.2398(10) 0.2591(9) 0.145(5) Uiso 0.720(15) GR . 1
H36d H 0.784(9) 0.336(8) 0.2603(4) 0.20(2) Uiso 0.280(15) GR . 2
H36e H 0.682(2) 0.285(12) 0.2744(14) 0.20(2) Uiso 0.280(15) GR . 2
H36f H 0.780(10) 0.209(5) 0.2750(14) 0.20(2) Uiso 0.280(15) GR . 2
H37a H 0.638(2) 0.2404(8) 0.2740(6) 0.141(5) Uiso 0.720(15) GR . 1
H37b H 0.5962(14) 0.142(3) 0.24957(17) 0.141(5) Uiso 0.720(15) GR . 1
H37c H 0.6944(11) 0.121(2) 0.2716(6) 0.141(5) Uiso 0.720(15) GR . 1
H37d H 0.609(5) 0.110(3) 0.238(4) 0.22(2) Uiso 0.280(15) GR . 2
H37e H 0.668(11) 0.082(6) 0.2034(7) 0.22(2) Uiso 0.280(15) GR . 2
H37f H 0.717(6) 0.054(3) 0.240(4) 0.22(2) Uiso 0.280(15) GR . 2
H31d H 0.452(3) 0.762(7) -0.003(5) 0.151(14) Uiso 0.139(6) GR . 2
H31e H 0.518(11) 0.865(8) 0.011(3) 0.151(14) Uiso 0.139(6) GR . 2
H31f H 0.534(9) 0.818(14) -0.027(2) 0.151(14) Uiso 0.139(6) GR . 2
H32d H 0.695(9) 0.835(16) 0.027(5) 0.199(19) Uiso 0.139(6) GR . 2
H32e H 0.750(3) 0.725(5) 0.013(7) 0.199(19) Uiso 0.139(6) GR . 2
H32f H 0.703(10) 0.813(19) -0.014(3) 0.199(19) Uiso 0.139(6) GR . 2
H33d H 0.653(13) 0.553(11) -0.010(4) 0.181(17) Uiso 0.139(6) GR . 2
H33e H 0.537(7) 0.567(13) -0.018(5) 0.181(17) Uiso 0.139(6) GR . 2
H33f H 0.616(18) 0.635(3) -0.0403(13) 0.181(17) Uiso 0.139(6) GR . 2


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 1.378(2) . ?
O1 C7 1.379(2) . ?
C1 C2 1.392(3) . ?
C1 C6 1.384(3) . ?
C2 C3 1.380(3) . ?
C2 C19 1.497(3) . ?
C3 C4 1.387(3) . ?
C4 C5 1.379(3) . ?
C4 C30 1.533(3) . ?
C5 C6 1.398(3) . ?
C6 C27 1.522(3) . ?
C7 C8 1.378(3) . ?
C7 C12 1.383(3) . ?
C8 C9 1.400(3) . ?
C8 C27 1.526(3) . ?
C9 C10 1.387(3) . ?
C10 C11 1.390(3) . ?
C10 C34 1.532(3) . ?
C11 C12 1.375(3) . ?
C13 C14 1.445(5) . ?
C13 C18 1.430(4) . ?
C13 C26 1.378(5) . ?
C14 C15 1.337(6) . ?
C15 C16 1.393(6) . ?
C16 C17 1.357(4) . ?
C17 C18 1.421(4) . ?
C18 C19 1.405(4) . ?
C19 C20 1.407(4) . ?
C20 C21 1.417(4) . ?
C20 C25 1.436(4) . ?
C21 C22 1.351(4) . ?
C22 C23 1.407(5) . ?
C23 C24 1.349(5) . ?
C24 C25 1.419(5) . ?
C25 C26 1.400(5) . ?
C27 C28 1.535(3) . ?
C27 C29 1.542(3) . ?
C30 C31 1.505(4) . ?
C30 C32 1.546(5) . ?
C30 C33 1.515(4) . ?
C30 C31a 1.54(2) . ?
C30 C32a 1.51(3) . ?
C30 C33a 1.61(2) . ?
C34 C35 1.477(5) . ?
C34 C35a 1.657(15) . ?
C34 C36 1.505(6) . ?
C34 C36a 1.427(13) . ?
C34 C37 1.550(5) . ?
C34 C37a 1.493(14) . ?

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
C7 O1 C1 118.70(15) . . ?
C2 C1 O1 115.06(18) . . ?
C6 C1 O1 123.21(18) . . ?
C6 C1 C2 121.74(18) . . ?
C3 C2 C1 118.1(2) . . ?
C19 C2 C1 122.31(18) . . ?
C19 C2 C3 119.63(19) . . ?
C4 C3 C2 123.1(2) . . ?
C5 C4 C3 116.47(19) . . ?
C30 C4 C3 120.0(2) . . ?
C30 C4 C5 123.5(2) . . ?
C6 C5 C4 123.5(2) . . ?
C5 C6 C1 117.17(19) . . ?
C27 C6 C1 122.21(17) . . ?
C27 C6 C5 120.62(18) . . ?
C8 C7 O1 123.28(17) . . ?
C12 C7 O1 114.99(18) . . ?
C12 C7 C8 121.72(19) . . ?
C9 C8 C7 116.37(18) . . ?
C27 C8 C7 122.30(18) . . ?
C27 C8 C9 121.33(18) . . ?
C10 C9 C8 123.9(2) . . ?
C11 C10 C9 116.84(19) . . ?
C34 C10 C9 121.8(2) . . ?
C34 C10 C11 121.36(19) . . ?
C12 C11 C10 121.2(2) . . ?
C11 C12 C7 120.0(2) . . ?
C18 C13 C14 117.6(4) . . ?
C26 C13 C14 123.1(3) . . ?
C26 C13 C18 119.3(3) . . ?
C15 C14 C13 121.6(4) . . ?
C16 C15 C14 120.7(4) . . ?
C17 C16 C15 120.5(4) . . ?
C18 C17 C16 121.7(3) . . ?
C17 C18 C13 117.9(3) . . ?
C19 C18 C13 119.4(3) . . ?
C19 C18 C17 122.8(2) . . ?
C18 C19 C2 119.3(2) . . ?
C20 C19 C2 119.7(2) . . ?
C20 C19 C18 120.9(2) . . ?
C21 C20 C19 123.0(2) . . ?
C25 C20 C19 119.2(3) . . ?
C25 C20 C21 117.8(3) . . ?
C22 C21 C20 121.5(3) . . ?
C23 C22 C21 120.8(4) . . ?
C24 C23 C22 119.7(4) . . ?
C25 C24 C23 121.9(4) . . ?
C24 C25 C20 118.2(3) . . ?
C26 C25 C20 118.5(3) . . ?
C26 C25 C24 123.3(3) . . ?
C25 C26 C13 122.6(3) . . ?
C8 C27 C6 110.11(16) . . ?
C28 C27 C6 109.14(18) . . ?
C28 C27 C8 109.95(17) . . ?
C29 C27 C6 109.11(18) . . ?
C29 C27 C8 109.29(18) . . ?
C29 C27 C28 109.2(2) . . ?
C31 C30 C4 109.9(2) . . ?
C32 C30 C4 108.5(2) . . ?
C32 C30 C31 109.8(3) . . ?
C33 C30 C4 112.3(2) . . ?
C33 C30 C31 110.1(3) . . ?
C33 C30 C32 106.2(3) . . ?
C31a C30 C4 113.5(10) . . ?
C31a C30 C31 58.3(12) . . ?
C31a C30 C32 53.0(12) . . ?
C31a C30 C33 133.8(10) . . ?
C32a C30 C4 113.4(14) . . ?
C32a C30 C31 136.6(14) . . ?
C32a C30 C32 58.5(16) . . ?
C32a C30 C33 49.7(16) . . ?
C32a C30 C31a 105.0(19) . . ?
C33a C30 C4 108.2(11) . . ?
C33a C30 C31 52.1(13) . . ?
C33a C30 C32 143.0(11) . . ?
C33a C30 C33 63.0(13) . . ?
C33a C30 C31a 107.0(17) . . ?
C33a C30 C32a 110(2) . . ?
C35 C34 C10 110.7(3) . . ?
C35a C34 C10 111.2(5) . . ?
C35a C34 C35 51.4(7) . . ?
C36 C34 C10 108.2(3) . . ?
C36 C34 C35 111.6(5) . . ?
C36 C34 C35a 62.8(8) . . ?
C36a C34 C10 114.4(7) . . ?
C36a C34 C35 134.0(7) . . ?
C36a C34 C35a 102.1(12) . . ?
C36a C34 C36 44.8(11) . . ?
C37 C34 C10 111.1(2) . . ?
C37 C34 C35 108.5(4) . . ?
C37 C34 C35a 137.5(5) . . ?
C37 C34 C36 106.8(4) . . ?
C37 C34 C36a 63.1(12) . . ?
C37a C34 C10 110.6(7) . . ?
C37a C34 C35 54.3(10) . . ?
C37a C34 C35a 102.9(12) . . ?
C37a C34 C36 141.2(7) . . ?
C37a C34 C36a 114.7(13) . . ?
C37a C34 C37 57.8(11) . . ?

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 179.5(2) . . . . ?
O1 C1 C2 C19 0.6(2) . . . . ?
O1 C1 C6 C5 -179.4(2) . . . . ?
O1 C1 C6 C27 1.1(3) . . . . ?
O1 C7 C8 C9 -179.6(2) . . . . ?
O1 C7 C8 C27 -0.0(2) . . . . ?
O1 C7 C12 C11 -179.99(19) . . . . ?
C1 C2 C3 C4 -0.1(3) . . . . ?
C1 C2 C19 C18 -100.3(2) . . . . ?
C1 C2 C19 C20 83.9(2) . . . . ?
C1 C6 C5 C4 -0.3(2) . . . . ?
C1 C6 C27 C8 -4.1(2) . . . . ?
C1 C6 C27 C28 -124.8(2) . . . . ?
C1 C6 C27 C29 115.9(2) . . . . ?
C2 C3 C4 C5 0.7(3) . . . . ?
C2 C3 C4 C30 -179.5(2) . . . . ?
C2 C19 C18 C13 -173.4(2) . . . . ?
C2 C19 C18 C17 7.7(2) . . . . ?
C2 C19 C20 C21 -8.5(2) . . . . ?
C2 C19 C20 C25 170.9(2) . . . . ?
C3 C4 C5 C6 -0.4(3) . . . . ?
C3 C4 C30 C31 -66.0(3) . . . . ?
C3 C4 C30 C32 54.1(3) . . . . ?
C3 C4 C30 C33 171.1(3) . . . . ?
C3 C4 C30 C31a -2.8(14) . . . . ?
C3 C4 C30 C32a 116.9(19) . . . . ?
C3 C4 C30 C33a -121.3(14) . . . . ?
C4 C5 C6 C27 179.2(2) . . . . ?
C5 C6 C27 C8 176.4(2) . . . . ?
C5 C6 C27 C28 55.7(2) . . . . ?
C5 C6 C27 C29 -63.6(2) . . . . ?
C6 C27 C8 C7 3.6(2) . . . . ?
C6 C27 C8 C9 -176.88(17) . . . . ?
C7 C8 C9 C10 -0.0(2) . . . . ?
C7 C8 C27 C28 123.8(2) . . . . ?
C7 C8 C27 C29 -116.3(2) . . . . ?
C7 C12 C11 C10 -0.7(3) . . . . ?
C8 C9 C10 C11 -0.2(3) . . . . ?
C8 C9 C10 C34 -178.8(2) . . . . ?
C9 C10 C11 C12 0.6(2) . . . . ?
C9 C10 C34 C35 -41.8(5) . . . . ?
C9 C10 C34 C35a 13.5(10) . . . . ?
C9 C10 C34 C36 80.7(4) . . . . ?
C9 C10 C34 C36a 128.6(15) . . . . ?
C9 C10 C34 C37 -162.4(4) . . . . ?
C9 C10 C34 C37a -100.1(13) . . . . ?
C13 C14 C15 C16 1.6(4) . . . . ?
C13 C18 C17 C16 -1.1(3) . . . . ?
C13 C18 C19 C20 2.3(3) . . . . ?
C13 C26 C25 C20 -0.6(3) . . . . ?
C13 C26 C25 C24 179.3(3) . . . . ?
C14 C15 C16 C17 -1.1(5) . . . . ?
C15 C16 C17 C18 0.9(4) . . . . ?
C16 C17 C18 C19 177.8(2) . . . . ?
C17 C18 C19 C20 -176.6(2) . . . . ?
C18 C19 C20 C21 175.8(2) . . . . ?
C18 C19 C20 C25 -4.8(3) . . . . ?
C19 C20 C21 C22 178.3(3) . . . . ?
C19 C20 C25 C24 -175.9(2) . . . . ?
C19 C20 C25 C26 4.0(3) . . . . ?
C20 C21 C22 C23 -1.8(3) . . . . ?
C20 C25 C24 C23 -3.3(3) . . . . ?
C21 C22 C23 C24 2.0(4) . . . . ?
C22 C23 C24 C25 0.6(4) . . . . ?
C23 C24 C25 C26 176.8(3) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_id
C30 C31 1 1
C30 C32 1 2
C30 C33 1 3
C30 C31a 1 1
C30 C32a 1 2
C30 C33a 1 3

loop_
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
_restr_equal_distance_class_average
_restr_equal_distance_class_esd
_restr_equal_distance_class_diff_max
1 0.0200 1.5207 0.0160 0.0160
2 0.0200 1.5260 0.0204 0.0204
3 0.0200 1.5611 0.0457 0.0457

loop_
_restr_U_iso_atom_site_label
_restr_U_iso_weight_param
C31 0.0100
C32 0.0100
C33 0.0100
C31a 0.0100
C32a 0.0100
C33a 0.0100

####################################################################### 
# 
# 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_20220506-lqy333k
_database_code_depnum_ccdc_archive 'CCDC 2180373'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2022-06-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2022-05-31
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H4 Cl2, C51 H46 O'
_chemical_formula_sum            'C53 H50 Cl2 O'
_chemical_formula_weight         773.83
_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'
Cl Cl 0.3639 0.7018 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.85566(17)
_cell_length_b                   13.06940(17)
_cell_length_c                   15.2213(2)
_cell_angle_alpha                94.2229(11)
_cell_angle_beta                 114.1173(14)
_cell_angle_gamma                108.4838(12)
_cell_volume                     2151.93(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15393
_cell_measurement_temperature    333.00(10)
_cell_measurement_theta_max      66.5180
_cell_measurement_theta_min      3.2470
_shelx_estimated_absorpt_T_max   0.854
_shelx_estimated_absorpt_T_min   0.792
_exptl_absorpt_coefficient_mu    1.634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24876
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         3.273
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      333.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     71.00  98.00   0.50    0.30    --   76.75-125.00  30.00   54
  2  ω     43.00  69.00   0.50    0.30    --   76.75-125.00  60.00   52
  3  ω     31.00  77.00   0.50    0.30    --   72.93-125.00 120.00   92
  4  ω     52.00  98.00   0.50    0.30    --   76.75-125.00 -60.00   92
  5  ω     25.00  57.00   0.50    0.30    --   62.89-125.00-120.00   64
  6  ω     44.00  98.00   0.50    0.30    --   76.75-125.00-180.00  108
  7  ω    -70.00 -21.00   0.50    0.30    --  -63.72 125.00 -90.00   98
  8  ω    -97.00 -35.00   0.50    0.30    --  -76.43 125.00-180.00  124
  9  ω    -72.00 -41.00   0.50    0.30    --  -76.43 125.00-120.00   62
 10  ω   -102.00 -67.00   0.50    0.30    --  -81.49 125.00 -90.00   70
 11  ω    -97.00 -50.00   0.50    0.30    --  -76.43 125.00   0.00   94
 12  ω    -67.00 -39.00   0.50    0.30    --  -81.49 125.00   0.00   56
 13  ω   -102.00 -77.00   0.50    0.30    --  -81.49 125.00  30.00   50
 14  ω   -102.00 -77.00   0.50    0.30    --  -81.49 125.00  90.00   50
 15  ω   -102.00 -54.00   0.50    0.30    --  -81.49 125.00 150.00   96
 16  ω    -71.00 -34.00   0.50    0.30    --  -76.43 125.00 120.00   74
 17  ω   -102.00 -77.00   0.50    0.30    --  -81.49 125.00   0.00   50
 18  ω   -101.00 -41.00   0.50    0.30    --  -81.49 125.00  60.00  120
 19  ω   -102.00 -53.00   0.50    0.30    --  -81.49 125.00 120.00   98
 20  ω   -102.00 -40.00   0.50    0.30    --  -81.49 125.00 -60.00  124
 21  ω    -70.00 -45.00   0.50    0.30    --  -81.49 125.00-120.00   50
 22  ω   -101.00 -47.00   0.50    0.30    --  -81.49 125.00-180.00  108
 23  ω   -102.00 -76.00   0.50    0.30    --  -81.49 125.00-150.00   52
 24  ω   -102.00 -73.00   0.50    0.30    --  -81.49 125.00-120.00   58
 25  ω   -100.00 -54.00   0.50    0.30    --  -63.72 -15.00  90.00   92
 26  ω    -92.00 -58.00   0.50    0.30    --  -63.72 -15.00  30.00   68
 27  ω   -100.00 -55.00   0.50    0.30    --  -63.72 -15.00 -30.00   90
 28  ω   -120.00 -84.00   0.50    0.30    --  -76.43 -15.00 -60.00   72
 29  ω    -91.00 -63.00   0.50    0.30    --  -71.74 -15.00 -60.00   56
 30  ω   -103.00 -66.00   0.50    0.30    --  -63.72 -15.00-120.00   74
 31  ω   -102.00 -55.00   0.50    0.30    --  -63.72 -15.00-180.00   94
 32  ω   -117.00 -75.00   0.50    0.30    --  -81.49 -15.00-150.00   84
 33  ω   -114.00 -62.00   0.50    0.30    --  -71.74 -15.00-120.00  104
 34  ω   -124.00 -76.00   0.50    0.30    --  -81.49 -15.00   0.00   96
 35  ω   -104.00 -67.00   0.50    0.30    --  -76.43 -15.00  30.00   74
 36  ω   -119.00 -86.00   0.50    0.30    --  -81.49 -15.00  90.00   66
 37  ω   -123.00 -79.00   0.50    0.30    --  -81.49 -15.00 150.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0622024000
_diffrn_orient_matrix_UB_12      0.0614603000
_diffrn_orient_matrix_UB_13      -0.0589063000
_diffrn_orient_matrix_UB_21      0.0786876000
_diffrn_orient_matrix_UB_22      -0.0712254000
_diffrn_orient_matrix_UB_23      0.0178635000
_diffrn_orient_matrix_UB_31      -0.1005563000
_diffrn_orient_matrix_UB_32      -0.0865883000
_diffrn_orient_matrix_UB_33      -0.0960446000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6266
_reflns_number_total             7472
_reflns_odcompleteness_completeness 97.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7472
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0632
_refine_ls_restrained_S_all      1.091
_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)+(0.1193P)²+0.4168P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1961
_refine_ls_wR_factor_ref         0.2037
_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. Restrained distances
 C52-C53
 1.54 with sigma of 0.02
 C53-Cl2
 1.78 with sigma of 0.02
 C52-Cl1
 1.78 with sigma of 0.02
 C52A-Cl1A
 1.78 with sigma of 0.02
 C53A-Cl2A
 1.78 with sigma of 0.02
 C52A-C53A
 1.54 with sigma of 0.02
3. Others
 Sof(Cl2A)=Sof(C53A)=Sof(H53C)=Sof(H53D)=Sof(C52A)=Sof(H52C)=Sof(H52D)=
 Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C53)=Sof(H53A)=Sof(H53B)=
 FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C53(H53A,H53B), C53A(H53C,H53D), C52A(H52C,H52D)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C5(H5), C10(H10), C20(H20), C39(H39), C34(H34), C15(H15),
 C36(H36), C25(H25), C29(H29), C18(H18), C38(H38), C37(H37), C32(H32), C17(H17),
  C22(H22), C16(H16), C24(H24), C31(H31), C30(H30), C23(H23)
4.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C47(H47A,H47B,H47C), C51(H51A,H51B,
 H51C), C49(H49A,H49B,H49C), C46(H46A,H46B,H46C), C45(H45A,H45B,H45C), C50(H50A,
 H50B,H50C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Cl1 Cl 0.0234(7) 0.1148(8) 0.6304(5) 0.227(4) Uani 0.499(10) 1 d D . P A 1
O1 O 0.73433(11) 0.49652(9) 0.75497(9) 0.0548(3) Uani 1 1 d . . . . .
Cl2 Cl -0.2398(6) -0.0274(6) 0.7252(7) 0.184(2) Uani 0.499(10) 1 d D . P A 1
C2 C 0.81887(16) 0.68480(13) 0.83258(13) 0.0482(4) Uani 1 1 d . . . . .
C12 C 0.65256(15) 0.38916(12) 0.73391(12) 0.0452(4) Uani 1 1 d . . . . .
C6 C 0.64984(15) 0.56024(12) 0.85456(12) 0.0442(4) Uani 1 1 d . . . . .
C11 C 0.66196(16) 0.31119(13) 0.67314(13) 0.0471(4) Uani 1 1 d . . . . .
C7 C 0.56705(15) 0.35965(12) 0.77015(12) 0.0441(4) Uani 1 1 d . . . . .
C1 C 0.73172(15) 0.57873(12) 0.81433(12) 0.0458(4) Uani 1 1 d . . . . .
C3 C 0.82145(17) 0.77210(13) 0.89233(13) 0.0518(4) Uani 1 1 d . . . . .
H3 H 0.879192 0.842828 0.904913 0.062 Uiso 1 1 calc R U . . .
C8 C 0.49010(15) 0.24807(13) 0.74398(12) 0.0478(4) Uani 1 1 d . . . . .
H8 H 0.432260 0.227064 0.767779 0.057 Uiso 1 1 calc R U . . .
C9 C 0.49578(16) 0.16686(13) 0.68403(13) 0.0490(4) Uani 1 1 d . . . . .
C27 C 0.75412(16) 0.34378(12) 0.63387(13) 0.0482(4) Uani 1 1 d . . . . .
C28 C 0.88073(17) 0.37383(14) 0.69808(14) 0.0535(4) Uani 1 1 d . . . . .
C13 C 0.90888(16) 0.70567(12) 0.79091(13) 0.0492(4) Uani 1 1 d . . . . .
C5 C 0.65654(15) 0.65062(13) 0.91343(12) 0.0474(4) Uani 1 1 d . . . . .
H5 H 0.601856 0.638997 0.940486 0.057 Uiso 1 1 calc R U . . .
C4 C 0.74139(16) 0.75817(13) 0.93406(13) 0.0497(4) Uani 1 1 d . . . . .
C41 C 0.55583(15) 0.44430(12) 0.83678(12) 0.0445(4) Uani 1 1 d . . . . .
C14 C 1.03494(17) 0.73438(13) 0.85517(14) 0.0522(4) Uani 1 1 d . . . . .
C40 C 0.71339(17) 0.33992(13) 0.53198(14) 0.0505(4) Uani 1 1 d . . . . .
C26 C 0.86876(18) 0.70283(14) 0.68907(14) 0.0553(5) Uani 1 1 d . . . . .
C10 C 0.58264(16) 0.20074(13) 0.64917(13) 0.0506(4) Uani 1 1 d . . . . .
H10 H 0.588031 0.148004 0.608532 0.061 Uiso 1 1 calc R U . . .
C42 C 0.42587(17) 0.44411(15) 0.78897(16) 0.0614(5) Uani 1 1 d . . . . .
H42A H 0.367415 0.371630 0.779333 0.092 Uiso 1 1 calc R U . . .
H42B H 0.408805 0.463062 0.726153 0.092 Uiso 1 1 calc R U . . .
H42C H 0.419546 0.497511 0.831309 0.092 Uiso 1 1 calc R U . . .
C19 C 1.12296(18) 0.76564(15) 0.81708(16) 0.0594(5) Uani 1 1 d . . . . .
C33 C 0.96737(18) 0.39807(16) 0.65844(16) 0.0616(5) Uani 1 1 d . . . . .
C35 C 0.8023(2) 0.36482(14) 0.49423(15) 0.0576(5) Uani 1 1 d . . . . .
C44 C 0.74254(18) 0.85366(14) 0.99972(15) 0.0577(5) Uani 1 1 d . . . . .
C21 C 0.9583(2) 0.73551(16) 0.65276(16) 0.0628(5) Uani 1 1 d . . . . .
C48 C 0.40886(18) 0.04516(13) 0.65942(15) 0.0582(5) Uani 1 1 d . . . . .
C20 C 1.0821(2) 0.76656(17) 0.71751(17) 0.0666(5) Uani 1 1 d . . . . .
H20 H 1.139719 0.788696 0.693551 0.080 Uiso 1 1 calc R U . . .
C39 C 0.5876(2) 0.31190(16) 0.46357(16) 0.0641(5) Uani 1 1 d . . . . .
H39 H 0.528728 0.296735 0.486518 0.077 Uiso 1 1 calc R U . . .
C43 C 0.5830(2) 0.41277(15) 0.93739(14) 0.0613(5) Uani 1 1 d . . . . .
H43A H 0.577046 0.465980 0.980206 0.092 Uiso 1 1 calc R U . . .
H43B H 0.664597 0.412395 0.967219 0.092 Uiso 1 1 calc R U . . .
H43C H 0.524135 0.340324 0.927287 0.092 Uiso 1 1 calc R U . . .
C34 C 0.9255(2) 0.39263(17) 0.55777(16) 0.0646(5) Uani 1 1 d . . . . .
H34 H 0.981958 0.408165 0.532417 0.078 Uiso 1 1 calc R U . . .
C15 C 1.0815(2) 0.73537(16) 0.95793(17) 0.0665(5) Uani 1 1 d . . . . .
H15 H 1.026673 0.715092 0.984720 0.080 Uiso 1 1 calc R U . . .
C36 C 0.7592(3) 0.35834(18) 0.39029(17) 0.0712(6) Uani 1 1 d . . . . .
H36 H 0.815740 0.373945 0.364980 0.085 Uiso 1 1 calc R U . . .
C25 C 0.7427(2) 0.6714(2) 0.61959(17) 0.0722(6) Uani 1 1 d . . . . .
H25 H 0.682428 0.649843 0.640880 0.087 Uiso 1 1 calc R U . . .
C29 C 0.9277(2) 0.37971(19) 0.80142(16) 0.0686(5) Uani 1 1 d . . . . .
H29 H 0.873580 0.365125 0.829104 0.082 Uiso 1 1 calc R U . . .
C18 C 1.2508(2) 0.79697(19) 0.8834(2) 0.0763(6) Uani 1 1 d . . . . .
H18 H 1.308438 0.817712 0.859400 0.092 Uiso 1 1 calc R U . . .
C38 C 0.5513(2) 0.3068(2) 0.36513(17) 0.0771(6) Uani 1 1 d . . . . .
H38 H 0.468450 0.287709 0.321855 0.092 Uiso 1 1 calc R U . . .
C37 C 0.6395(3) 0.33038(19) 0.32863(18) 0.0781(6) Uani 1 1 d . . . . .
H37 H 0.614165 0.326426 0.261403 0.094 Uiso 1 1 calc R U . . .
C32 C 1.0945(2) 0.4237(2) 0.7237(2) 0.0843(7) Uani 1 1 d . . . . .
H32 H 1.151142 0.437953 0.698440 0.101 Uiso 1 1 calc R U . . .
C17 C 1.2891(2) 0.7970(2) 0.9798(2) 0.0832(7) Uani 1 1 d . . . . .
H17 H 1.372776 0.818174 1.021776 0.100 Uiso 1 1 calc R U . . .
C22 C 0.9174(3) 0.7369(2) 0.55076(19) 0.0840(7) Uani 1 1 d . . . . .
H22 H 0.975164 0.759460 0.527038 0.101 Uiso 1 1 calc R U . . .
C16 C 1.2040(2) 0.7652(2) 1.01769(19) 0.0801(6) Uani 1 1 d . . . . .
H16 H 1.231588 0.764603 1.084373 0.096 Uiso 1 1 calc R U . . .
C47 C 0.8531(3) 0.96053(18) 1.0260(2) 0.1041(10) Uani 1 1 d . . . . .
H47A H 0.927439 0.946291 1.053840 0.156 Uiso 1 1 calc R U . . .
H47B H 0.856160 1.015644 1.073285 0.156 Uiso 1 1 calc R U . . .
H47C H 0.845207 0.986933 0.967241 0.156 Uiso 1 1 calc R U . . .
C51 C 0.4074(3) -0.02625(19) 0.5750(2) 0.1001(9) Uani 1 1 d . . . . .
H51A H 0.345132 -0.099166 0.556767 0.150 Uiso 1 1 calc R U . . .
H51B H 0.486457 -0.031418 0.595894 0.150 Uiso 1 1 calc R U . . .
H51C H 0.389617 0.006779 0.519035 0.150 Uiso 1 1 calc R U . . .
C24 C 0.7090(3) 0.6722(3) 0.52297(19) 0.0940(8) Uani 1 1 d . . . . .
H24 H 0.625906 0.649797 0.478832 0.113 Uiso 1 1 calc R U . . .
C49 C 0.2766(2) 0.0369(2) 0.6267(3) 0.1089(11) Uani 1 1 d . . . . .
H49A H 0.252483 0.070729 0.571640 0.163 Uiso 1 1 calc R U . . .
H49B H 0.271767 0.074658 0.680589 0.163 Uiso 1 1 calc R U . . .
H49C H 0.222402 -0.039697 0.607202 0.163 Uiso 1 1 calc R U . . .
C46 C 0.7552(3) 0.8246(2) 1.0983(2) 0.0984(9) Uani 1 1 d . . . . .
H46A H 0.685212 0.759744 1.086360 0.148 Uiso 1 1 calc R U . . .
H46B H 0.759252 0.885606 1.140510 0.148 Uiso 1 1 calc R U . . .
H46C H 0.829138 0.810315 1.129875 0.148 Uiso 1 1 calc R U . . .
C31 C 1.1334(2) 0.4276(3) 0.8204(2) 0.0993(9) Uani 1 1 d . . . . .
H31 H 1.216551 0.444694 0.861482 0.119 Uiso 1 1 calc R U . . .
C30 C 1.0491(2) 0.4060(3) 0.8605(2) 0.0916(8) Uani 1 1 d . . . . .
H30 H 1.077341 0.409890 0.927944 0.110 Uiso 1 1 calc R U . . .
C23 C 0.7975(3) 0.7064(3) 0.4883(2) 0.0984(9) Uani 1 1 d . . . . .
H23 H 0.772809 0.707769 0.421936 0.118 Uiso 1 1 calc R U . . .
C45 C 0.6233(3) 0.8700(3) 0.9493(3) 0.1239(13) Uani 1 1 d . . . . .
H45A H 0.617379 0.894562 0.890178 0.186 Uiso 1 1 calc R U . . .
H45B H 0.620715 0.924884 0.993134 0.186 Uiso 1 1 calc R U . . .
H45C H 0.555506 0.801152 0.932522 0.186 Uiso 1 1 calc R U . . .
C50 C 0.4485(4) 0.0002(2) 0.7500(2) 0.1220(13) Uani 1 1 d . . . . .
H50A H 0.398013 -0.077144 0.733981 0.183 Uiso 1 1 calc R U . . .
H50B H 0.439593 0.039782 0.800479 0.183 Uiso 1 1 calc R U . . .
H50C H 0.533166 0.009270 0.773533 0.183 Uiso 1 1 calc R U . . .
C52 C -0.0780(8) 0.1026(7) 0.6693(6) 0.096(3) Uani 0.499(10) 1 d D . P A 1
H52A H -0.040903 0.158834 0.730060 0.115 Uiso 0.499(10) 1 calc R U P A 1
H52B H -0.145230 0.117690 0.620653 0.115 Uiso 0.499(10) 1 calc R U P A 1
C53 C -0.1310(13) -0.0098(11) 0.6887(12) 0.125(4) Uani 0.499(10) 1 d D . P A 1
H53A H -0.063687 -0.023366 0.738923 0.150 Uiso 0.499(10) 1 calc R U P A 1
H53B H -0.164756 -0.065968 0.628539 0.150 Uiso 0.499(10) 1 calc R U P A 1
Cl2A Cl -0.2114(10) 0.0325(10) 0.7573(8) 0.219(3) Uani 0.501(10) 1 d D . P A 2
C53A C -0.1252(11) 0.0804(12) 0.7017(9) 0.168(6) Uani 0.501(10) 1 d D . P A 2
H53C H -0.174586 0.100489 0.643356 0.201 Uiso 0.501(10) 1 calc R U P A 2
H53D H -0.057499 0.148211 0.745947 0.201 Uiso 0.501(10) 1 calc R U P A 2
C52A C -0.0724(14) 0.0086(11) 0.6707(10) 0.181(9) Uani 0.501(10) 1 d D . P A 2
H52C H -0.137637 -0.056683 0.620613 0.217 Uiso 0.501(10) 1 calc R U P A 2
H52D H -0.024176 -0.015280 0.726861 0.217 Uiso 0.501(10) 1 calc R U P A 2
Cl1A Cl 0.0219(3) 0.0863(6) 0.6227(3) 0.162(2) Uani 0.501(10) 1 d D . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C52 1.608(9) . ?
O1 C12 1.3783(18) . ?
O1 C1 1.3699(19) . ?
Cl2 C53 1.664(12) . ?
C2 C1 1.399(2) . ?
C2 C3 1.389(2) . ?
C2 C13 1.497(2) . ?
C12 C11 1.393(2) . ?
C12 C7 1.385(2) . ?
C6 C1 1.389(2) . ?
C6 C5 1.386(2) . ?
C6 C41 1.530(2) . ?
C11 C27 1.496(2) . ?
C11 C10 1.394(2) . ?
C7 C8 1.393(2) . ?
C7 C41 1.526(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.389(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.388(2) . ?
C9 C10 1.389(2) . ?
C9 C48 1.537(2) . ?
C27 C28 1.413(3) . ?
C27 C40 1.411(3) . ?
C28 C33 1.435(2) . ?
C28 C29 1.422(3) . ?
C13 C14 1.410(3) . ?
C13 C26 1.413(3) . ?
C5 H5 0.9300 . ?
C5 C4 1.395(2) . ?
C4 C44 1.533(2) . ?
C41 C42 1.525(3) . ?
C41 C43 1.544(2) . ?
C14 C19 1.436(2) . ?
C14 C15 1.425(3) . ?
C40 C35 1.439(2) . ?
C40 C39 1.423(3) . ?
C26 C21 1.434(2) . ?
C26 C25 1.424(3) . ?
C10 H10 0.9300 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C19 C20 1.389(3) . ?
C19 C18 1.430(3) . ?
C33 C34 1.389(3) . ?
C33 C32 1.431(3) . ?
C35 C34 1.381(3) . ?
C35 C36 1.432(3) . ?
C44 C47 1.525(3) . ?
C44 C46 1.532(3) . ?
C44 C45 1.502(4) . ?
C21 C20 1.386(3) . ?
C21 C22 1.425(3) . ?
C48 C51 1.522(3) . ?
C48 C49 1.528(3) . ?
C48 C50 1.496(3) . ?
C20 H20 0.9300 . ?
C39 H39 0.9300 . ?
C39 C38 1.364(3) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C34 H34 0.9300 . ?
C15 H15 0.9300 . ?
C15 C16 1.359(3) . ?
C36 H36 0.9300 . ?
C36 C37 1.339(4) . ?
C25 H25 0.9300 . ?
C25 C24 1.355(3) . ?
C29 H29 0.9300 . ?
C29 C30 1.353(3) . ?
C18 H18 0.9300 . ?
C18 C17 1.344(4) . ?
C38 H38 0.9300 . ?
C38 C37 1.417(4) . ?
C37 H37 0.9300 . ?
C32 H32 0.9300 . ?
C32 C31 1.338(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.402(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.340(4) . ?
C16 H16 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C24 H24 0.9300 . ?
C24 C23 1.405(4) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C31 H31 0.9300 . ?
C31 C30 1.414(4) . ?
C30 H30 0.9300 . ?
C23 H23 0.9300 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 C53 1.518(13) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
Cl2A C53A 1.654(15) . ?
C53A H53C 0.9700 . ?
C53A H53D 0.9700 . ?
C53A C52A 1.471(15) . ?
C52A H52C 0.9700 . ?
C52A H52D 0.9700 . ?
C52A Cl1A 1.758(14) . ?

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 C12 119.04(12) . . ?
C1 C2 C13 122.03(14) . . ?
C3 C2 C1 118.10(15) . . ?
C3 C2 C13 119.86(14) . . ?
O1 C12 C11 115.04(14) . . ?
O1 C12 C7 123.11(14) . . ?
C7 C12 C11 121.85(14) . . ?
C1 C6 C41 121.93(14) . . ?
C5 C6 C1 117.87(14) . . ?
C5 C6 C41 120.20(14) . . ?
C12 C11 C27 121.55(14) . . ?
C12 C11 C10 118.23(15) . . ?
C10 C11 C27 120.22(14) . . ?
C12 C7 C8 117.55(14) . . ?
C12 C7 C41 122.35(13) . . ?
C8 C7 C41 120.10(14) . . ?
O1 C1 C2 115.06(14) . . ?
O1 C1 C6 123.49(13) . . ?
C6 C1 C2 121.46(14) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 C2 122.73(14) . . ?
C4 C3 H3 118.6 . . ?
C7 C8 H8 118.5 . . ?
C9 C8 C7 123.03(15) . . ?
C9 C8 H8 118.5 . . ?
C8 C9 C10 117.22(14) . . ?
C8 C9 C48 120.04(15) . . ?
C10 C9 C48 122.74(15) . . ?
C28 C27 C11 119.94(15) . . ?
C40 C27 C11 119.65(16) . . ?
C40 C27 C28 120.36(15) . . ?
C27 C28 C33 119.44(17) . . ?
C27 C28 C29 123.09(16) . . ?
C29 C28 C33 117.46(18) . . ?
C14 C13 C2 119.35(16) . . ?
C14 C13 C26 120.37(15) . . ?
C26 C13 C2 120.17(16) . . ?
C6 C5 H5 118.4 . . ?
C6 C5 C4 123.17(15) . . ?
C4 C5 H5 118.4 . . ?
C3 C4 C5 116.67(15) . . ?
C3 C4 C44 123.41(14) . . ?
C5 C4 C44 119.91(15) . . ?
C6 C41 C43 108.65(13) . . ?
C7 C41 C6 110.09(12) . . ?
C7 C41 C43 108.75(14) . . ?
C42 C41 C6 109.82(14) . . ?
C42 C41 C7 109.98(14) . . ?
C42 C41 C43 109.53(15) . . ?
C13 C14 C19 119.39(17) . . ?
C13 C14 C15 123.43(17) . . ?
C15 C14 C19 117.18(18) . . ?
C27 C40 C35 119.03(17) . . ?
C27 C40 C39 123.23(16) . . ?
C39 C40 C35 117.75(17) . . ?
C13 C26 C21 119.26(18) . . ?
C13 C26 C25 123.33(17) . . ?
C25 C26 C21 117.39(18) . . ?
C11 C10 H10 118.9 . . ?
C9 C10 C11 122.12(15) . . ?
C9 C10 H10 118.9 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C20 C19 C14 119.30(18) . . ?
C20 C19 C18 121.81(19) . . ?
C18 C19 C14 118.9(2) . . ?
C34 C33 C28 119.41(18) . . ?
C34 C33 C32 121.80(19) . . ?
C32 C33 C28 118.76(19) . . ?
C34 C35 C40 119.87(17) . . ?
C34 C35 C36 121.74(18) . . ?
C36 C35 C40 118.4(2) . . ?
C47 C44 C4 111.91(16) . . ?
C47 C44 C46 105.9(2) . . ?
C46 C44 C4 109.41(16) . . ?
C45 C44 C4 109.52(18) . . ?
C45 C44 C47 111.4(2) . . ?
C45 C44 C46 108.5(2) . . ?
C20 C21 C26 119.53(19) . . ?
C20 C21 C22 121.61(19) . . ?
C22 C21 C26 118.9(2) . . ?
C51 C48 C9 112.13(16) . . ?
C51 C48 C49 106.8(2) . . ?
C49 C48 C9 110.25(17) . . ?
C50 C48 C9 109.03(17) . . ?
C50 C48 C51 109.7(2) . . ?
C50 C48 C49 108.8(3) . . ?
C19 C20 H20 119.0 . . ?
C21 C20 C19 122.04(17) . . ?
C21 C20 H20 119.0 . . ?
C40 C39 H39 119.2 . . ?
C38 C39 C40 121.6(2) . . ?
C38 C39 H39 119.2 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C33 C34 H34 119.1 . . ?
C35 C34 C33 121.88(17) . . ?
C35 C34 H34 119.1 . . ?
C14 C15 H15 119.2 . . ?
C16 C15 C14 121.6(2) . . ?
C16 C15 H15 119.2 . . ?
C35 C36 H36 119.2 . . ?
C37 C36 C35 121.7(2) . . ?
C37 C36 H36 119.2 . . ?
C26 C25 H25 119.4 . . ?
C24 C25 C26 121.1(2) . . ?
C24 C25 H25 119.4 . . ?
C28 C29 H29 119.2 . . ?
C30 C29 C28 121.6(2) . . ?
C30 C29 H29 119.2 . . ?
C19 C18 H18 119.4 . . ?
C17 C18 C19 121.2(2) . . ?
C17 C18 H18 119.4 . . ?
C39 C38 H38 119.9 . . ?
C39 C38 C37 120.2(2) . . ?
C37 C38 H38 119.9 . . ?
C36 C37 C38 120.4(2) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C33 C32 H32 119.4 . . ?
C31 C32 C33 121.2(2) . . ?
C31 C32 H32 119.4 . . ?
C18 C17 H17 119.7 . . ?
C18 C17 C16 120.5(2) . . ?
C16 C17 H17 119.7 . . ?
C21 C22 H22 119.3 . . ?
C23 C22 C21 121.4(2) . . ?
C23 C22 H22 119.3 . . ?
C15 C16 C17 120.7(2) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C48 C51 H51A 109.5 . . ?
C48 C51 H51B 109.5 . . ?
C48 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C25 C24 H24 119.4 . . ?
C25 C24 C23 121.2(3) . . ?
C23 C24 H24 119.4 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C32 C31 H31 119.8 . . ?
C32 C31 C30 120.5(2) . . ?
C30 C31 H31 119.8 . . ?
C29 C30 C31 120.5(2) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C22 C23 C24 120.0(2) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
Cl1 C52 H52A 108.4 . . ?
Cl1 C52 H52B 108.4 . . ?
H52A C52 H52B 107.5 . . ?
C53 C52 Cl1 115.4(8) . . ?
C53 C52 H52A 108.4 . . ?
C53 C52 H52B 108.4 . . ?
Cl2 C53 H53A 108.1 . . ?
Cl2 C53 H53B 108.1 . . ?
C52 C53 Cl2 116.9(9) . . ?
C52 C53 H53A 108.1 . . ?
C52 C53 H53B 108.1 . . ?
H53A C53 H53B 107.3 . . ?
Cl2A C53A H53C 107.6 . . ?
Cl2A C53A H53D 107.6 . . ?
H53C C53A H53D 107.1 . . ?
C52A C53A Cl2A 118.8(12) . . ?
C52A C53A H53C 107.6 . . ?
C52A C53A H53D 107.6 . . ?
C53A C52A H52C 110.2 . . ?
C53A C52A H52D 110.2 . . ?
C53A C52A Cl1A 107.5(11) . . ?
H52C C52A H52D 108.5 . . ?
Cl1A C52A H52C 110.2 . . ?
Cl1A C52A H52D 110.2 . . ?

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
Cl1 C52 C53 Cl2 -177.9(9) . . . . ?
O1 C12 C11 C27 -0.5(3) . . . . ?
O1 C12 C11 C10 179.62(15) . . . . ?
O1 C12 C7 C8 -179.55(16) . . . . ?
O1 C12 C7 C41 0.2(3) . . . . ?
C2 C3 C4 C5 0.2(3) . . . . ?
C2 C3 C4 C44 -179.68(18) . . . . ?
C2 C13 C14 C19 -173.56(14) . . . . ?
C2 C13 C14 C15 5.8(2) . . . . ?
C2 C13 C26 C21 172.86(15) . . . . ?
C2 C13 C26 C25 -5.6(3) . . . . ?
C12 O1 C1 C2 179.32(15) . . . . ?
C12 O1 C1 C6 -0.5(3) . . . . ?
C12 C11 C27 C28 72.2(2) . . . . ?
C12 C11 C27 C40 -110.34(19) . . . . ?
C12 C11 C10 C9 -0.1(3) . . . . ?
C12 C7 C8 C9 0.0(3) . . . . ?
C12 C7 C41 C6 0.3(2) . . . . ?
C12 C7 C41 C42 121.40(18) . . . . ?
C12 C7 C41 C43 -118.66(18) . . . . ?
C6 C5 C4 C3 0.0(3) . . . . ?
C6 C5 C4 C44 179.85(17) . . . . ?
C11 C12 C7 C8 0.3(3) . . . . ?
C11 C12 C7 C41 -179.99(16) . . . . ?
C11 C27 C28 C33 176.05(15) . . . . ?
C11 C27 C28 C29 -2.9(3) . . . . ?
C11 C27 C40 C35 -176.17(14) . . . . ?
C11 C27 C40 C39 3.5(2) . . . . ?
C7 C12 C11 C27 179.69(16) . . . . ?
C7 C12 C11 C10 -0.2(3) . . . . ?
C7 C8 C9 C10 -0.3(3) . . . . ?
C7 C8 C9 C48 179.23(16) . . . . ?
C1 O1 C12 C11 -179.95(15) . . . . ?
C1 O1 C12 C7 -0.1(3) . . . . ?
C1 C2 C3 C4 -0.1(3) . . . . ?
C1 C2 C13 C14 -110.46(19) . . . . ?
C1 C2 C13 C26 73.2(2) . . . . ?
C1 C6 C5 C4 -0.2(3) . . . . ?
C1 C6 C41 C7 -0.8(2) . . . . ?
C1 C6 C41 C42 -122.06(18) . . . . ?
C1 C6 C41 C43 118.16(18) . . . . ?
C3 C2 C1 O1 -179.93(16) . . . . ?
C3 C2 C1 C6 -0.1(3) . . . . ?
C3 C2 C13 C14 68.7(2) . . . . ?
C3 C2 C13 C26 -107.6(2) . . . . ?
C3 C4 C44 C47 -8.6(3) . . . . ?
C3 C4 C44 C46 -125.7(2) . . . . ?
C3 C4 C44 C45 115.4(3) . . . . ?
C8 C7 C41 C6 180.00(15) . . . . ?
C8 C7 C41 C42 -58.9(2) . . . . ?
C8 C7 C41 C43 61.1(2) . . . . ?
C8 C9 C10 C11 0.4(3) . . . . ?
C8 C9 C48 C51 166.6(2) . . . . ?
C8 C9 C48 C49 47.8(3) . . . . ?
C8 C9 C48 C50 -71.7(3) . . . . ?
C27 C11 C10 C9 179.97(17) . . . . ?
C27 C28 C33 C34 0.6(3) . . . . ?
C27 C28 C33 C32 -177.36(19) . . . . ?
C27 C28 C29 C30 178.3(2) . . . . ?
C27 C40 C35 C34 -0.4(2) . . . . ?
C27 C40 C35 C36 178.74(15) . . . . ?
C27 C40 C39 C38 -178.60(17) . . . . ?
C28 C27 C40 C35 1.2(2) . . . . ?
C28 C27 C40 C39 -179.07(15) . . . . ?
C28 C33 C34 C35 0.2(3) . . . . ?
C28 C33 C32 C31 -1.4(4) . . . . ?
C28 C29 C30 C31 -0.6(4) . . . . ?
C13 C2 C1 O1 -0.7(3) . . . . ?
C13 C2 C1 C6 179.10(17) . . . . ?
C13 C2 C3 C4 -179.35(17) . . . . ?
C13 C14 C19 C20 -0.3(2) . . . . ?
C13 C14 C19 C18 178.62(16) . . . . ?
C13 C14 C15 C16 -178.97(18) . . . . ?
C13 C26 C21 C20 1.6(3) . . . . ?
C13 C26 C21 C22 -177.36(18) . . . . ?
C13 C26 C25 C24 178.6(2) . . . . ?
C5 C6 C1 O1 -179.93(16) . . . . ?
C5 C6 C1 C2 0.3(3) . . . . ?
C5 C6 C41 C7 -179.87(15) . . . . ?
C5 C6 C41 C42 58.9(2) . . . . ?
C5 C6 C41 C43 -60.9(2) . . . . ?
C5 C4 C44 C47 171.5(2) . . . . ?
C5 C4 C44 C46 54.4(3) . . . . ?
C5 C4 C44 C45 -64.4(3) . . . . ?
C41 C6 C1 O1 1.0(3) . . . . ?
C41 C6 C1 C2 -178.79(16) . . . . ?
C41 C6 C5 C4 178.87(16) . . . . ?
C41 C7 C8 C9 -179.75(16) . . . . ?
C14 C13 C26 C21 -3.5(2) . . . . ?
C14 C13 C26 C25 178.05(17) . . . . ?
C14 C19 C20 C21 -1.6(3) . . . . ?
C14 C19 C18 C17 0.3(3) . . . . ?
C14 C15 C16 C17 0.4(3) . . . . ?
C40 C27 C28 C33 -1.4(2) . . . . ?
C40 C27 C28 C29 179.73(17) . . . . ?
C40 C35 C34 C33 -0.3(3) . . . . ?
C40 C35 C36 C37 0.3(3) . . . . ?
C40 C39 C38 C37 -0.5(3) . . . . ?
C26 C13 C14 C19 2.8(2) . . . . ?
C26 C13 C14 C15 -177.84(16) . . . . ?
C26 C21 C20 C19 1.0(3) . . . . ?
C26 C21 C22 C23 -1.3(4) . . . . ?
C26 C25 C24 C23 -1.3(4) . . . . ?
C10 C11 C27 C28 -107.87(19) . . . . ?
C10 C11 C27 C40 69.6(2) . . . . ?
C10 C9 C48 C51 -13.9(3) . . . . ?
C10 C9 C48 C49 -132.7(2) . . . . ?
C10 C9 C48 C50 107.8(3) . . . . ?
C19 C14 C15 C16 0.4(3) . . . . ?
C19 C18 C17 C16 0.5(4) . . . . ?
C33 C28 C29 C30 -0.7(3) . . . . ?
C33 C32 C31 C30 0.2(5) . . . . ?
C35 C40 C39 C38 1.1(3) . . . . ?
C35 C36 C37 C38 0.4(3) . . . . ?
C21 C26 C25 C24 0.1(3) . . . . ?
C21 C22 C23 C24 0.1(5) . . . . ?
C48 C9 C10 C11 -179.15(17) . . . . ?
C20 C19 C18 C17 179.2(2) . . . . ?
C20 C21 C22 C23 179.7(2) . . . . ?
C39 C40 C35 C34 179.90(16) . . . . ?
C39 C40 C35 C36 -1.0(2) . . . . ?
C39 C38 C37 C36 -0.3(3) . . . . ?
C34 C33 C32 C31 -179.3(3) . . . . ?
C34 C35 C36 C37 179.39(19) . . . . ?
C15 C14 C19 C20 -179.65(17) . . . . ?
C15 C14 C19 C18 -0.8(3) . . . . ?
C36 C35 C34 C33 -179.45(18) . . . . ?
C25 C26 C21 C20 -179.82(19) . . . . ?
C25 C26 C21 C22 1.2(3) . . . . ?
C25 C24 C23 C22 1.2(5) . . . . ?
C29 C28 C33 C34 179.59(18) . . . . ?
C29 C28 C33 C32 1.6(3) . . . . ?
C18 C19 C20 C21 179.52(19) . . . . ?
C18 C17 C16 C15 -0.9(4) . . . . ?
C32 C33 C34 C35 178.1(2) . . . . ?
C32 C31 C30 C29 0.8(5) . . . . ?
C22 C21 C20 C19 179.9(2) . . . . ?
Cl2A C53A C52A Cl1A -176.0(8) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.943
_oxdiff_exptl_absorpt_empirical_full_min 0.326
####################################################################### 
# 
# 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_20220506-lqy303k
_database_code_depnum_ccdc_archive 'CCDC 2180362'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2022-06-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2022-05-31
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H4 Cl2, C51 H46 O'
_chemical_formula_sum            'C53 H50 Cl2 O'
_chemical_formula_weight         773.83
_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'
Cl Cl 0.3639 0.7018 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.8331(3)
_cell_length_b                   13.0210(3)
_cell_length_c                   15.1558(3)
_cell_angle_alpha                93.893(2)
_cell_angle_beta                 114.337(2)
_cell_angle_gamma                108.437(2)
_cell_volume                     2130.70(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15198
_cell_measurement_temperature    303.00(10)
_cell_measurement_theta_max      66.5380
_cell_measurement_theta_min      3.2560
_shelx_estimated_absorpt_T_max   0.852
_shelx_estimated_absorpt_T_min   0.790
_exptl_absorpt_coefficient_mu    1.650
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24534
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         3.288
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      303.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     59.00 107.00   0.50    0.30    --   62.89  15.00-180.00   96
  2  ω     78.00 115.00   0.50    0.30    --   76.75  15.00   0.00   74
  3  ω     62.00 116.00   0.50    0.30    --   72.93  15.00 120.00  108
  4  ω     59.00  96.00   0.50    0.30    --   62.89  15.00-120.00   74
  5  ω    -68.00 -25.00   0.50    0.30    --  -63.72 125.00-180.00   86
  6  ω    -97.00 -50.00   0.50    0.30    --  -76.43 125.00-180.00   94
  7  ω   -102.00 -42.00   0.50    0.30    --  -81.49 125.00 -90.00  120
  8  ω    -54.00 -29.00   0.50    0.30    --  -71.74 125.00 -30.00   50
  9  ω    -67.00 -39.00   0.50    0.30    --  -76.43 125.00  30.00   56
 10  ω   -102.00 -48.00   0.50    0.30    --  -81.49 125.00  30.00  108
 11  ω   -102.00 -41.00   0.50    0.30    --  -81.49 125.00  60.00  122
 12  ω    -72.00 -40.00   0.50    0.30    --  -81.49 125.00 120.00   64
 13  ω   -102.00 -76.00   0.50    0.30    --  -81.49 125.00 150.00   52
 14  ω   -101.00 -75.00   0.50    0.30    --  -81.49 125.00  90.00   52
 15  ω    -69.00 -39.00   0.50    0.30    --  -81.49 125.00 -30.00   60
 16  ω   -102.00 -77.00   0.50    0.30    --  -81.49 125.00 -60.00   50
 17  ω   -102.00 -55.00   0.50    0.30    --  -81.49 125.00-120.00   94
 18  ω   -102.00 -76.00   0.50    0.30    --  -81.49 125.00-180.00   52
 19  ω   -102.00 -76.00   0.50    0.30    --  -81.49 125.00-150.00   52
 20  ω   -102.00 -77.00   0.50    0.30    --  -81.49 125.00   0.00   50
 21  ω   -105.00 -55.00   0.50    0.30    --  -63.72 -15.00  30.00  100
 22  ω   -114.00 -62.00   0.50    0.30    --  -71.74 -15.00  90.00  104
 23  ω   -105.00 -72.00   0.50    0.30    --  -63.72 -15.00 -60.00   66
 24  ω   -125.00 -72.00   0.50    0.30    --  -81.49 -15.00   0.00  106
 25  ω   -110.00 -75.00   0.50    0.30    --  -81.49 -15.00 -90.00   70
 26  ω   -121.00 -83.00   0.50    0.30    --  -81.49 -15.00 150.00   76
 27  ω   -117.00 -79.00   0.50    0.30    --  -76.43 -15.00-120.00   76
 28  ω   -109.00 -74.00   0.50    0.30    --  -71.74 -15.00-150.00   70
 29  ω   -115.00 -75.00   0.50    0.30    --  -71.74 -15.00-180.00   80
 30  ω     47.00  98.00   0.50    0.30    --   76.75-125.00-180.00  102
 31  ω     25.00  75.00   0.50    0.30    --   62.89-125.00 -30.00  100
 32  ω     35.00  98.00   0.50    0.30    --   76.75-125.00  30.00  126
 33  ω     35.00  98.00   0.50    0.30    --   76.75-125.00  90.00  126
 34  ω     41.00  98.00   0.50    0.30    --   76.75-125.00 -60.00  114
 35  ω     45.00  98.00   0.50    0.30    --   76.75-125.00-120.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0561387000
_diffrn_orient_matrix_UB_12      0.0681269000
_diffrn_orient_matrix_UB_13      -0.0598753000
_diffrn_orient_matrix_UB_21      0.0835825000
_diffrn_orient_matrix_UB_22      -0.0664317000
_diffrn_orient_matrix_UB_23      0.0130143000
_diffrn_orient_matrix_UB_31      -0.1006365000
_diffrn_orient_matrix_UB_32      -0.0858072000
_diffrn_orient_matrix_UB_33      -0.0968645000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6215
_reflns_number_total             7455
_reflns_odcompleteness_completeness 97.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7455
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0587
_refine_ls_restrained_S_all      1.127
_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)+(0.1083P)²+0.4227P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1835
_refine_ls_wR_factor_ref         0.1943
_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. Restrained distances
 C52-C53
 1.54 with sigma of 0.02
 C53-Cl2
 1.78 with sigma of 0.02
 C52-Cl1
 1.78 with sigma of 0.02
 C52A-Cl1A
 1.78 with sigma of 0.02
 C53A-Cl2A
 1.78 with sigma of 0.02
 C52A-C53A
 1.54 with sigma of 0.02
3. Others
 Sof(Cl2A)=Sof(C53A)=Sof(H53C)=Sof(H53D)=Sof(C52A)=Sof(H52C)=Sof(H52D)=
 Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C53)=Sof(H53A)=Sof(H53B)=
 FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C53(H53A,H53B), C53A(H53C,H53D), C52A(H52C,H52D)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C5(H5), C10(H10), C20(H20), C39(H39), C34(H34), C15(H15),
 C36(H36), C25(H25), C29(H29), C18(H18), C38(H38), C37(H37), C32(H32), C17(H17),
  C22(H22), C16(H16), C24(H24), C31(H31), C30(H30), C23(H23)
4.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C47(H47A,H47B,H47C), C51(H51A,H51B,
 H51C), C49(H49A,H49B,H49C), C46(H46A,H46B,H46C), C45(H45A,H45B,H45C), C50(H50A,
 H50B,H50C)
;
_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
Cl1 Cl 0.0203(5) 0.1072(6) 0.6260(4) 0.173(2) Uani 0.555(10) 1 d D . P A 1
O1 O 0.73457(11) 0.49644(9) 0.75499(9) 0.0486(3) Uani 1 1 d . . . . .
Cl2 Cl -0.2417(5) -0.0243(5) 0.7295(5) 0.1594(19) Uani 0.555(10) 1 d D . P A 1
C2 C 0.81977(15) 0.68465(13) 0.83352(12) 0.0433(4) Uani 1 1 d . . . . .
C12 C 0.65250(14) 0.38928(12) 0.73372(12) 0.0406(4) Uani 1 1 d . . . . .
C6 C 0.65072(14) 0.55996(13) 0.85562(12) 0.0402(4) Uani 1 1 d . . . . .
C11 C 0.66118(15) 0.31108(13) 0.67226(12) 0.0422(4) Uani 1 1 d . . . . .
C7 C 0.56687(14) 0.35926(13) 0.77024(12) 0.0397(4) Uani 1 1 d . . . . .
C1 C 0.73258(15) 0.57867(13) 0.81537(12) 0.0418(4) Uani 1 1 d . . . . .
C3 C 0.82286(16) 0.77234(13) 0.89393(13) 0.0459(4) Uani 1 1 d . . . . .
H3 H 0.880736 0.843215 0.906634 0.055 Uiso 1 1 calc R U . . .
C8 C 0.48968(15) 0.24772(13) 0.74377(12) 0.0428(4) Uani 1 1 d . . . . .
H8 H 0.431975 0.226575 0.767847 0.051 Uiso 1 1 calc R U . . .
C9 C 0.49464(15) 0.16629(13) 0.68304(12) 0.0432(4) Uani 1 1 d . . . . .
C27 C 0.75353(15) 0.34349(13) 0.63274(13) 0.0434(4) Uani 1 1 d . . . . .
C28 C 0.88033(16) 0.37329(14) 0.69736(14) 0.0481(4) Uani 1 1 d . . . . .
C13 C 0.90965(15) 0.70619(12) 0.79148(13) 0.0442(4) Uani 1 1 d . . . . .
C5 C 0.65788(15) 0.65039(13) 0.91507(12) 0.0432(4) Uani 1 1 d . . . . .
H5 H 0.603279 0.638587 0.942352 0.052 Uiso 1 1 calc R U . . .
C4 C 0.74266(15) 0.75778(13) 0.93586(12) 0.0439(4) Uani 1 1 d . . . . .
C41 C 0.55622(14) 0.44384(13) 0.83760(12) 0.0407(4) Uani 1 1 d . . . . .
C14 C 1.03618(16) 0.73537(13) 0.85605(14) 0.0469(4) Uani 1 1 d . . . . .
C40 C 0.71259(16) 0.33957(13) 0.53038(13) 0.0453(4) Uani 1 1 d . . . . .
C26 C 0.86900(17) 0.70332(14) 0.68947(14) 0.0490(4) Uani 1 1 d . . . . .
C10 C 0.58171(15) 0.20079(13) 0.64815(12) 0.0449(4) Uani 1 1 d . . . . .
H10 H 0.586984 0.148186 0.607210 0.054 Uiso 1 1 calc R U . . .
C42 C 0.42560(16) 0.44452(15) 0.78921(15) 0.0549(5) Uani 1 1 d . . . . .
H42A H 0.366664 0.371668 0.778392 0.082 Uiso 1 1 calc R U . . .
H42B H 0.409165 0.465203 0.726656 0.082 Uiso 1 1 calc R U . . .
H42C H 0.419093 0.497101 0.832239 0.082 Uiso 1 1 calc R U . . .
C19 C 1.12417(17) 0.76711(14) 0.81757(15) 0.0533(5) Uani 1 1 d . . . . .
C33 C 0.96714(17) 0.39715(16) 0.65766(15) 0.0549(5) Uani 1 1 d . . . . .
C35 C 0.80129(19) 0.36439(14) 0.49239(14) 0.0519(4) Uani 1 1 d . . . . .
C44 C 0.74425(17) 0.85339(14) 1.00198(14) 0.0510(4) Uani 1 1 d . . . . .
C21 C 0.95825(18) 0.73631(16) 0.65236(15) 0.0558(5) Uani 1 1 d . . . . .
C48 C 0.40753(17) 0.04465(13) 0.65838(14) 0.0508(4) Uani 1 1 d . . . . .
C20 C 1.08273(18) 0.76805(17) 0.71765(16) 0.0595(5) Uani 1 1 d . . . . .
H20 H 1.140241 0.790712 0.693522 0.071 Uiso 1 1 calc R U . . .
C39 C 0.58624(19) 0.31177(16) 0.46150(15) 0.0574(5) Uani 1 1 d . . . . .
H39 H 0.527359 0.297034 0.484555 0.069 Uiso 1 1 calc R U . . .
C43 C 0.58290(19) 0.41117(14) 0.93814(14) 0.0542(5) Uani 1 1 d . . . . .
H43A H 0.574617 0.462985 0.980509 0.081 Uiso 1 1 calc R U . . .
H43B H 0.665498 0.412476 0.969154 0.081 Uiso 1 1 calc R U . . .
H43C H 0.525241 0.337695 0.927455 0.081 Uiso 1 1 calc R U . . .
C34 C 0.92523(18) 0.39190(16) 0.55673(16) 0.0581(5) Uani 1 1 d . . . . .
H34 H 0.981867 0.407280 0.531366 0.070 Uiso 1 1 calc R U . . .
C15 C 1.08335(19) 0.73636(16) 0.95947(16) 0.0591(5) Uani 1 1 d . . . . .
H15 H 1.028642 0.715283 0.986425 0.071 Uiso 1 1 calc R U . . .
C36 C 0.7581(2) 0.35757(17) 0.38802(16) 0.0640(5) Uani 1 1 d . . . . .
H36 H 0.814681 0.373265 0.362622 0.077 Uiso 1 1 calc R U . . .
C25 C 0.74198(19) 0.67113(19) 0.61937(16) 0.0642(5) Uani 1 1 d . . . . .
H25 H 0.681934 0.648992 0.641000 0.077 Uiso 1 1 calc R U . . .
C29 C 0.92766(18) 0.37895(18) 0.80155(15) 0.0613(5) Uani 1 1 d . . . . .
H29 H 0.873525 0.364383 0.829354 0.074 Uiso 1 1 calc R U . . .
C18 C 1.25253(19) 0.79904(18) 0.88421(19) 0.0674(6) Uani 1 1 d . . . . .
H18 H 1.309997 0.819971 0.859874 0.081 Uiso 1 1 calc R U . . .
C38 C 0.5498(2) 0.30630(19) 0.36253(16) 0.0682(6) Uani 1 1 d . . . . .
H38 H 0.466785 0.287515 0.318992 0.082 Uiso 1 1 calc R U . . .
C37 C 0.6377(2) 0.32905(19) 0.32583(16) 0.0699(6) Uani 1 1 d . . . . .
H37 H 0.611943 0.324223 0.258116 0.084 Uiso 1 1 calc R U . . .
C32 C 1.09423(19) 0.4226(2) 0.72318(19) 0.0739(6) Uani 1 1 d . . . . .
H32 H 1.150857 0.437032 0.697809 0.089 Uiso 1 1 calc R U . . .
C17 C 1.2918(2) 0.79938(19) 0.9813(2) 0.0728(6) Uani 1 1 d . . . . .
H17 H 1.375730 0.820880 1.023359 0.087 Uiso 1 1 calc R U . . .
C22 C 0.9167(2) 0.7380(2) 0.55012(17) 0.0737(6) Uani 1 1 d . . . . .
H22 H 0.974459 0.761009 0.526219 0.088 Uiso 1 1 calc R U . . .
C16 C 1.2064(2) 0.76738(19) 1.01955(18) 0.0703(6) Uani 1 1 d . . . . .
H16 H 1.234471 0.767455 1.086776 0.084 Uiso 1 1 calc R U . . .
C47 C 0.8537(3) 0.96088(17) 1.0270(2) 0.0867(8) Uani 1 1 d . . . . .
H47A H 0.929064 0.948088 1.057666 0.130 Uiso 1 1 calc R U . . .
H47B H 0.854489 1.017048 1.071989 0.130 Uiso 1 1 calc R U . . .
H47C H 0.846429 0.985234 0.967094 0.130 Uiso 1 1 calc R U . . .
C51 C 0.4063(3) -0.02689(17) 0.5738(2) 0.0814(7) Uani 1 1 d . . . . .
H51A H 0.345561 -0.100511 0.556839 0.122 Uiso 1 1 calc R U . . .
H51B H 0.486334 -0.030509 0.594579 0.122 Uiso 1 1 calc R U . . .
H51C H 0.386371 0.005288 0.516865 0.122 Uiso 1 1 calc R U . . .
C24 C 0.7070(2) 0.6721(2) 0.52208(18) 0.0818(7) Uani 1 1 d . . . . .
H24 H 0.623568 0.649537 0.477833 0.098 Uiso 1 1 calc R U . . .
C49 C 0.2749(2) 0.03684(19) 0.6254(2) 0.0865(8) Uani 1 1 d . . . . .
H49A H 0.250043 0.069518 0.569065 0.130 Uiso 1 1 calc R U . . .
H49B H 0.270590 0.075940 0.679000 0.130 Uiso 1 1 calc R U . . .
H49C H 0.220792 -0.039837 0.607306 0.130 Uiso 1 1 calc R U . . .
C46 C 0.7574(3) 0.82361(19) 1.10112(17) 0.0807(7) Uani 1 1 d . . . . .
H46A H 0.687938 0.757899 1.089066 0.121 Uiso 1 1 calc R U . . .
H46B H 0.760181 0.884062 1.143153 0.121 Uiso 1 1 calc R U . . .
H46C H 0.832177 0.810207 1.133255 0.121 Uiso 1 1 calc R U . . .
C31 C 1.1339(2) 0.4262(3) 0.8210(2) 0.0848(7) Uani 1 1 d . . . . .
H31 H 1.217153 0.442765 0.862276 0.102 Uiso 1 1 calc R U . . .
C30 C 1.0495(2) 0.4050(2) 0.86100(18) 0.0799(7) Uani 1 1 d . . . . .
H30 H 1.077847 0.408973 0.928841 0.096 Uiso 1 1 calc R U . . .
C23 C 0.7964(3) 0.7073(2) 0.48719(18) 0.0840(7) Uani 1 1 d . . . . .
H23 H 0.771571 0.709070 0.420547 0.101 Uiso 1 1 calc R U . . .
C45 C 0.6240(3) 0.8704(2) 0.9509(2) 0.1008(10) Uani 1 1 d . . . . .
H45A H 0.616156 0.891742 0.889817 0.151 Uiso 1 1 calc R U . . .
H45B H 0.623251 0.927828 0.993599 0.151 Uiso 1 1 calc R U . . .
H45C H 0.556209 0.802358 0.936993 0.151 Uiso 1 1 calc R U . . .
C50 C 0.4484(3) -0.0015(2) 0.7499(2) 0.0961(9) Uani 1 1 d . . . . .
H50A H 0.400121 -0.079702 0.733205 0.144 Uiso 1 1 calc R U . . .
H50B H 0.436988 0.035741 0.800028 0.144 Uiso 1 1 calc R U . . .
H50C H 0.534155 0.010055 0.774601 0.144 Uiso 1 1 calc R U . . .
C52 C -0.0797(6) 0.1012(6) 0.6692(5) 0.088(2) Uani 0.555(10) 1 d D . P A 1
H52A H -0.039099 0.158241 0.730108 0.105 Uiso 0.555(10) 1 calc R U P A 1
H52B H -0.146608 0.118171 0.621221 0.105 Uiso 0.555(10) 1 calc R U P A 1
C53 C -0.1340(9) -0.0098(8) 0.6902(8) 0.104(3) Uani 0.555(10) 1 d D . P A 1
H53A H -0.066734 -0.024608 0.740111 0.125 Uiso 0.555(10) 1 calc R U P A 1
H53B H -0.170144 -0.066732 0.629926 0.125 Uiso 0.555(10) 1 calc R U P A 1
Cl2A Cl -0.2150(9) 0.0314(10) 0.7567(7) 0.181(3) Uani 0.445(10) 1 d D . P A 2
C53A C -0.1263(10) 0.0847(10) 0.7015(9) 0.139(5) Uani 0.445(10) 1 d D . P A 2
H53C H -0.174423 0.106774 0.643296 0.166 Uiso 0.445(10) 1 calc R U P A 2
H53D H -0.057029 0.151031 0.747129 0.166 Uiso 0.445(10) 1 calc R U P A 2
C52A C -0.0780(11) 0.0072(10) 0.6708(8) 0.128(5) Uani 0.445(10) 1 d D . P A 2
H52C H -0.145201 -0.056707 0.619933 0.154 Uiso 0.445(10) 1 calc R U P A 2
H52D H -0.032089 -0.018719 0.727171 0.154 Uiso 0.445(10) 1 calc R U P A 2
Cl1A Cl 0.0204(3) 0.0841(6) 0.6233(3) 0.142(2) Uani 0.445(10) 1 d D . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C52 1.649(7) . ?
O1 C12 1.3746(18) . ?
O1 C1 1.3741(18) . ?
Cl2 C53 1.682(10) . ?
C2 C1 1.396(2) . ?
C2 C3 1.394(2) . ?
C2 C13 1.497(2) . ?
C12 C11 1.395(2) . ?
C12 C7 1.388(2) . ?
C6 C1 1.386(2) . ?
C6 C5 1.388(2) . ?
C6 C41 1.531(2) . ?
C11 C27 1.498(2) . ?
C11 C10 1.390(2) . ?
C7 C8 1.391(2) . ?
C7 C41 1.527(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.390(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.391(2) . ?
C9 C10 1.390(2) . ?
C9 C48 1.534(2) . ?
C27 C28 1.412(3) . ?
C27 C40 1.409(2) . ?
C28 C33 1.435(2) . ?
C28 C29 1.426(3) . ?
C13 C14 1.410(3) . ?
C13 C26 1.407(3) . ?
C5 H5 0.9300 . ?
C5 C4 1.390(2) . ?
C4 C44 1.534(2) . ?
C41 C42 1.531(2) . ?
C41 C43 1.540(2) . ?
C14 C19 1.437(2) . ?
C14 C15 1.426(3) . ?
C40 C35 1.437(2) . ?
C40 C39 1.426(3) . ?
C26 C21 1.437(2) . ?
C26 C25 1.429(3) . ?
C10 H10 0.9300 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C19 C20 1.385(3) . ?
C19 C18 1.430(3) . ?
C33 C34 1.385(3) . ?
C33 C32 1.426(3) . ?
C35 C34 1.387(3) . ?
C35 C36 1.430(3) . ?
C44 C47 1.523(3) . ?
C44 C46 1.532(3) . ?
C44 C45 1.511(3) . ?
C21 C20 1.388(3) . ?
C21 C22 1.420(3) . ?
C48 C51 1.524(3) . ?
C48 C49 1.530(3) . ?
C48 C50 1.507(3) . ?
C20 H20 0.9300 . ?
C39 H39 0.9300 . ?
C39 C38 1.364(3) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C34 H34 0.9300 . ?
C15 H15 0.9300 . ?
C15 C16 1.359(3) . ?
C36 H36 0.9300 . ?
C36 C37 1.343(3) . ?
C25 H25 0.9300 . ?
C25 C24 1.355(3) . ?
C29 H29 0.9300 . ?
C29 C30 1.354(3) . ?
C18 H18 0.9300 . ?
C18 C17 1.344(3) . ?
C38 H38 0.9300 . ?
C38 C37 1.413(3) . ?
C37 H37 0.9300 . ?
C32 H32 0.9300 . ?
C32 C31 1.346(3) . ?
C17 H17 0.9300 . ?
C17 C16 1.406(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.341(4) . ?
C16 H16 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C24 H24 0.9300 . ?
C24 C23 1.416(3) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C31 H31 0.9300 . ?
C31 C30 1.412(3) . ?
C30 H30 0.9300 . ?
C23 H23 0.9300 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 C53 1.512(11) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
Cl2A C53A 1.686(15) . ?
C53A H53C 0.9700 . ?
C53A H53D 0.9700 . ?
C53A C52A 1.479(13) . ?
C52A H52C 0.9700 . ?
C52A H52D 0.9700 . ?
C52A Cl1A 1.778(13) . ?

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 C12 118.90(12) . . ?
C1 C2 C13 122.31(14) . . ?
C3 C2 C1 118.10(14) . . ?
C3 C2 C13 119.59(13) . . ?
O1 C12 C11 115.11(13) . . ?
O1 C12 C7 123.31(13) . . ?
C7 C12 C11 121.58(14) . . ?
C1 C6 C5 117.81(14) . . ?
C1 C6 C41 122.01(13) . . ?
C5 C6 C41 120.17(13) . . ?
C12 C11 C27 121.59(14) . . ?
C10 C11 C12 118.35(14) . . ?
C10 C11 C27 120.05(14) . . ?
C12 C7 C8 117.62(14) . . ?
C12 C7 C41 122.22(13) . . ?
C8 C7 C41 120.15(13) . . ?
O1 C1 C2 114.91(13) . . ?
O1 C1 C6 123.50(13) . . ?
C6 C1 C2 121.59(14) . . ?
C2 C3 H3 118.8 . . ?
C4 C3 C2 122.44(14) . . ?
C4 C3 H3 118.8 . . ?
C7 C8 H8 118.4 . . ?
C9 C8 C7 123.18(14) . . ?
C9 C8 H8 118.4 . . ?
C8 C9 C48 120.08(14) . . ?
C10 C9 C8 116.91(14) . . ?
C10 C9 C48 123.01(14) . . ?
C28 C27 C11 119.90(15) . . ?
C40 C27 C11 119.66(15) . . ?
C40 C27 C28 120.39(14) . . ?
C27 C28 C33 119.48(16) . . ?
C27 C28 C29 123.13(15) . . ?
C29 C28 C33 117.38(17) . . ?
C14 C13 C2 119.29(15) . . ?
C26 C13 C2 120.18(15) . . ?
C26 C13 C14 120.44(15) . . ?
C6 C5 H5 118.4 . . ?
C6 C5 C4 123.25(14) . . ?
C4 C5 H5 118.4 . . ?
C3 C4 C5 116.81(14) . . ?
C3 C4 C44 123.14(14) . . ?
C5 C4 C44 120.04(14) . . ?
C6 C41 C42 109.73(14) . . ?
C6 C41 C43 108.84(13) . . ?
C7 C41 C6 110.05(12) . . ?
C7 C41 C42 109.81(13) . . ?
C7 C41 C43 108.86(14) . . ?
C42 C41 C43 109.52(14) . . ?
C13 C14 C19 119.38(17) . . ?
C13 C14 C15 123.44(16) . . ?
C15 C14 C19 117.18(17) . . ?
C27 C40 C35 119.14(16) . . ?
C27 C40 C39 123.16(15) . . ?
C39 C40 C35 117.70(16) . . ?
C13 C26 C21 119.42(17) . . ?
C13 C26 C25 123.41(16) . . ?
C25 C26 C21 117.16(17) . . ?
C11 C10 C9 122.35(14) . . ?
C11 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C20 C19 C14 119.24(17) . . ?
C20 C19 C18 121.86(17) . . ?
C18 C19 C14 118.89(19) . . ?
C34 C33 C28 119.39(17) . . ?
C34 C33 C32 121.76(17) . . ?
C32 C33 C28 118.82(18) . . ?
C34 C35 C40 119.66(17) . . ?
C34 C35 C36 121.80(17) . . ?
C36 C35 C40 118.52(18) . . ?
C47 C44 C4 112.09(15) . . ?
C47 C44 C46 106.62(18) . . ?
C46 C44 C4 109.38(16) . . ?
C45 C44 C4 109.38(16) . . ?
C45 C44 C47 110.6(2) . . ?
C45 C44 C46 108.7(2) . . ?
C20 C21 C26 119.23(17) . . ?
C20 C21 C22 121.75(17) . . ?
C22 C21 C26 119.00(19) . . ?
C51 C48 C9 112.12(15) . . ?
C51 C48 C49 107.03(18) . . ?
C49 C48 C9 110.28(16) . . ?
C50 C48 C9 108.95(16) . . ?
C50 C48 C51 109.1(2) . . ?
C50 C48 C49 109.3(2) . . ?
C19 C20 C21 122.19(16) . . ?
C19 C20 H20 118.9 . . ?
C21 C20 H20 118.9 . . ?
C40 C39 H39 119.3 . . ?
C38 C39 C40 121.43(18) . . ?
C38 C39 H39 119.3 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C33 C34 C35 121.93(16) . . ?
C33 C34 H34 119.0 . . ?
C35 C34 H34 119.0 . . ?
C14 C15 H15 119.2 . . ?
C16 C15 C14 121.54(19) . . ?
C16 C15 H15 119.2 . . ?
C35 C36 H36 119.2 . . ?
C37 C36 C35 121.54(19) . . ?
C37 C36 H36 119.2 . . ?
C26 C25 H25 119.2 . . ?
C24 C25 C26 121.51(19) . . ?
C24 C25 H25 119.2 . . ?
C28 C29 H29 119.2 . . ?
C30 C29 C28 121.60(18) . . ?
C30 C29 H29 119.2 . . ?
C19 C18 H18 119.3 . . ?
C17 C18 C19 121.31(19) . . ?
C17 C18 H18 119.3 . . ?
C39 C38 H38 119.8 . . ?
C39 C38 C37 120.3(2) . . ?
C37 C38 H38 119.8 . . ?
C36 C37 C38 120.5(2) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C33 C32 H32 119.3 . . ?
C31 C32 C33 121.35(19) . . ?
C31 C32 H32 119.3 . . ?
C18 C17 H17 119.9 . . ?
C18 C17 C16 120.3(2) . . ?
C16 C17 H17 119.9 . . ?
C21 C22 H22 119.2 . . ?
C23 C22 C21 121.6(2) . . ?
C23 C22 H22 119.2 . . ?
C15 C16 C17 120.8(2) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C48 C51 H51A 109.5 . . ?
C48 C51 H51B 109.5 . . ?
C48 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C25 C24 H24 119.7 . . ?
C25 C24 C23 120.6(2) . . ?
C23 C24 H24 119.7 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C32 C31 H31 119.9 . . ?
C32 C31 C30 120.2(2) . . ?
C30 C31 H31 119.9 . . ?
C29 C30 C31 120.6(2) . . ?
C29 C30 H30 119.7 . . ?
C31 C30 H30 119.7 . . ?
C22 C23 C24 120.1(2) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
Cl1 C52 H52A 108.6 . . ?
Cl1 C52 H52B 108.6 . . ?
H52A C52 H52B 107.6 . . ?
C53 C52 Cl1 114.5(7) . . ?
C53 C52 H52A 108.6 . . ?
C53 C52 H52B 108.6 . . ?
Cl2 C53 H53A 108.0 . . ?
Cl2 C53 H53B 108.0 . . ?
C52 C53 Cl2 117.3(7) . . ?
C52 C53 H53A 108.0 . . ?
C52 C53 H53B 108.0 . . ?
H53A C53 H53B 107.2 . . ?
Cl2A C53A H53C 108.7 . . ?
Cl2A C53A H53D 108.7 . . ?
H53C C53A H53D 107.6 . . ?
C52A C53A Cl2A 114.1(11) . . ?
C52A C53A H53C 108.7 . . ?
C52A C53A H53D 108.7 . . ?
C53A C52A H52C 110.6 . . ?
C53A C52A H52D 110.6 . . ?
C53A C52A Cl1A 105.9(10) . . ?
H52C C52A H52D 108.7 . . ?
Cl1A C52A H52C 110.6 . . ?
Cl1A C52A H52D 110.6 . . ?

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
Cl1 C52 C53 Cl2 -177.3(6) . . . . ?
O1 C12 C11 C27 -0.3(2) . . . . ?
O1 C12 C11 C10 179.52(15) . . . . ?
O1 C12 C7 C8 -179.47(15) . . . . ?
O1 C12 C7 C41 0.2(3) . . . . ?
C2 C3 C4 C5 0.2(3) . . . . ?
C2 C3 C4 C44 -179.63(17) . . . . ?
C2 C13 C14 C19 -173.70(15) . . . . ?
C2 C13 C14 C15 5.7(2) . . . . ?
C2 C13 C26 C21 173.07(15) . . . . ?
C2 C13 C26 C25 -5.6(3) . . . . ?
C12 O1 C1 C2 179.52(14) . . . . ?
C12 O1 C1 C6 -0.8(3) . . . . ?
C12 C11 C27 C28 71.6(2) . . . . ?
C12 C11 C27 C40 -110.97(18) . . . . ?
C12 C11 C10 C9 0.0(3) . . . . ?
C12 C7 C8 C9 -0.1(3) . . . . ?
C12 C7 C41 C6 0.2(2) . . . . ?
C12 C7 C41 C42 121.15(17) . . . . ?
C12 C7 C41 C43 -118.96(17) . . . . ?
C6 C5 C4 C3 0.0(3) . . . . ?
C6 C5 C4 C44 179.75(16) . . . . ?
C11 C12 C7 C8 0.3(3) . . . . ?
C11 C12 C7 C41 179.99(15) . . . . ?
C11 C27 C28 C33 175.95(15) . . . . ?
C11 C27 C28 C29 -2.7(3) . . . . ?
C11 C27 C40 C35 -176.29(14) . . . . ?
C11 C27 C40 C39 3.6(2) . . . . ?
C7 C12 C11 C27 179.94(16) . . . . ?
C7 C12 C11 C10 -0.3(3) . . . . ?
C7 C8 C9 C10 -0.2(3) . . . . ?
C7 C8 C9 C48 179.14(16) . . . . ?
C1 O1 C12 C11 -179.77(15) . . . . ?
C1 O1 C12 C7 0.0(2) . . . . ?
C1 C2 C3 C4 -0.2(3) . . . . ?
C1 C2 C13 C14 -110.92(19) . . . . ?
C1 C2 C13 C26 72.6(2) . . . . ?
C1 C6 C5 C4 0.0(3) . . . . ?
C1 C6 C41 C7 -1.0(2) . . . . ?
C1 C6 C41 C42 -121.96(17) . . . . ?
C1 C6 C41 C43 118.21(17) . . . . ?
C3 C2 C1 O1 179.78(15) . . . . ?
C3 C2 C1 C6 0.1(3) . . . . ?
C3 C2 C13 C14 68.4(2) . . . . ?
C3 C2 C13 C26 -108.14(19) . . . . ?
C3 C4 C44 C47 -7.7(3) . . . . ?
C3 C4 C44 C46 -125.7(2) . . . . ?
C3 C4 C44 C45 115.3(2) . . . . ?
C8 C7 C41 C6 179.95(15) . . . . ?
C8 C7 C41 C42 -59.1(2) . . . . ?
C8 C7 C41 C43 60.8(2) . . . . ?
C8 C9 C10 C11 0.2(3) . . . . ?
C8 C9 C48 C51 167.26(19) . . . . ?
C8 C9 C48 C49 48.1(2) . . . . ?
C8 C9 C48 C50 -71.9(2) . . . . ?
C27 C11 C10 C9 179.82(16) . . . . ?
C27 C28 C33 C34 0.8(3) . . . . ?
C27 C28 C33 C32 -177.43(18) . . . . ?
C27 C28 C29 C30 178.3(2) . . . . ?
C27 C40 C35 C34 -0.1(2) . . . . ?
C27 C40 C35 C36 178.57(15) . . . . ?
C27 C40 C39 C38 -178.44(17) . . . . ?
C28 C27 C40 C35 1.1(2) . . . . ?
C28 C27 C40 C39 -179.04(15) . . . . ?
C28 C33 C34 C35 0.1(3) . . . . ?
C28 C33 C32 C31 -1.0(4) . . . . ?
C28 C29 C30 C31 -0.8(4) . . . . ?
C13 C2 C1 O1 -0.9(2) . . . . ?
C13 C2 C1 C6 179.40(16) . . . . ?
C13 C2 C3 C4 -179.50(16) . . . . ?
C13 C14 C19 C20 -0.2(2) . . . . ?
C13 C14 C19 C18 178.56(16) . . . . ?
C13 C14 C15 C16 -178.54(18) . . . . ?
C13 C26 C21 C20 1.4(3) . . . . ?
C13 C26 C21 C22 -177.14(18) . . . . ?
C13 C26 C25 C24 178.4(2) . . . . ?
C5 C6 C1 O1 -179.65(15) . . . . ?
C5 C6 C1 C2 0.0(3) . . . . ?
C5 C6 C41 C7 -179.96(15) . . . . ?
C5 C6 C41 C42 59.1(2) . . . . ?
C5 C6 C41 C43 -60.7(2) . . . . ?
C5 C4 C44 C47 172.5(2) . . . . ?
C5 C4 C44 C46 54.5(2) . . . . ?
C5 C4 C44 C45 -64.4(2) . . . . ?
C41 C6 C1 O1 1.4(3) . . . . ?
C41 C6 C1 C2 -178.98(15) . . . . ?
C41 C6 C5 C4 178.97(15) . . . . ?
C41 C7 C8 C9 -179.78(15) . . . . ?
C14 C13 C26 C21 -3.4(2) . . . . ?
C14 C13 C26 C25 177.96(17) . . . . ?
C14 C19 C20 C21 -1.8(3) . . . . ?
C14 C19 C18 C17 0.3(3) . . . . ?
C14 C15 C16 C17 -0.2(3) . . . . ?
C40 C27 C28 C33 -1.4(2) . . . . ?
C40 C27 C28 C29 179.91(16) . . . . ?
C40 C35 C34 C33 -0.5(3) . . . . ?
C40 C35 C36 C37 0.2(3) . . . . ?
C40 C39 C38 C37 -0.4(3) . . . . ?
C26 C13 C14 C19 2.8(2) . . . . ?
C26 C13 C14 C15 -177.82(16) . . . . ?
C26 C21 C20 C19 1.2(3) . . . . ?
C26 C21 C22 C23 -1.5(4) . . . . ?
C26 C25 C24 C23 -1.1(4) . . . . ?
C10 C11 C27 C28 -108.15(19) . . . . ?
C10 C11 C27 C40 69.2(2) . . . . ?
C10 C9 C48 C51 -13.5(3) . . . . ?
C10 C9 C48 C49 -132.6(2) . . . . ?
C10 C9 C48 C50 107.4(2) . . . . ?
C19 C14 C15 C16 0.9(3) . . . . ?
C19 C18 C17 C16 0.4(3) . . . . ?
C33 C28 C29 C30 -0.4(3) . . . . ?
C33 C32 C31 C30 -0.2(4) . . . . ?
C35 C40 C39 C38 1.5(3) . . . . ?
C35 C36 C37 C38 0.9(3) . . . . ?
C21 C26 C25 C24 -0.3(3) . . . . ?
C21 C22 C23 C24 0.1(4) . . . . ?
C48 C9 C10 C11 -179.09(17) . . . . ?
C20 C19 C18 C17 179.0(2) . . . . ?
C20 C21 C22 C23 180.0(2) . . . . ?
C39 C40 C35 C34 179.98(16) . . . . ?
C39 C40 C35 C36 -1.3(2) . . . . ?
C39 C38 C37 C36 -0.8(3) . . . . ?
C34 C33 C32 C31 -179.2(2) . . . . ?
C34 C35 C36 C37 178.85(19) . . . . ?
C15 C14 C19 C20 -179.61(16) . . . . ?
C15 C14 C19 C18 -0.9(3) . . . . ?
C36 C35 C34 C33 -179.14(18) . . . . ?
C25 C26 C21 C20 -179.87(18) . . . . ?
C25 C26 C21 C22 1.6(3) . . . . ?
C25 C24 C23 C22 1.3(4) . . . . ?
C29 C28 C33 C34 179.55(18) . . . . ?
C29 C28 C33 C32 1.3(3) . . . . ?
C18 C19 C20 C21 179.45(18) . . . . ?
C18 C17 C16 C15 -0.4(4) . . . . ?
C32 C33 C34 C35 178.33(19) . . . . ?
C32 C31 C30 C29 1.1(4) . . . . ?
C22 C21 C20 C19 179.73(19) . . . . ?
Cl2A C53A C52A Cl1A -176.0(7) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.623
_oxdiff_exptl_absorpt_empirical_full_min 0.381
####################################################################### 
# 
# 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_mo_190713b_0m
_database_code_depnum_ccdc_archive 'CCDC 2180353'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2022-06-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2021-07-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_chemical_formula_moiety         'C51 H46 O'
_chemical_formula_sum            'C51 H46 O'
_chemical_formula_weight         674.876
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' custom
C 0.00300 0.00200 2.31000 1.02000 1.58900 0.86500 20.84400 10.20800 0.56900
51.65100 0.216 'Custom 4-Gaussian' custom
O 0.01100 0.00600 3.04900 2.28700 1.54600 0.86700 13.27700 5.70100 0.32400
32.90900 0.251 'Custom 4-Gaussian' custom

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_symmetry_Int_Tables_number      2
_cell_length_a                   11.3817(17)
_cell_length_b                   18.157(3)
_cell_length_c                   19.306(3)
_cell_angle_alpha                83.855(2)
_cell_angle_beta                 81.230(2)
_cell_angle_gamma                81.719(2)
_cell_volume                     3887.2(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.834
_cell_measurement_theta_min      2.273
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.5313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Bruker,2008)'
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_meas      .
_exptl_crystal_description       needle
_exptl_crystal_F_000             1440.643
_exptl_crystal_preparation       'Solvent evaporation'
_exptl_crystal_recrystallization_method 'Solvent evaporation'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 0.9713
_diffrn_reflns_Laue_measured_fraction_max 0.9718
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            37364
_diffrn_reflns_point_group_measured_fraction_full 0.9713
_diffrn_reflns_point_group_measured_fraction_max 0.9718
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.63
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.9713
_diffrn_measured_fraction_theta_max 0.9718
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              21
_reflns_limit_k_min              -21
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                9821
_reflns_number_total             14065
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.3464
_refine_diff_density_min         -0.3128
_refine_diff_density_rms         0.0619
_refine_ls_d_res_high            0.8255
_refine_ls_d_res_low             12.4997
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0625
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    191
_refine_ls_number_parameters     1047
_refine_ls_number_reflns         14065
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0731
_refine_ls_restrained_S_all      1.0579
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0851P)²+2.9885P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1960
_refine_ls_wR_factor_ref         0.2234
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C20A-C22A \\sim C20A-C22B
 with sigma of 0.02
 C20A-C21A \\sim C20A-C21B
 with sigma of 0.02
 C20A-C23A \\sim C20A-C23B
 with sigma of 0.02
 C14-C15 \\sim C14-C0AA
 with sigma of 0.02
 C14-C17 \\sim C14-C2AA
 with sigma of 0.02
 C14-C16 \\sim C14-C1AA
 with sigma of 0.02
 C21-C20 \\sim C5AA-C20
 with sigma of 0.02
 C20-C22 \\sim C20-C4AA
 with sigma of 0.02
 C20-C23 \\sim C20-C3AA
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C23B) \\sim Ueq, Uanis(C22B) \\sim Ueq, Uanis(C21B) \\sim Ueq,
Uanis(C0AA) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C4AA) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C5AA) \\sim Ueq, Uanis(C3AA) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(C21B)=Sof(H21g)=Sof(H21h)=Sof(H21i)=Sof(C23B)=Sof(H23g)=Sof(H23h)=
 Sof(H23i)=Sof(C22B)=Sof(H22g)=Sof(H22h)=Sof(H22i)=Sof(H21g)=Sof(H21h)=
 Sof(H21i)=Sof(H23g)=Sof(H23h)=Sof(H23i)=Sof(H22g)=Sof(H22h)=Sof(H22i)=1-FVAR(1)
 Sof(C22A)=Sof(H22d)=Sof(H22e)=Sof(H22f)=Sof(C21A)=Sof(H21d)=Sof(H21e)=
 Sof(H21f)=Sof(C23A)=Sof(H23d)=Sof(H23e)=Sof(H23f)=Sof(H22d)=Sof(H22e)=
 Sof(H22f)=Sof(H21d)=Sof(H21e)=Sof(H21f)=Sof(H23d)=Sof(H23e)=Sof(H23f)=FVAR(1)
 Sof(C0AA)=Sof(H0Aa)=Sof(H0Ab)=Sof(H0Ac)=Sof(C1AA)=Sof(H1Aa)=Sof(H1Ab)=
 Sof(H1Ac)=Sof(C2AA)=Sof(H2Aa)=Sof(H2Ab)=Sof(H2Ac)=Sof(H0Aa)=Sof(H0Ab)=
 Sof(H0Ac)=Sof(H1Aa)=Sof(H1Ab)=Sof(H1Ac)=Sof(H2Aa)=Sof(H2Ab)=Sof(H2Ac)=1-FVAR(2)
 Sof(C15)=Sof(H15a)=Sof(H15b)=Sof(H15c)=Sof(C17)=Sof(H17a)=Sof(H17b)=Sof(H17c)=
 Sof(C16)=Sof(H16a)=Sof(H16b)=Sof(H16c)=Sof(H15a)=Sof(H15b)=Sof(H15c)=Sof(H17a)=
 Sof(H17b)=Sof(H17c)=Sof(H16a)=Sof(H16b)=Sof(H16c)=FVAR(2)
 Sof(C3AA)=Sof(H3Aa)=Sof(H3Ab)=Sof(H3Ac)=Sof(C4AA)=Sof(H4Aa)=Sof(H4Ab)=
 Sof(H4Ac)=Sof(C5AA)=Sof(H5Aa)=Sof(H5Ab)=Sof(H5Ac)=Sof(H3Aa)=Sof(H3Ab)=
 Sof(H3Ac)=Sof(H4Aa)=Sof(H4Ab)=Sof(H4Ac)=Sof(H5Aa)=Sof(H5Ab)=Sof(H5Ac)=1-FVAR(3)
 Sof(C21)=Sof(H21a)=Sof(H21b)=Sof(H21c)=Sof(C22)=Sof(H22a)=Sof(H22b)=Sof(H22c)=
 Sof(C23)=Sof(H23a)=Sof(H23b)=Sof(H23c)=Sof(H21a)=Sof(H21b)=Sof(H21c)=Sof(H22a)=
 Sof(H22b)=Sof(H22c)=Sof(H23a)=Sof(H23b)=Sof(H23c)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C11(H11), C13(H13), C31(H31), C45(H45), C34(H34), C35(H35),
 C36(H36), C37(H37), C26(H26), C29(H29), C28(H28), C27(H27), C48(H48), C51(H51),
  C50(H50), C49(H49), C40(H40), C43(H43), C42(H42), C41(H41), C13A(H13A),
 C11A(H11A), C6A(H6A), C2A(H2A), C45A(H45A), C31A(H31A), C40A(H40A), C43A(H43A),
  C42A(H42A), C41A(H41A), C48A(H48A), C51A(H51A), C50A(H50A), C49A(H49A),
 C26A(H26A), C27A(H27A), C28A(H28A), C29A(H29A), C34A(H34A), C35A(H35A),
 C36A(H36A), C37A(H37A)
5.b Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C19(H19a,H19b,H19c), C18(H18a,H18b,H18c), C15(H15a,H15b,
 H15c), C22(H22a,H22b,H22c), C17(H17a,H17b,H17c), C16(H16a,H16b,H16c), C23(H23a,
 H23b,H23c), C18A(H18d,H18e,H18f), C19A(H19d,H19e,H19f), C16A(H16d,H16e,H16f),
 C15A(H15d,H15e,H15f), C17A(H17d,H17e,H17f), C22A(H22d,H22e,H22f), C21A(H21d,
 H21e,H21f), C23A(H23d,H23e,H23f), C21B(H21g,H21h,H21i), C23B(H23g,H23h,H23i),
 C22B(H22g,H22h,H22i), C0AA(H0Aa,H0Ab,H0Ac), C1AA(H1Aa,H1Ab,H1Ac), C2AA(H2Aa,
 H2Ab,H2Ac), C3AA(H3Aa,H3Ab,H3Ac), C4AA(H4Aa,H4Ab,H4Ac), C5AA(H5Aa,H5Ab,H5Ac)
;
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_disorder_group
O1 O 0.63922(16) 0.83683(9) 0.12324(9) 0.0432(4) Uani 1.000000 . . .
C21 C 0.8360(8) 1.1009(3) -0.0940(4) 0.103(3) Uani 0.687(7) D U 1
C24 C 0.5599(2) 0.73182(14) 0.22204(13) 0.0387(6) Uani 1.000000 . . .
C4 C 0.5757(2) 0.86606(13) 0.18296(13) 0.0376(5) Uani 1.000000 . . .
C33 C 0.6779(2) 0.69561(13) 0.22123(12) 0.0380(5) Uani 1.000000 . . .
C9 C 0.6902(2) 0.88392(13) 0.07048(13) 0.0362(5) Uani 1.000000 . . .
C8 C 0.6767(2) 0.96046(13) 0.07272(13) 0.0378(5) Uani 1.000000 . . .
C10 C 0.7570(2) 0.84827(13) 0.01344(13) 0.0373(5) Uani 1.000000 . . .
C47 C 0.6749(2) 0.72686(14) 0.00962(12) 0.0402(6) Uani 1.000000 . . .
C38 C 0.7726(2) 0.76421(13) 0.01485(12) 0.0370(5) Uani 1.000000 . . .
C25 C 0.4682(2) 0.69253(14) 0.20976(13) 0.0410(6) Uani 1.000000 . . .
C5 C 0.5329(2) 0.81274(14) 0.23446(13) 0.0410(6) Uani 1.000000 . . .
C39 C 0.8851(2) 0.72310(14) 0.02351(13) 0.0414(6) Uani 1.000000 . . .
C3 C 0.5553(2) 0.94140(14) 0.19157(14) 0.0422(6) Uani 1.000000 . . .
C32 C 0.7036(2) 0.61792(14) 0.20868(13) 0.0420(6) Uani 1.000000 . . .
C44 C 0.8975(3) 0.64267(15) 0.02866(13) 0.0464(6) Uani 1.000000 . . .
C30 C 0.4949(3) 0.61390(15) 0.19992(14) 0.0473(6) Uani 1.000000 . . .
C34 C 0.7749(3) 0.73290(16) 0.23148(15) 0.0497(7) Uani 1.000000 . . .
C13 C 0.7319(2) 1.00239(14) 0.01503(14) 0.0441(6) Uani 1.000000 . . .
C46 C 0.6893(3) 0.64653(15) 0.01437(14) 0.0476(6) Uani 1.000000 . . .
C7 C 0.6036(2) 0.99895(14) 0.13495(15) 0.0462(6) Uani 1.000000 . . .
C12 C 0.7980(2) 0.97061(15) -0.04317(14) 0.0454(6) Uani 1.000000 . . .
C11 C 0.8095(2) 0.89301(15) -0.04232(14) 0.0444(6) Uani 1.000000 . . .
C31 C 0.6118(3) 0.57935(15) 0.19956(15) 0.0483(7) Uani 1.000000 . . .
C6 C 0.4670(3) 0.83752(16) 0.29649(15) 0.0506(7) Uani 1.000000 . . .
C45 C 0.7994(3) 0.60747(15) 0.02440(15) 0.0524(7) Uani 1.000000 . . .
C2 C 0.4885(2) 0.96312(16) 0.25473(15) 0.0509(7) Uani 1.000000 . . .
C37 C 0.8245(3) 0.58319(16) 0.20675(14) 0.0501(7) Uani 1.000000 . . .
C40 C 0.9880(3) 0.75680(18) 0.02894(17) 0.0574(8) Uani 1.000000 . . .
C36 C 0.9130(3) 0.62055(18) 0.21741(16) 0.0573(8) Uani 1.000000 . . .
C1 C 0.4433(3) 0.91270(17) 0.30782(15) 0.0547(7) Uani 1.000000 . . .
C26 C 0.3492(3) 0.72723(17) 0.20455(15) 0.0516(7) Uani 1.000000 . . .
C29 C 0.4000(3) 0.57444(19) 0.19010(18) 0.0640(8) Uani 1.000000 . . .
C35 C 0.8876(3) 0.69646(18) 0.22962(17) 0.0577(8) Uani 1.000000 . . .
C48 C 0.5600(3) 0.76482(18) -0.00005(17) 0.0570(7) Uani 1.000000 . . .
C27 C 0.2626(3) 0.6876(2) 0.19290(18) 0.0657(9) Uani 1.000000 . . .
C20 C 0.8577(3) 1.01803(16) -0.10550(16) 0.0558(7) Uani 1.000000 D . .
C43 C 1.0116(3) 0.60236(18) 0.03805(16) 0.0614(8) Uani 1.000000 . . .
C51 C 0.5893(4) 0.6103(2) 0.00869(19) 0.0699(9) Uani 1.000000 . . .
C42 C 1.1066(3) 0.6367(2) 0.04166(18) 0.0721(10) Uani 1.000000 . . .
C28 C 0.2879(3) 0.6099(2) 0.18719(19) 0.0712(9) Uani 1.000000 . . .
C41 C 1.0945(3) 0.7154(2) 0.03752(19) 0.0723(10) Uani 1.000000 . . .
C14 C 0.3693(3) 0.9398(2) 0.37599(18) 0.0732(10) Uani 1.000000 D . .
C50 C 0.4824(4) 0.6491(2) -0.0015(2) 0.0830(11) Uani 1.000000 . . .
C49 C 0.4671(3) 0.7278(2) -0.0058(2) 0.0749(10) Uani 1.000000 . . .
C19 C 0.4991(4) 1.0520(2) 0.1085(2) 0.0867(13) Uani 1.000000 . . .
C18 C 0.6836(4) 1.0434(2) 0.1676(2) 0.0940(14) Uani 1.000000 . . .
C15 C 0.4356(8) 0.9979(6) 0.4055(4) 0.088(3) Uani 0.528(9) D U 1
C22 C 0.8106(7) 1.0066(4) -0.1720(3) 0.096(2) Uani 0.687(7) D U 1
C17 C 0.3233(14) 0.8830(6) 0.4249(6) 0.131(4) Uani 0.528(9) D U 1
C16 C 0.2578(7) 0.9960(6) 0.3527(4) 0.090(3) Uani 0.528(9) D U 1
C23 C 0.9916(5) 0.9932(4) -0.1146(4) 0.098(2) Uani 0.687(7) D U 1
O2 O 0.91743(17) 0.32161(9) 0.41915(9) 0.0451(4) Uani 1.000000 . . .
C38A C 0.8550(2) 0.41346(12) 0.30605(12) 0.0338(5) Uani 1.000000 . . .
C10A C 0.8217(2) 0.43668(13) 0.37978(12) 0.0353(5) Uani 1.000000 . . .
C9A C 0.8554(2) 0.38865(12) 0.43679(12) 0.0345(5) Uani 1.000000 . . .
C11A C 0.7587(2) 0.50633(13) 0.39309(13) 0.0391(6) Uani 1.000000 . . .
C8A C 0.8276(2) 0.40811(13) 0.50557(12) 0.0365(5) Uani 1.000000 . . .
C39A C 0.9747(2) 0.41181(13) 0.27327(12) 0.0368(5) Uani 1.000000 . . .
C4A C 0.9617(2) 0.27159(13) 0.47081(13) 0.0378(5) Uani 1.000000 . . .
C3A C 0.9400(2) 0.28393(13) 0.54120(13) 0.0399(6) Uani 1.000000 . . .
C47A C 0.7663(2) 0.39559(13) 0.26968(13) 0.0380(5) Uani 1.000000 . . .
C12A C 0.7287(2) 0.52885(13) 0.46112(13) 0.0396(6) Uani 1.000000 . . .
C13A C 0.7646(2) 0.47857(13) 0.51579(13) 0.0393(6) Uani 1.000000 . . .
C46A C 0.7968(2) 0.37960(15) 0.19708(14) 0.0446(6) Uani 1.000000 . . .
C44A C 1.0042(2) 0.39478(14) 0.20098(13) 0.0435(6) Uani 1.000000 . . .
C5A C 1.0291(2) 0.20683(14) 0.44581(14) 0.0414(6) Uani 1.000000 . . .
C24A C 1.0440(2) 0.19861(13) 0.36843(14) 0.0434(6) Uani 1.000000 . . .
C45A C 0.9148(3) 0.37957(16) 0.16526(14) 0.0505(7) Uani 1.000000 . . .
C7A C 0.8609(3) 0.35332(15) 0.56767(13) 0.0451(6) Uani 1.000000 . . .
C40A C 1.0683(2) 0.42795(15) 0.30784(15) 0.0465(6) Uani 1.000000 . . .
C25A C 1.1554(3) 0.20496(14) 0.32657(15) 0.0482(7) Uani 1.000000 . . .
C20A C 0.6595(3) 0.60597(14) 0.47479(14) 0.0470(6) Uani 1.000000 D . .
C48A C 0.6450(2) 0.39293(15) 0.30122(15) 0.0478(6) Uani 1.000000 . . .
C1A C 1.0591(2) 0.16304(15) 0.56608(15) 0.0473(6) Uani 1.000000 . . .
C6A C 1.0765(2) 0.15359(15) 0.49430(15) 0.0482(6) Uani 1.000000 . . .
C33A C 0.9427(3) 0.19057(14) 0.33810(15) 0.0491(7) Uani 1.000000 . . .
C2A C 0.9908(2) 0.22811(15) 0.58792(14) 0.0469(6) Uani 1.000000 . . .
C51A C 0.7048(3) 0.36393(18) 0.16054(16) 0.0591(8) Uani 1.000000 . . .
C43A C 1.1251(3) 0.39450(18) 0.16836(16) 0.0582(8) Uani 1.000000 . . .
C30A C 1.1634(3) 0.20418(16) 0.25145(17) 0.0612(8) Uani 1.000000 . . .
C49A C 0.5611(3) 0.37678(17) 0.26419(17) 0.0581(8) Uani 1.000000 . . .
C32A C 0.9506(3) 0.19288(17) 0.26311(18) 0.0629(9) Uani 1.000000 . . .
C41A C 1.1826(3) 0.42696(18) 0.27420(17) 0.0584(8) Uani 1.000000 . . .
C42A C 1.2115(3) 0.40966(19) 0.20331(18) 0.0641(9) Uani 1.000000 . . .
C26A C 1.2597(3) 0.21396(16) 0.35494(19) 0.0598(8) Uani 1.000000 . . .
C14A C 1.1192(3) 0.10395(17) 0.61745(17) 0.0597(8) Uani 1.000000 . . .
C50A C 0.5918(3) 0.36288(19) 0.19271(18) 0.0649(9) Uani 1.000000 . . .
C34A C 0.8291(3) 0.18297(17) 0.3785(2) 0.0633(8) Uani 1.000000 . . .
C31A C 1.0603(4) 0.19946(19) 0.22241(18) 0.0744(10) Uani 1.000000 . . .
C18A C 0.9242(4) 0.39173(19) 0.61568(19) 0.0811(12) Uani 1.000000 . . .
C37A C 0.8440(5) 0.1878(2) 0.2336(2) 0.0885(13) Uani 1.000000 . . .
C19A C 0.7438(3) 0.3283(2) 0.60944(18) 0.0759(11) Uani 1.000000 . . .
C35A C 0.7309(4) 0.1788(2) 0.3479(3) 0.0848(12) Uani 1.000000 . . .
C29A C 1.2765(4) 0.2094(2) 0.2100(2) 0.0838(12) Uani 1.000000 . . .
C16A C 1.1081(6) 0.0257(2) 0.6014(3) 0.133(2) Uani 1.000000 . . .
C27A C 1.3662(3) 0.2191(2) 0.3124(2) 0.0791(11) Uani 1.000000 . . .
C28A C 1.3734(4) 0.2157(2) 0.2386(3) 0.0893(13) Uani 1.000000 . . .
C15A C 1.0641(4) 0.1127(2) 0.6934(2) 0.0907(13) Uani 1.000000 . . .
C17A C 1.2491(4) 0.1148(4) 0.6107(3) 0.132(2) Uani 1.000000 . . .
C36A C 0.7385(4) 0.1819(2) 0.2746(3) 0.0977(15) Uani 1.000000 . . .
C22A C 0.5446(7) 0.5978(3) 0.5242(5) 0.106(4) Uani 0.641(8) D . 1
C21A C 0.7358(8) 0.6497(4) 0.5108(5) 0.108(3) Uani 0.641(8) D U 1
C23A C 0.6282(8) 0.6525(4) 0.4093(3) 0.101(3) Uani 0.641(8) D . 1
C21B C 0.6314(12) 0.6192(6) 0.5517(5) 0.077(4) Uani 0.359(8) D U 2
C23B C 0.7360(11) 0.6656(5) 0.4407(7) 0.083(4) Uani 0.359(8) D U 2
C22B C 0.5446(11) 0.6140(8) 0.4411(8) 0.094(4) Uani 0.359(8) D U 2
C0AA C 0.4135(9) 0.8854(5) 0.4419(4) 0.079(3) Uani 0.472(9) D U 2
C1AA C 0.3752(17) 1.0152(8) 0.3885(9) 0.146(6) Uani 0.472(9) D U 2
C2AA C 0.2419(8) 0.9238(9) 0.3785(6) 0.119(4) Uani 0.472(9) D U 2
C3AA C 0.9189(16) 0.9741(8) -0.1671(7) 0.092(5) Uani 0.313(7) D U 2
C4AA C 0.7654(13) 1.0792(8) -0.1341(8) 0.092(5) Uani 0.313(7) D U 2
C5AA C 0.9546(13) 1.0562(9) -0.0816(7) 0.086(4) Uani 0.313(7) D U 2
H2 H 0.4736(2) 1.01374(16) 0.26150(15) 0.0611(8) Uiso 1.000000 R . .
H6 H 0.4381(3) 0.80259(16) 0.33135(15) 0.0607(8) Uiso 1.000000 R . .
H11 H 0.8542(2) 0.87028(15) -0.08059(14) 0.0533(7) Uiso 1.000000 R . .
H13 H 0.7238(2) 1.05401(14) 0.01582(14) 0.0529(7) Uiso 1.000000 R . .
H31 H 0.6289(3) 0.52873(15) 0.19297(15) 0.0579(8) Uiso 1.000000 R . .
H45 H 0.8079(3) 0.55554(15) 0.02844(15) 0.0629(9) Uiso 1.000000 R . .
H34 H 0.7605(3) 0.78319(16) 0.23960(15) 0.0596(8) Uiso 1.000000 R . .
H35 H 0.9494(3) 0.72213(18) 0.23655(17) 0.0693(9) Uiso 1.000000 R . .
H36 H 0.9908(3) 0.59620(18) 0.21671(16) 0.0687(9) Uiso 1.000000 R . .
H37 H 0.8427(3) 0.53320(16) 0.19784(14) 0.0601(8) Uiso 1.000000 R . .
H26 H 0.3303(3) 0.77818(17) 0.20922(15) 0.0619(8) Uiso 1.000000 R . .
H29 H 0.4156(3) 0.52334(19) 0.18561(18) 0.0767(10) Uiso 1.000000 R . .
H28 H 0.2270(3) 0.5829(2) 0.18140(19) 0.0854(11) Uiso 1.000000 R . .
H27 H 0.1860(3) 0.7118(2) 0.18865(18) 0.0789(10) Uiso 1.000000 R . .
H48 H 0.5479(3) 0.81674(18) -0.00257(17) 0.0684(9) Uiso 1.000000 R . .
H51 H 0.5977(4) 0.5584(2) 0.01207(19) 0.0839(11) Uiso 1.000000 R . .
H50 H 0.4186(4) 0.6239(2) -0.0057(2) 0.0996(14) Uiso 1.000000 R . .
H49 H 0.3930(3) 0.7544(2) -0.0125(2) 0.0899(12) Uiso 1.000000 R . .
H40 H 0.9821(3) 0.80861(18) 0.02655(17) 0.0689(9) Uiso 1.000000 R . .
H43 H 1.0204(3) 0.55042(18) 0.04179(16) 0.0737(10) Uiso 1.000000 R . .
H42 H 1.1804(3) 0.6088(2) 0.04690(18) 0.0865(12) Uiso 1.000000 R . .
H41 H 1.1604(3) 0.7391(2) 0.04071(19) 0.0868(11) Uiso 1.000000 R . .
H13A H 0.7455(2) 0.49271(13) 0.56147(13) 0.0471(7) Uiso 1.000000 R . .
H11A H 0.7358(2) 0.53889(13) 0.35552(13) 0.0470(7) Uiso 1.000000 R . .
H6A H 1.1215(2) 0.11011(15) 0.47857(15) 0.0578(8) Uiso 1.000000 R . .
H2A H 0.9780(2) 0.23510(15) 0.63564(14) 0.0563(8) Uiso 1.000000 R . .
H45A H 0.9345(3) 0.36900(16) 0.11851(14) 0.0607(8) Uiso 1.000000 R . .
H31A H 1.0654(4) 0.20077(19) 0.17376(18) 0.0892(13) Uiso 1.000000 R . .
H40A H 1.0512(2) 0.43943(15) 0.35441(15) 0.0558(8) Uiso 1.000000 R . .
H43A H 1.1451(3) 0.38358(18) 0.12171(16) 0.0698(9) Uiso 1.000000 R . .
H42A H 1.2899(3) 0.40875(19) 0.18088(18) 0.0770(10) Uiso 1.000000 R . .
H41A H 1.2423(3) 0.43776(18) 0.29801(17) 0.0700(9) Uiso 1.000000 R . .
H48A H 0.6230(2) 0.40245(15) 0.34813(15) 0.0573(8) Uiso 1.000000 R . .
H51A H 0.7234(3) 0.35424(18) 0.11351(16) 0.0709(9) Uiso 1.000000 R . .
H50A H 0.5331(3) 0.35289(19) 0.16766(18) 0.0779(10) Uiso 1.000000 R . .
H49A H 0.4828(3) 0.37487(17) 0.28608(17) 0.0697(9) Uiso 1.000000 R . .
H26A H 1.2555(3) 0.21638(16) 0.40314(19) 0.0717(9) Uiso 1.000000 R . .
H27A H 1.4341(3) 0.2248(2) 0.3317(2) 0.0949(13) Uiso 1.000000 R . .
H28A H 1.4466(4) 0.2180(2) 0.2100(3) 0.1071(16) Uiso 1.000000 R . .
H29A H 1.2832(4) 0.2084(2) 0.1615(2) 0.1005(14) Uiso 1.000000 R . .
H34A H 0.8219(3) 0.18076(17) 0.4273(2) 0.0760(10) Uiso 1.000000 R . .
H35A H 0.6579(4) 0.1740(2) 0.3758(3) 0.1018(14) Uiso 1.000000 R . .
H36A H 0.6702(4) 0.1798(2) 0.2542(3) 0.1172(18) Uiso 1.000000 R . .
H37A H 0.8480(5) 0.1887(2) 0.1850(2) 0.1063(16) Uiso 1.000000 R . .
H21a H 0.880(4) 1.1282(5) -0.1324(16) 0.155(4) Uiso 0.687(7) GR . 1
H21b H 0.7520(10) 1.1185(8) -0.092(3) 0.155(4) Uiso 0.687(7) GR . 1
H21c H 0.863(5) 1.1082(5) -0.0507(16) 0.155(4) Uiso 0.687(7) GR . 1
H19a H 0.5300(4) 1.0910(10) 0.0763(13) 0.1300(19) Uiso 1.000000 GR . .
H19b H 0.4532(16) 1.0246(4) 0.0849(14) 0.1300(19) Uiso 1.000000 GR . .
H19c H 0.4486(16) 1.0736(13) 0.1477(3) 0.1300(19) Uiso 1.000000 GR . .
H18a H 0.7505(17) 1.0102(4) 0.1825(16) 0.141(2) Uiso 1.000000 GR . .
H18b H 0.712(2) 1.0813(12) 0.1333(6) 0.141(2) Uiso 1.000000 GR . .
H18c H 0.6379(9) 1.0664(16) 0.2075(11) 0.141(2) Uiso 1.000000 GR . .
H15a H 0.507(3) 0.9725(8) 0.423(3) 0.133(4) Uiso 0.528(9) GR . 1
H15b H 0.457(5) 1.035(2) 0.3687(9) 0.133(4) Uiso 0.528(9) GR . 1
H15c H 0.383(2) 1.021(3) 0.443(2) 0.133(4) Uiso 0.528(9) GR . 1
H22a H 0.7256(10) 1.022(3) -0.1669(11) 0.144(3) Uiso 0.687(7) GR . 1
H22b H 0.849(3) 1.036(2) -0.2109(5) 0.144(3) Uiso 0.687(7) GR . 1
H22c H 0.827(4) 0.9547(6) -0.1805(15) 0.144(3) Uiso 0.687(7) GR . 1
H17a H 0.266(7) 0.861(4) 0.405(2) 0.196(6) Uiso 0.528(9) GR . 1
H17b H 0.3880(17) 0.845(3) 0.436(4) 0.196(6) Uiso 0.528(9) GR . 1
H17c H 0.285(8) 0.9044(12) 0.467(2) 0.196(6) Uiso 0.528(9) GR . 1
H16a H 0.2864(7) 1.0381(18) 0.324(3) 0.134(4) Uiso 0.528(9) GR . 1
H16b H 0.213(3) 0.9707(12) 0.326(3) 0.134(4) Uiso 0.528(9) GR . 1
H16c H 0.207(3) 1.013(3) 0.3938(4) 0.134(4) Uiso 0.528(9) GR . 1
H23a H 1.0299(8) 1.022(2) -0.1538(18) 0.148(4) Uiso 0.687(7) GR . 1
H23b H 1.0229(10) 1.000(3) -0.0726(11) 0.148(4) Uiso 0.687(7) GR . 1
H23c H 1.0069(6) 0.9413(9) -0.123(3) 0.148(4) Uiso 0.687(7) GR . 1
H18d H 0.8696(9) 0.4315(10) 0.6361(12) 0.1217(18) Uiso 1.000000 GR . .
H18e H 0.950(2) 0.3560(4) 0.6524(9) 0.1217(18) Uiso 1.000000 GR . .
H18f H 0.9923(15) 0.4117(14) 0.5886(3) 0.1217(18) Uiso 1.000000 GR . .
H19d H 0.7631(4) 0.2912(11) 0.6467(9) 0.1138(16) Uiso 1.000000 GR . .
H19e H 0.6944(11) 0.3706(4) 0.6290(12) 0.1138(16) Uiso 1.000000 GR . .
H19f H 0.7013(12) 0.3075(14) 0.5785(4) 0.1138(16) Uiso 1.000000 GR . .
H16d H 1.0289(14) 0.0240(7) 0.591(3) 0.199(3) Uiso 1.000000 GR . .
H16e H 1.166(3) 0.0121(10) 0.5616(16) 0.199(3) Uiso 1.000000 GR . .
H16f H 1.123(4) -0.0087(4) 0.6415(9) 0.199(3) Uiso 1.000000 GR . .
H15d H 1.077(3) 0.1602(8) 0.7064(6) 0.136(2) Uiso 1.000000 GR . .
H15e H 0.9796(7) 0.1100(18) 0.6984(4) 0.136(2) Uiso 1.000000 GR . .
H15f H 1.101(2) 0.0735(11) 0.7236(3) 0.136(2) Uiso 1.000000 GR . .
H17d H 1.2852(11) 0.112(3) 0.5626(6) 0.197(3) Uiso 1.000000 GR . .
H17e H 1.2552(4) 0.1629(12) 0.625(2) 0.197(3) Uiso 1.000000 GR . .
H17f H 1.2899(10) 0.0766(16) 0.640(2) 0.197(3) Uiso 1.000000 GR . .
H22d H 0.494(2) 0.572(3) 0.5025(14) 0.158(5) Uiso 0.641(8) GR . 1
H22e H 0.5630(7) 0.570(3) 0.5672(13) 0.158(5) Uiso 0.641(8) GR . 1
H22f H 0.504(3) 0.6464(4) 0.534(3) 0.158(5) Uiso 0.641(8) GR . 1
H21d H 0.758(5) 0.6210(16) 0.5527(19) 0.163(4) Uiso 0.641(8) GR . 1
H21e H 0.807(3) 0.659(3) 0.4792(13) 0.163(4) Uiso 0.641(8) GR . 1
H21f H 0.690(2) 0.6964(16) 0.523(3) 0.163(4) Uiso 0.641(8) GR . 1
H23d H 0.6999(10) 0.657(3) 0.3767(13) 0.151(5) Uiso 0.641(8) GR . 1
H23e H 0.574(4) 0.6287(17) 0.3881(17) 0.151(5) Uiso 0.641(8) GR . 1
H23f H 0.590(5) 0.7011(12) 0.4213(6) 0.151(5) Uiso 0.641(8) GR . 1
H21g H 0.587(7) 0.581(3) 0.5764(9) 0.116(5) Uiso 0.359(8) GR . 2
H21h H 0.7048(12) 0.618(5) 0.5709(12) 0.116(5) Uiso 0.359(8) GR . 2
H21i H 0.585(7) 0.667(2) 0.5568(6) 0.116(5) Uiso 0.359(8) GR . 2
H23g H 0.807(4) 0.661(3) 0.463(3) 0.124(6) Uiso 0.359(8) GR . 2
H23h H 0.758(7) 0.659(3) 0.3915(12) 0.124(6) Uiso 0.359(8) GR . 2
H23i H 0.691(3) 0.7141(6) 0.446(4) 0.124(6) Uiso 0.359(8) GR . 2
H22g H 0.5646(12) 0.605(5) 0.3922(15) 0.140(6) Uiso 0.359(8) GR . 2
H22h H 0.494(4) 0.578(4) 0.465(3) 0.140(6) Uiso 0.359(8) GR . 2
H22i H 0.503(5) 0.6635(19) 0.445(5) 0.140(6) Uiso 0.359(8) GR . 2
H0Aa H 0.392(5) 0.8365(11) 0.4404(19) 0.118(4) Uiso 0.472(9) GR . 2
H0Ab H 0.4991(11) 0.882(3) 0.4390(19) 0.118(4) Uiso 0.472(9) GR . 2
H0Ac H 0.376(5) 0.9053(19) 0.4851(4) 0.118(4) Uiso 0.472(9) GR . 2
H1Aa H 0.456(3) 1.0209(19) 0.393(7) 0.219(9) Uiso 0.472(9) GR . 2
H1Ab H 0.350(11) 1.0482(10) 0.350(3) 0.219(9) Uiso 0.472(9) GR . 2
H1Ac H 0.324(9) 1.027(2) 0.431(4) 0.219(9) Uiso 0.472(9) GR . 2
H2Aa H 0.209(3) 0.949(5) 0.338(3) 0.179(7) Uiso 0.472(9) GR . 2
H2Ab H 0.2413(13) 0.8710(11) 0.379(5) 0.179(7) Uiso 0.472(9) GR . 2
H2Ac H 0.194(2) 0.941(5) 0.421(3) 0.179(7) Uiso 0.472(9) GR . 2
H3Aa H 0.860(2) 0.953(5) -0.186(4) 0.137(7) Uiso 0.313(7) GR . 2
H3Ab H 0.958(9) 1.0069(15) -0.203(3) 0.137(7) Uiso 0.313(7) GR . 2
H3Ac H 0.977(7) 0.935(4) -0.1509(14) 0.137(7) Uiso 0.313(7) GR . 2
H4Aa H 0.721(7) 1.106(4) -0.0960(11) 0.138(7) Uiso 0.313(7) GR . 2
H4Ab H 0.8061(14) 1.113(4) -0.168(4) 0.138(7) Uiso 0.313(7) GR . 2
H4Ac H 0.711(6) 1.0568(10) -0.157(5) 0.138(7) Uiso 0.313(7) GR . 2
H5Aa H 0.989(7) 1.088(5) -0.1202(17) 0.129(6) Uiso 0.313(7) GR . 2
H5Ab H 0.919(2) 1.086(5) -0.043(4) 0.129(6) Uiso 0.313(7) GR . 2
H5Ac H 1.016(5) 1.0189(9) -0.066(5) 0.129(6) Uiso 0.313(7) GR . 2


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 C4 1.378(3) . ?
O1 C9 1.372(3) . ?
C21 C20 1.523(7) . ?
C21 H21a 0.9600 . ?
C21 H21b 0.9600 . ?
C21 H21c 0.9600 . ?
C24 C33 1.406(3) . ?
C24 C25 1.408(4) . ?
C24 C5 1.494(3) . ?
C4 C5 1.395(4) . ?
C4 C3 1.378(3) . ?
C33 C32 1.438(3) . ?
C33 C34 1.423(4) . ?
C9 C8 1.381(3) . ?
C9 C10 1.402(3) . ?
C8 C13 1.399(4) . ?
C8 C7 1.527(4) . ?
C10 C38 1.509(3) . ?
C10 C11 1.390(3) . ?
C47 C38 1.405(3) . ?
C47 C46 1.439(4) . ?
C47 C48 1.417(4) . ?
C38 C39 1.410(4) . ?
C25 C30 1.443(4) . ?
C25 C26 1.422(4) . ?
C5 C6 1.394(4) . ?
C39 C44 1.441(4) . ?
C39 C40 1.419(4) . ?
C3 C7 1.525(4) . ?
C3 C2 1.398(4) . ?
C32 C31 1.381(4) . ?
C32 C37 1.425(4) . ?
C44 C45 1.381(4) . ?
C44 C43 1.422(4) . ?
C30 C31 1.387(4) . ?
C30 C29 1.425(4) . ?
C34 C35 1.354(4) . ?
C34 H34 0.9300 . ?
C13 C12 1.385(4) . ?
C13 H13 0.9300 . ?
C46 C45 1.378(4) . ?
C46 C51 1.417(4) . ?
C7 C19 1.534(4) . ?
C7 C18 1.542(4) . ?
C12 C11 1.395(4) . ?
C12 C20 1.532(4) . ?
C11 H11 0.9300 . ?
C31 H31 0.9300 . ?
C6 C1 1.387(4) . ?
C6 H6 0.9300 . ?
C45 H45 0.9300 . ?
C2 C1 1.388(4) . ?
C2 H2 0.9300 . ?
C37 C36 1.344(4) . ?
C37 H37 0.9300 . ?
C40 C41 1.354(4) . ?
C40 H40 0.9300 . ?
C36 C35 1.405(4) . ?
C36 H36 0.9300 . ?
C1 C14 1.538(4) . ?
C26 C27 1.360(4) . ?
C26 H26 0.9300 . ?
C29 C28 1.350(5) . ?
C29 H29 0.9300 . ?
C35 H35 0.9300 . ?
C48 C49 1.356(4) . ?
C48 H48 0.9300 . ?
C27 C28 1.411(5) . ?
C27 H27 0.9300 . ?
C20 C22 1.509(7) . ?
C20 C23 1.515(7) . ?
C20 C3AA 1.525(13) . ?
C20 C4AA 1.533(13) . ?
C20 C5AA 1.534(12) . ?
C43 C42 1.338(5) . ?
C43 H43 0.9300 . ?
C51 C50 1.345(5) . ?
C51 H51 0.9300 . ?
C42 C41 1.410(5) . ?
C42 H42 0.9300 . ?
C28 H28 0.9300 . ?
C41 H41 0.9300 . ?
C14 C15 1.580(9) . ?
C14 C17 1.424(11) . ?
C14 C16 1.599(9) . ?
C14 C0AA 1.622(9) . ?
C14 C1AA 1.428(14) . ?
C14 C2AA 1.512(11) . ?
C50 C49 1.410(5) . ?
C50 H50 0.9300 . ?
C49 H49 0.9300 . ?
C19 H19a 0.9600 . ?
C19 H19b 0.9600 . ?
C19 H19c 0.9600 . ?
C18 H18a 0.9600 . ?
C18 H18b 0.9600 . ?
C18 H18c 0.9600 . ?
C15 H15a 0.9600 . ?
C15 H15b 0.9600 . ?
C15 H15c 0.9600 . ?
C22 H22a 0.9600 . ?
C22 H22b 0.9600 . ?
C22 H22c 0.9600 . ?
C17 H17a 0.9600 . ?
C17 H17b 0.9600 . ?
C17 H17c 0.9600 . ?
C16 H16a 0.9600 . ?
C16 H16b 0.9600 . ?
C16 H16c 0.9600 . ?
C23 H23a 0.9600 . ?
C23 H23b 0.9600 . ?
C23 H23c 0.9600 . ?
O2 C9A 1.365(3) . ?
O2 C4A 1.379(3) . ?
C38A C10A 1.505(3) . ?
C38A C39A 1.409(3) . ?
C38A C47A 1.407(3) . ?
C10A C9A 1.395(3) . ?
C10A C11A 1.390(3) . ?
C9A C8A 1.389(3) . ?
C11A C12A 1.395(3) . ?
C11A H11A 0.9300 . ?
C8A C13A 1.392(3) . ?
C8A C7A 1.531(3) . ?
C39A C44A 1.441(3) . ?
C39A C40A 1.419(4) . ?
C4A C3A 1.380(3) . ?
C4A C5A 1.398(3) . ?
C3A C7A 1.527(3) . ?
C3A C2A 1.403(4) . ?
C47A C46A 1.442(3) . ?
C47A C48A 1.426(4) . ?
C12A C13A 1.390(4) . ?
C12A C20A 1.533(3) . ?
C13A H13A 0.9300 . ?
C46A C45A 1.390(4) . ?
C46A C51A 1.424(4) . ?
C44A C45A 1.386(4) . ?
C44A C43A 1.423(4) . ?
C5A C24A 1.499(4) . ?
C5A C6A 1.383(4) . ?
C24A C25A 1.408(4) . ?
C24A C33A 1.402(4) . ?
C45A H45A 0.9300 . ?
C7A C18A 1.534(4) . ?
C7A C19A 1.550(4) . ?
C40A C41A 1.361(4) . ?
C40A H40A 0.9300 . ?
C25A C30A 1.441(4) . ?
C25A C26A 1.418(4) . ?
C20A C22A 1.512(6) . ?
C20A C21A 1.538(7) . ?
C20A C23A 1.504(6) . ?
C20A C21B 1.508(10) . ?
C20A C23B 1.519(11) . ?
C20A C22B 1.529(12) . ?
C48A C49A 1.358(4) . ?
C48A H48A 0.9300 . ?
C1A C6A 1.395(4) . ?
C1A C2A 1.386(4) . ?
C1A C14A 1.540(4) . ?
C6A H6A 0.9300 . ?
C33A C32A 1.433(4) . ?
C33A C34A 1.421(4) . ?
C2A H2A 0.9300 . ?
C51A C50A 1.342(5) . ?
C51A H51A 0.9300 . ?
C43A C42A 1.348(5) . ?
C43A H43A 0.9300 . ?
C30A C31A 1.392(5) . ?
C30A C29A 1.418(5) . ?
C49A C50A 1.411(5) . ?
C49A H49A 0.9300 . ?
C32A C31A 1.384(5) . ?
C32A C37A 1.435(5) . ?
C41A C42A 1.416(4) . ?
C41A H41A 0.9300 . ?
C42A H42A 0.9300 . ?
C26A C27A 1.366(5) . ?
C26A H26A 0.9300 . ?
C14A C16A 1.514(5) . ?
C14A C15A 1.521(5) . ?
C14A C17A 1.504(5) . ?
C50A H50A 0.9300 . ?
C34A C35A 1.356(5) . ?
C34A H34A 0.9300 . ?
C31A H31A 0.9300 . ?
C18A H18d 0.9600 . ?
C18A H18e 0.9600 . ?
C18A H18f 0.9600 . ?
C37A C36A 1.346(6) . ?
C37A H37A 0.9300 . ?
C19A H19d 0.9600 . ?
C19A H19e 0.9600 . ?
C19A H19f 0.9600 . ?
C35A C36A 1.400(7) . ?
C35A H35A 0.9300 . ?
C29A C28A 1.330(6) . ?
C29A H29A 0.9300 . ?
C16A H16d 0.9600 . ?
C16A H16e 0.9600 . ?
C16A H16f 0.9600 . ?
C27A C28A 1.422(6) . ?
C27A H27A 0.9300 . ?
C28A H28A 0.9300 . ?
C15A H15d 0.9600 . ?
C15A H15e 0.9600 . ?
C15A H15f 0.9600 . ?
C17A H17d 0.9600 . ?
C17A H17e 0.9600 . ?
C17A H17f 0.9600 . ?
C36A H36A 0.9300 . ?
C22A H22d 0.9600 . ?
C22A H22e 0.9600 . ?
C22A H22f 0.9600 . ?
C21A H21d 0.9600 . ?
C21A H21e 0.9600 . ?
C21A H21f 0.9600 . ?
C23A H23d 0.9600 . ?
C23A H23e 0.9600 . ?
C23A H23f 0.9600 . ?
C21B H21g 0.9600 . ?
C21B H21h 0.9600 . ?
C21B H21i 0.9600 . ?
C23B H23g 0.9600 . ?
C23B H23h 0.9600 . ?
C23B H23i 0.9600 . ?
C22B H22g 0.9600 . ?
C22B H22h 0.9600 . ?
C22B H22i 0.9600 . ?
C0AA H0Aa 0.9600 . ?
C0AA H0Ab 0.9600 . ?
C0AA H0Ac 0.9600 . ?
C1AA H1Aa 0.9600 . ?
C1AA H1Ab 0.9600 . ?
C1AA H1Ac 0.9600 . ?
C2AA H2Aa 0.9600 . ?
C2AA H2Ab 0.9600 . ?
C2AA H2Ac 0.9600 . ?
C3AA H3Aa 0.9600 . ?
C3AA H3Ab 0.9600 . ?
C3AA H3Ac 0.9600 . ?
C4AA H4Aa 0.9600 . ?
C4AA H4Ab 0.9600 . ?
C4AA H4Ac 0.9600 . ?
C5AA H5Aa 0.9600 . ?
C5AA H5Ab 0.9600 . ?
C5AA H5Ac 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 O1 C4 119.21(18) . . ?
H21a C21 C20 109.5 . . ?
H21b C21 C20 109.5 . . ?
H21b C21 H21a 109.5 . . ?
H21c C21 C20 109.5 . . ?
H21c C21 H21a 109.5 . . ?
H21c C21 H21b 109.5 . . ?
C25 C24 C33 120.2(2) . . ?
C5 C24 C33 119.7(2) . . ?
C5 C24 C25 120.1(2) . . ?
C5 C4 O1 114.3(2) . . ?
C3 C4 O1 123.4(2) . . ?
C3 C4 C5 122.4(2) . . ?
C32 C33 C24 119.4(2) . . ?
C34 C33 C24 122.8(2) . . ?
C34 C33 C32 117.8(2) . . ?
C8 C9 O1 123.0(2) . . ?
C10 C9 O1 114.7(2) . . ?
C10 C9 C8 122.3(2) . . ?
C13 C8 C9 117.4(2) . . ?
C7 C8 C9 122.0(2) . . ?
C7 C8 C13 120.6(2) . . ?
C38 C10 C9 120.1(2) . . ?
C11 C10 C9 117.5(2) . . ?
C11 C10 C38 122.3(2) . . ?
C46 C47 C38 119.9(2) . . ?
C48 C47 C38 122.9(2) . . ?
C48 C47 C46 117.2(2) . . ?
C47 C38 C10 120.3(2) . . ?
C39 C38 C10 119.6(2) . . ?
C39 C38 C47 120.1(2) . . ?
C30 C25 C24 119.5(2) . . ?
C26 C25 C24 122.9(2) . . ?
C26 C25 C30 117.5(2) . . ?
C4 C5 C24 119.5(2) . . ?
C6 C5 C24 122.4(2) . . ?
C6 C5 C4 118.1(2) . . ?
C44 C39 C38 119.2(2) . . ?
C40 C39 C38 123.3(2) . . ?
C40 C39 C44 117.4(2) . . ?
C7 C3 C4 121.7(2) . . ?
C2 C3 C4 117.2(2) . . ?
C2 C3 C7 121.1(2) . . ?
C31 C32 C33 119.7(2) . . ?
C37 C32 C33 118.1(2) . . ?
C37 C32 C31 122.2(2) . . ?
C45 C44 C39 119.4(2) . . ?
C43 C44 C39 118.2(3) . . ?
C43 C44 C45 122.4(3) . . ?
C31 C30 C25 119.2(2) . . ?
C29 C30 C25 118.7(3) . . ?
C29 C30 C31 122.1(3) . . ?
C35 C34 C33 121.2(3) . . ?
H34 C34 C33 119.41(15) . . ?
H34 C34 C35 119.41(18) . . ?
C12 C13 C8 123.1(2) . . ?
H13 C13 C8 118.47(14) . . ?
H13 C13 C12 118.47(15) . . ?
C45 C46 C47 119.0(3) . . ?
C51 C46 C47 118.7(3) . . ?
C51 C46 C45 122.3(3) . . ?
C3 C7 C8 110.6(2) . . ?
C19 C7 C8 108.6(3) . . ?
C19 C7 C3 109.8(2) . . ?
C18 C7 C8 109.7(2) . . ?
C18 C7 C3 108.2(3) . . ?
C18 C7 C19 109.9(3) . . ?
C11 C12 C13 117.0(2) . . ?
C20 C12 C13 121.8(2) . . ?
C20 C12 C11 121.1(2) . . ?
C12 C11 C10 122.7(2) . . ?
H11 C11 C10 118.67(14) . . ?
H11 C11 C12 118.67(15) . . ?
C30 C31 C32 121.9(2) . . ?
H31 C31 C32 119.04(15) . . ?
H31 C31 C30 119.04(16) . . ?
C1 C6 C5 122.0(3) . . ?
H6 C6 C5 119.00(16) . . ?
H6 C6 C1 119.00(17) . . ?
C46 C45 C44 122.4(2) . . ?
H45 C45 C44 118.81(16) . . ?
H45 C45 C46 118.81(16) . . ?
C1 C2 C3 123.1(2) . . ?
H2 C2 C3 118.44(16) . . ?
H2 C2 C1 118.44(15) . . ?
C36 C37 C32 122.0(3) . . ?
H37 C37 C32 119.02(16) . . ?
H37 C37 C36 119.02(17) . . ?
C41 C40 C39 121.6(3) . . ?
H40 C40 C39 119.19(16) . . ?
H40 C40 C41 119.2(2) . . ?
C35 C36 C37 119.8(3) . . ?
H36 C36 C37 120.08(17) . . ?
H36 C36 C35 120.08(18) . . ?
C2 C1 C6 117.3(2) . . ?
C14 C1 C6 121.8(3) . . ?
C14 C1 C2 120.9(3) . . ?
C27 C26 C25 121.4(3) . . ?
H26 C26 C25 119.28(17) . . ?
H26 C26 C27 119.3(2) . . ?
C28 C29 C30 121.2(3) . . ?
H29 C29 C30 119.40(18) . . ?
H29 C29 C28 119.4(2) . . ?
C36 C35 C34 121.1(3) . . ?
H35 C35 C34 119.44(18) . . ?
H35 C35 C36 119.44(18) . . ?
C49 C48 C47 122.1(3) . . ?
H48 C48 C47 118.96(16) . . ?
H48 C48 C49 119.0(2) . . ?
C28 C27 C26 120.6(3) . . ?
H27 C27 C26 119.7(2) . . ?
H27 C27 C28 119.72(19) . . ?
C12 C20 C21 112.0(3) . . ?
C22 C20 C21 109.2(5) . . ?
C22 C20 C12 110.0(3) . . ?
C23 C20 C21 108.4(5) . . ?
C23 C20 C12 108.7(3) . . ?
C23 C20 C22 108.5(5) . . ?
C3AA C20 C21 133.5(6) . . ?
C3AA C20 C12 114.4(5) . . ?
C3AA C20 C22 50.8(7) . . ?
C3AA C20 C23 59.1(7) . . ?
C4AA C20 C21 51.2(7) . . ?
C4AA C20 C12 110.6(5) . . ?
C4AA C20 C22 61.7(7) . . ?
C4AA C20 C23 140.3(6) . . ?
C4AA C20 C3AA 107.2(9) . . ?
C5AA C20 C21 59.2(6) . . ?
C5AA C20 C12 109.7(5) . . ?
C5AA C20 C22 140.0(6) . . ?
C5AA C20 C23 52.6(6) . . ?
C5AA C20 C3AA 106.6(9) . . ?
C5AA C20 C4AA 107.9(9) . . ?
C42 C43 C44 122.1(3) . . ?
H43 C43 C44 118.93(19) . . ?
H43 C43 C42 118.9(2) . . ?
C50 C51 C46 121.7(3) . . ?
H51 C51 C46 119.13(19) . . ?
H51 C51 C50 119.1(2) . . ?
C41 C42 C43 119.8(3) . . ?
H42 C42 C43 120.1(2) . . ?
H42 C42 C41 120.1(2) . . ?
C27 C28 C29 120.4(3) . . ?
H28 C28 C29 119.8(2) . . ?
H28 C28 C27 119.80(19) . . ?
C42 C41 C40 120.8(3) . . ?
H41 C41 C40 119.6(2) . . ?
H41 C41 C42 119.6(2) . . ?
C15 C14 C1 109.6(4) . . ?
C17 C14 C1 115.5(5) . . ?
C17 C14 C15 117.2(7) . . ?
C16 C14 C1 106.3(4) . . ?
C16 C14 C15 98.4(5) . . ?
C16 C14 C17 107.8(7) . . ?
C0AA C14 C1 108.3(4) . . ?
C0AA C14 C15 83.1(6) . . ?
C0AA C14 C17 43.0(6) . . ?
C0AA C14 C16 142.5(5) . . ?
C1AA C14 C1 115.9(7) . . ?
C1AA C14 C15 30.9(7) . . ?
C1AA C14 C17 127.3(8) . . ?
C1AA C14 C16 67.5(8) . . ?
C1AA C14 C0AA 108.4(8) . . ?
C2AA C14 C1 108.6(5) . . ?
C2AA C14 C15 137.4(6) . . ?
C2AA C14 C17 59.4(7) . . ?
C2AA C14 C16 52.5(6) . . ?
C2AA C14 C0AA 102.2(7) . . ?
C2AA C14 C1AA 112.5(9) . . ?
C49 C50 C51 120.1(3) . . ?
H50 C50 C51 120.0(2) . . ?
H50 C50 C49 120.0(2) . . ?
C50 C49 C48 120.2(3) . . ?
H49 C49 C48 119.9(2) . . ?
H49 C49 C50 119.9(2) . . ?
H19a C19 C7 109.5 . . ?
H19b C19 C7 109.5 . . ?
H19b C19 H19a 109.5 . . ?
H19c C19 C7 109.5 . . ?
H19c C19 H19a 109.5 . . ?
H19c C19 H19b 109.5 . . ?
H18a C18 C7 109.5 . . ?
H18b C18 C7 109.5 . . ?
H18b C18 H18a 109.5 . . ?
H18c C18 C7 109.5 . . ?
H18c C18 H18a 109.5 . . ?
H18c C18 H18b 109.5 . . ?
H15a C15 C14 109.5 . . ?
H15b C15 C14 109.5 . . ?
H15b C15 H15a 109.5 . . ?
H15c C15 C14 109.5 . . ?
H15c C15 H15a 109.5 . . ?
H15c C15 H15b 109.5 . . ?
H22a C22 C20 109.5 . . ?
H22b C22 C20 109.5 . . ?
H22b C22 H22a 109.5 . . ?
H22c C22 C20 109.5 . . ?
H22c C22 H22a 109.5 . . ?
H22c C22 H22b 109.5 . . ?
H17a C17 C14 109.5 . . ?
H17b C17 C14 109.5 . . ?
H17b C17 H17a 109.5 . . ?
H17c C17 C14 109.5 . . ?
H17c C17 H17a 109.5 . . ?
H17c C17 H17b 109.5 . . ?
H16a C16 C14 109.5 . . ?
H16b C16 C14 109.5 . . ?
H16b C16 H16a 109.5 . . ?
H16c C16 C14 109.5 . . ?
H16c C16 H16a 109.5 . . ?
H16c C16 H16b 109.5 . . ?
H23a C23 C20 109.5 . . ?
H23b C23 C20 109.5 . . ?
H23b C23 H23a 109.5 . . ?
H23c C23 C20 109.5 . . ?
H23c C23 H23a 109.5 . . ?
H23c C23 H23b 109.5 . . ?
C4A O2 C9A 119.44(18) . . ?
C39A C38A C10A 119.6(2) . . ?
C47A C38A C10A 119.9(2) . . ?
C47A C38A C39A 120.5(2) . . ?
C9A C10A C38A 120.3(2) . . ?
C11A C10A C38A 121.5(2) . . ?
C11A C10A C9A 118.2(2) . . ?
C10A C9A O2 114.46(19) . . ?
C8A C9A O2 123.3(2) . . ?
C8A C9A C10A 122.2(2) . . ?
C12A C11A C10A 122.0(2) . . ?
H11A C11A C10A 119.01(14) . . ?
H11A C11A C12A 119.01(14) . . ?
C13A C8A C9A 117.1(2) . . ?
C7A C8A C9A 121.4(2) . . ?
C7A C8A C13A 121.4(2) . . ?
C44A C39A C38A 119.2(2) . . ?
C40A C39A C38A 122.9(2) . . ?
C40A C39A C44A 117.9(2) . . ?
C3A C4A O2 123.0(2) . . ?
C5A C4A O2 114.2(2) . . ?
C5A C4A C3A 122.9(2) . . ?
C7A C3A C4A 121.9(2) . . ?
C2A C3A C4A 116.7(2) . . ?
C2A C3A C7A 121.3(2) . . ?
C46A C47A C38A 119.6(2) . . ?
C48A C47A C38A 122.9(2) . . ?
C48A C47A C46A 117.4(2) . . ?
C13A C12A C11A 117.2(2) . . ?
C20A C12A C11A 121.3(2) . . ?
C20A C12A C13A 121.5(2) . . ?
C12A C13A C8A 123.3(2) . . ?
H13A C13A C8A 118.37(14) . . ?
H13A C13A C12A 118.37(13) . . ?
C45A C46A C47A 119.0(2) . . ?
C51A C46A C47A 118.8(2) . . ?
C51A C46A C45A 122.2(2) . . ?
C45A C44A C39A 119.5(2) . . ?
C43A C44A C39A 118.5(3) . . ?
C43A C44A C45A 122.0(2) . . ?
C24A C5A C4A 118.2(2) . . ?
C6A C5A C4A 117.8(2) . . ?
C6A C5A C24A 123.9(2) . . ?
C25A C24A C5A 120.3(2) . . ?
C33A C24A C5A 118.5(2) . . ?
C33A C24A C25A 121.0(3) . . ?
C44A C45A C46A 122.1(2) . . ?
H45A C45A C46A 118.94(15) . . ?
H45A C45A C44A 118.94(15) . . ?
C3A C7A C8A 110.3(2) . . ?
C18A C7A C8A 110.0(2) . . ?
C18A C7A C3A 110.9(2) . . ?
C19A C7A C8A 108.2(2) . . ?
C19A C7A C3A 107.9(2) . . ?
C19A C7A C18A 109.6(3) . . ?
C41A C40A C39A 121.3(3) . . ?
H40A C40A C39A 119.34(14) . . ?
H40A C40A C41A 119.34(18) . . ?
C30A C25A C24A 118.8(3) . . ?
C26A C25A C24A 122.9(3) . . ?
C26A C25A C30A 118.3(3) . . ?
C22A C20A C12A 110.2(3) . . ?
C21A C20A C12A 109.2(3) . . ?
C21A C20A C22A 107.5(5) . . ?
C23A C20A C12A 113.9(3) . . ?
C23A C20A C22A 108.2(5) . . ?
C23A C20A C21A 107.7(5) . . ?
C21B C20A C12A 113.7(4) . . ?
C21B C20A C22A 51.6(5) . . ?
C21B C20A C21A 57.5(6) . . ?
C21B C20A C23A 132.4(5) . . ?
C23B C20A C12A 108.9(4) . . ?
C23B C20A C22A 140.4(5) . . ?
C23B C20A C21A 52.5(6) . . ?
C23B C20A C23A 59.8(6) . . ?
C23B C20A C21B 106.0(7) . . ?
C22B C20A C12A 107.7(5) . . ?
C22B C20A C22A 63.5(7) . . ?
C22B C20A C21A 142.7(6) . . ?
C22B C20A C23A 50.8(6) . . ?
C22B C20A C21B 110.9(7) . . ?
C22B C20A C23B 109.6(8) . . ?
C49A C48A C47A 121.4(3) . . ?
H48A C48A C47A 119.31(15) . . ?
H48A C48A C49A 119.31(18) . . ?
C2A C1A C6A 117.6(2) . . ?
C14A C1A C6A 120.1(2) . . ?
C14A C1A C2A 122.3(3) . . ?
C1A C6A C5A 122.1(2) . . ?
H6A C6A C5A 118.96(15) . . ?
H6A C6A C1A 118.96(15) . . ?
C32A C33A C24A 119.7(3) . . ?
C34A C33A C24A 122.8(3) . . ?
C34A C33A C32A 117.4(3) . . ?
C1A C2A C3A 122.9(2) . . ?
H2A C2A C3A 118.56(15) . . ?
H2A C2A C1A 118.56(16) . . ?
C50A C51A C46A 121.2(3) . . ?
H51A C51A C46A 119.39(17) . . ?
H51A C51A C50A 119.39(18) . . ?
C42A C43A C44A 121.7(3) . . ?
H43A C43A C44A 119.14(17) . . ?
H43A C43A C42A 119.14(17) . . ?
C31A C30A C25A 119.0(3) . . ?
C29A C30A C25A 118.2(4) . . ?
C29A C30A C31A 122.7(3) . . ?
C50A C49A C48A 120.5(3) . . ?
H49A C49A C48A 119.76(18) . . ?
H49A C49A C50A 119.76(18) . . ?
C31A C32A C33A 118.8(3) . . ?
C37A C32A C33A 118.4(3) . . ?
C37A C32A C31A 122.9(3) . . ?
C42A C41A C40A 120.6(3) . . ?
H41A C41A C40A 119.68(18) . . ?
H41A C41A C42A 119.68(18) . . ?
C41A C42A C43A 120.0(3) . . ?
H42A C42A C43A 120.02(17) . . ?
H42A C42A C41A 120.02(18) . . ?
C27A C26A C25A 120.9(3) . . ?
H26A C26A C25A 119.57(17) . . ?
H26A C26A C27A 119.6(2) . . ?
C16A C14A C1A 111.2(3) . . ?
C15A C14A C1A 111.9(3) . . ?
C15A C14A C16A 107.8(3) . . ?
C17A C14A C1A 107.8(3) . . ?
C17A C14A C16A 110.2(4) . . ?
C17A C14A C15A 107.8(4) . . ?
C49A C50A C51A 120.7(3) . . ?
H50A C50A C51A 119.67(18) . . ?
H50A C50A C49A 119.67(18) . . ?
C35A C34A C33A 121.8(4) . . ?
H34A C34A C33A 119.08(18) . . ?
H34A C34A C35A 119.1(3) . . ?
C32A C31A C30A 122.6(3) . . ?
H31A C31A C30A 118.7(2) . . ?
H31A C31A C32A 118.7(2) . . ?
H18d C18A C7A 109.5 . . ?
H18e C18A C7A 109.5 . . ?
H18e C18A H18d 109.5 . . ?
H18f C18A C7A 109.5 . . ?
H18f C18A H18d 109.5 . . ?
H18f C18A H18e 109.5 . . ?
C36A C37A C32A 121.4(4) . . ?
H37A C37A C32A 119.3(2) . . ?
H37A C37A C36A 119.3(3) . . ?
H19d C19A C7A 109.5 . . ?
H19e C19A C7A 109.5 . . ?
H19e C19A H19d 109.5 . . ?
H19f C19A C7A 109.5 . . ?
H19f C19A H19d 109.5 . . ?
H19f C19A H19e 109.5 . . ?
C36A C35A C34A 120.7(4) . . ?
H35A C35A C34A 119.7(3) . . ?
H35A C35A C36A 119.7(3) . . ?
C28A C29A C30A 121.8(4) . . ?
H29A C29A C30A 119.1(3) . . ?
H29A C29A C28A 119.1(2) . . ?
H16d C16A C14A 109.5 . . ?
H16e C16A C14A 109.5 . . ?
H16e C16A H16d 109.5 . . ?
H16f C16A C14A 109.5 . . ?
H16f C16A H16d 109.5 . . ?
H16f C16A H16e 109.5 . . ?
C28A C27A C26A 120.0(4) . . ?
H27A C27A C26A 120.0(2) . . ?
H27A C27A C28A 120.0(2) . . ?
C27A C28A C29A 120.7(4) . . ?
H28A C28A C29A 119.6(2) . . ?
H28A C28A C27A 119.6(2) . . ?
H15d C15A C14A 109.5 . . ?
H15e C15A C14A 109.5 . . ?
H15e C15A H15d 109.5 . . ?
H15f C15A C14A 109.5 . . ?
H15f C15A H15d 109.5 . . ?
H15f C15A H15e 109.5 . . ?
H17d C17A C14A 109.5 . . ?
H17e C17A C14A 109.5 . . ?
H17e C17A H17d 109.5 . . ?
H17f C17A C14A 109.5 . . ?
H17f C17A H17d 109.5 . . ?
H17f C17A H17e 109.5 . . ?
C35A C36A C37A 120.3(4) . . ?
H36A C36A C37A 119.9(3) . . ?
H36A C36A C35A 119.9(3) . . ?
H22d C22A C20A 109.5 . . ?
H22e C22A C20A 109.5 . . ?
H22e C22A H22d 109.5 . . ?
H22f C22A C20A 109.5 . . ?
H22f C22A H22d 109.5 . . ?
H22f C22A H22e 109.5 . . ?
H21d C21A C20A 109.5 . . ?
H21e C21A C20A 109.5 . . ?
H21e C21A H21d 109.5 . . ?
H21f C21A C20A 109.5 . . ?
H21f C21A H21d 109.5 . . ?
H21f C21A H21e 109.5 . . ?
H23d C23A C20A 109.5 . . ?
H23e C23A C20A 109.5 . . ?
H23e C23A H23d 109.5 . . ?
H23f C23A C20A 109.5 . . ?
H23f C23A H23d 109.5 . . ?
H23f C23A H23e 109.5 . . ?
H21g C21B C20A 109.5 . . ?
H21h C21B C20A 109.5 . . ?
H21h C21B H21g 109.5 . . ?
H21i C21B C20A 109.5 . . ?
H21i C21B H21g 109.5 . . ?
H21i C21B H21h 109.5 . . ?
H23g C23B C20A 109.5 . . ?
H23h C23B C20A 109.5 . . ?
H23h C23B H23g 109.5 . . ?
H23i C23B C20A 109.5 . . ?
H23i C23B H23g 109.5 . . ?
H23i C23B H23h 109.5 . . ?
H22g C22B C20A 109.5 . . ?
H22h C22B C20A 109.5 . . ?
H22h C22B H22g 109.5 . . ?
H22i C22B C20A 109.5 . . ?
H22i C22B H22g 109.5 . . ?
H22i C22B H22h 109.5 . . ?
H0Aa C0AA C14 109.5 . . ?
H0Ab C0AA C14 109.5 . . ?
H0Ab C0AA H0Aa 109.5 . . ?
H0Ac C0AA C14 109.5 . . ?
H0Ac C0AA H0Aa 109.5 . . ?
H0Ac C0AA H0Ab 109.5 . . ?
H1Aa C1AA C14 109.5 . . ?
H1Ab C1AA C14 109.5 . . ?
H1Ab C1AA H1Aa 109.5 . . ?
H1Ac C1AA C14 109.5 . . ?
H1Ac C1AA H1Aa 109.5 . . ?
H1Ac C1AA H1Ab 109.5 . . ?
H2Aa C2AA C14 109.5 . . ?
H2Ab C2AA C14 109.5 . . ?
H2Ab C2AA H2Aa 109.5 . . ?
H2Ac C2AA C14 109.5 . . ?
H2Ac C2AA H2Aa 109.5 . . ?
H2Ac C2AA H2Ab 109.5 . . ?
H3Aa C3AA C20 109.5 . . ?
H3Ab C3AA C20 109.5 . . ?
H3Ab C3AA H3Aa 109.5 . . ?
H3Ac C3AA C20 109.5 . . ?
H3Ac C3AA H3Aa 109.5 . . ?
H3Ac C3AA H3Ab 109.5 . . ?
H4Aa C4AA C20 109.5 . . ?
H4Ab C4AA C20 109.5 . . ?
H4Ab C4AA H4Aa 109.5 . . ?
H4Ac C4AA C20 109.5 . . ?
H4Ac C4AA H4Aa 109.5 . . ?
H4Ac C4AA H4Ab 109.5 . . ?
H5Aa C5AA C20 109.5 . . ?
H5Ab C5AA C20 109.5 . . ?
H5Ab C5AA H5Aa 109.5 . . ?
H5Ac C5AA C20 109.5 . . ?
H5Ac C5AA H5Aa 109.5 . . ?
H5Ac C5AA H5Ab 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 C4 C5 C24 1.2(3) . . . . ?
O1 C4 C5 C6 -179.7(2) . . . . ?
O1 C4 C3 C7 -0.7(3) . . . . ?
O1 C4 C3 C2 179.5(3) . . . . ?
O1 C9 C8 C13 -179.1(2) . . . . ?
O1 C9 C8 C7 0.2(3) . . . . ?
O1 C9 C10 C38 -2.6(3) . . . . ?
O1 C9 C10 C11 179.1(2) . . . . ?
C21 C20 C12 C13 0.8(5) . . . . ?
C21 C20 C12 C11 -178.3(4) . . . . ?
C24 C33 C32 C31 -1.8(3) . . . . ?
C24 C33 C32 C37 178.7(2) . . . . ?
C24 C33 C34 C35 -179.3(3) . . . . ?
C24 C25 C30 C31 -3.0(3) . . . . ?
C24 C25 C30 C29 177.7(3) . . . . ?
C24 C25 C26 C27 -179.8(3) . . . . ?
C24 C5 C4 C3 -179.1(2) . . . . ?
C24 C5 C6 C1 179.4(3) . . . . ?
C4 C5 C6 C1 0.2(3) . . . . ?
C4 C3 C7 C8 -1.8(3) . . . . ?
C4 C3 C7 C19 118.1(3) . . . . ?
C4 C3 C7 C18 -122.0(3) . . . . ?
C4 C3 C2 C1 0.1(3) . . . . ?
C33 C32 C31 C30 2.0(3) . . . . ?
C33 C32 C37 C36 1.1(3) . . . . ?
C33 C34 C35 C36 0.1(3) . . . . ?
C9 C8 C13 C12 0.2(3) . . . . ?
C9 C8 C7 C3 2.0(3) . . . . ?
C9 C8 C7 C19 -118.6(3) . . . . ?
C9 C8 C7 C18 121.3(3) . . . . ?
C9 C10 C38 C47 70.1(3) . . . . ?
C9 C10 C38 C39 -108.1(2) . . . . ?
C9 C10 C11 C12 -0.0(3) . . . . ?
C8 C13 C12 C11 -0.7(3) . . . . ?
C8 C13 C12 C20 -179.9(3) . . . . ?
C8 C7 C3 C2 178.0(2) . . . . ?
C10 C38 C47 C46 -177.0(2) . . . . ?
C10 C38 C47 C48 2.7(3) . . . . ?
C10 C38 C39 C44 176.6(2) . . . . ?
C10 C38 C39 C40 -2.1(3) . . . . ?
C10 C11 C12 C13 0.6(3) . . . . ?
C10 C11 C12 C20 179.8(3) . . . . ?
C47 C38 C39 C44 -1.6(3) . . . . ?
C47 C38 C39 C40 179.8(2) . . . . ?
C47 C46 C45 C44 -1.3(3) . . . . ?
C47 C46 C51 C50 0.5(3) . . . . ?
C47 C48 C49 C50 0.6(4) . . . . ?
C38 C39 C44 C45 0.6(3) . . . . ?
C38 C39 C44 C43 -179.4(2) . . . . ?
C38 C39 C40 C41 179.7(3) . . . . ?
C25 C30 C31 C32 0.3(3) . . . . ?
C25 C30 C29 C28 2.6(3) . . . . ?
C25 C26 C27 C28 1.5(3) . . . . ?
C5 C6 C1 C2 -0.3(3) . . . . ?
C5 C6 C1 C14 179.2(3) . . . . ?
C39 C44 C45 C46 0.9(3) . . . . ?
C39 C44 C43 C42 -0.5(3) . . . . ?
C39 C40 C41 C42 -0.3(4) . . . . ?
C3 C2 C1 C6 0.2(3) . . . . ?
C3 C2 C1 C14 -179.4(3) . . . . ?
C32 C31 C30 C29 179.6(3) . . . . ?
C32 C37 C36 C35 -1.2(3) . . . . ?
C44 C45 C46 C51 178.8(3) . . . . ?
C44 C43 C42 C41 1.3(4) . . . . ?
C30 C29 C28 C27 0.9(4) . . . . ?
C34 C35 C36 C37 0.6(4) . . . . ?
C13 C12 C20 C22 -120.8(4) . . . . ?
C13 C12 C20 C23 120.5(4) . . . . ?
C13 C12 C20 C3AA -175.7(8) . . . . ?
C13 C12 C20 C4AA -54.5(8) . . . . ?
C13 C12 C20 C5AA 64.5(7) . . . . ?
C46 C51 C50 C49 -0.9(4) . . . . ?
C6 C1 C14 C15 132.7(5) . . . . ?
C6 C1 C14 C17 -2.3(8) . . . . ?
C6 C1 C14 C16 -121.8(5) . . . . ?
C6 C1 C14 C0AA 43.6(5) . . . . ?
C6 C1 C14 C1AA 165.6(10) . . . . ?
C6 C1 C14 C2AA -66.6(7) . . . . ?
C2 C1 C14 C15 -47.8(5) . . . . ?
C2 C1 C14 C17 177.2(8) . . . . ?
C2 C1 C14 C16 57.7(5) . . . . ?
C2 C1 C14 C0AA -136.9(5) . . . . ?
C2 C1 C14 C1AA -14.9(9) . . . . ?
C2 C1 C14 C2AA 112.9(7) . . . . ?
C40 C41 C42 C43 -0.9(4) . . . . ?
C26 C27 C28 C29 -3.0(4) . . . . ?
C48 C49 C50 C51 0.4(4) . . . . ?
O2 C9A C10A C38A -0.7(3) . . . . ?
O2 C9A C10A C11A -179.7(2) . . . . ?
O2 C9A C8A C13A 179.6(2) . . . . ?
O2 C9A C8A C7A -2.6(3) . . . . ?
O2 C4A C3A C7A 2.3(3) . . . . ?
O2 C4A C3A C2A 180.0(3) . . . . ?
O2 C4A C5A C24A -0.8(3) . . . . ?
O2 C4A C5A C6A -179.8(2) . . . . ?
C38A C10A C9A C8A 179.3(2) . . . . ?
C38A C10A C11A C12A -179.1(2) . . . . ?
C38A C39A C44A C45A -0.7(3) . . . . ?
C38A C39A C44A C43A 179.0(2) . . . . ?
C38A C39A C40A C41A -179.0(3) . . . . ?
C38A C47A C46A C45A 2.3(3) . . . . ?
C38A C47A C46A C51A -178.1(2) . . . . ?
C38A C47A C48A C49A 178.8(3) . . . . ?
C10A C9A C8A C13A -0.4(3) . . . . ?
C10A C9A C8A C7A 177.4(2) . . . . ?
C10A C11A C12A C13A 0.0(3) . . . . ?
C10A C11A C12A C20A 179.8(2) . . . . ?
C9A C8A C13A C12A 0.3(3) . . . . ?
C9A C8A C7A C3A 7.9(3) . . . . ?
C9A C8A C7A C18A 130.6(3) . . . . ?
C9A C8A C7A C19A -109.8(3) . . . . ?
C11A C12A C13A C8A -0.1(3) . . . . ?
C11A C12A C20A C22A 122.1(5) . . . . ?
C11A C12A C20A C21A -120.0(5) . . . . ?
C11A C12A C20A C23A 0.3(5) . . . . ?
C11A C12A C20A C21B 177.9(7) . . . . ?
C11A C12A C20A C23B -64.2(6) . . . . ?
C11A C12A C20A C22B 54.6(7) . . . . ?
C8A C13A C12A C20A -179.9(2) . . . . ?
C8A C7A C3A C4A -7.8(3) . . . . ?
C8A C7A C3A C2A 174.6(2) . . . . ?
C39A C44A C45A C46A -0.5(3) . . . . ?
C39A C44A C43A C42A 0.0(3) . . . . ?
C39A C40A C41A C42A -0.0(3) . . . . ?
C4A C3A C7A C18A -129.9(3) . . . . ?
C4A C3A C7A C19A 110.1(3) . . . . ?
C4A C3A C2A C1A -0.4(3) . . . . ?
C4A C5A C24A C25A 108.1(3) . . . . ?
C4A C5A C24A C33A -66.9(3) . . . . ?
C4A C5A C6A C1A -0.1(3) . . . . ?
C3A C2A C1A C6A -0.3(3) . . . . ?
C3A C2A C1A C14A 177.0(3) . . . . ?
C47A C46A C45A C44A -0.3(3) . . . . ?
C47A C46A C51A C50A -0.9(3) . . . . ?
C47A C48A C49A C50A -0.7(3) . . . . ?
C46A C45A C44A C43A 179.8(3) . . . . ?
C46A C51A C50A C49A -0.5(4) . . . . ?
C44A C43A C42A C41A -0.5(4) . . . . ?
C5A C24A C25A C30A -173.9(2) . . . . ?
C5A C24A C25A C26A 4.5(3) . . . . ?
C5A C24A C33A C32A 171.5(2) . . . . ?
C5A C24A C33A C34A -6.0(3) . . . . ?
C5A C6A C1A C2A 0.6(3) . . . . ?
C5A C6A C1A C14A -176.8(3) . . . . ?
C24A C25A C30A C31A 1.9(3) . . . . ?
C24A C25A C30A C29A -179.0(3) . . . . ?
C24A C25A C26A C27A 179.3(3) . . . . ?
C24A C33A C32A C31A 3.1(3) . . . . ?
C24A C33A C32A C37A -177.3(3) . . . . ?
C24A C33A C34A C35A 176.8(3) . . . . ?
C40A C41A C42A C43A 0.5(4) . . . . ?
C25A C30A C31A C32A -2.3(3) . . . . ?
C25A C30A C29A C28A -0.7(3) . . . . ?
C25A C26A C27A C28A 0.2(4) . . . . ?
C48A C49A C50A C51A 1.3(4) . . . . ?
C33A C32A C31A C30A -0.2(3) . . . . ?
C33A C32A C37A C36A 0.7(4) . . . . ?
C33A C34A C35A C36A 0.1(4) . . . . ?
C30A C31A C32A C37A -179.9(3) . . . . ?
C30A C29A C28A C27A -1.4(4) . . . . ?
C32A C37A C36A C35A -1.4(4) . . . . ?
C26A C27A C28A C29A 1.7(4) . . . . ?
C34A C35A C36A C37A 1.0(4) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_id
C21 C20 1 7
C20 C22 1 8
C20 C23 1 9
C20 C3AA 1 9
C20 C4AA 1 8
C14 C15 1 4
C14 C17 1 5
C14 C16 1 6
C14 C0AA 1 4
C14 C1AA 1 6
C14 C2AA 1 5
C20A C22A 1 1
C20A C21A 1 2
C20A C23A 1 3
C20A C21B 1 2
C20A C23B 1 3
C20A C22B 1 1
C5AA C20 1 7

loop_
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
_restr_equal_distance_class_average
_restr_equal_distance_class_esd
_restr_equal_distance_class_diff_max
1 0.0200 1.5208 0.0087 0.0087
2 0.0200 1.5233 0.0150 0.0150
3 0.0200 1.5114 0.0073 0.0073
4 0.0200 1.6010 0.0213 0.0213
5 0.0200 1.4678 0.0440 0.0440
6 0.0200 1.5138 0.0853 0.0853
7 0.0200 1.5288 0.0055 0.0055
8 0.0200 1.5207 0.0118 0.0118
9 0.0200 1.5201 0.0048 0.0048

loop_
_restr_U_iso_atom_site_label
_restr_U_iso_weight_param
C21 0.0100
C15 0.0100
C22 0.0100
C17 0.0100
C16 0.0100
C23 0.0100
C21A 0.0100
C21B 0.0100
C23B 0.0100
C22B 0.0100
C0AA 0.0100
C1AA 0.0100
C2AA 0.0100
C3AA 0.0100
C4AA 0.0100
C5AA 0.0100

####################################################################### 
# 
# 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_20220506-lqy348k
_database_code_depnum_ccdc_archive 'CCDC 2180374'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2022-06-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2022-05-31
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H4 Cl2, C51 H46 O'
_chemical_formula_sum            'C53 H50 Cl2 O'
_chemical_formula_weight         773.83
_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'
Cl Cl 0.3639 0.7018 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.86643(19)
_cell_length_b                   13.09253(19)
_cell_length_c                   15.2541(2)
_cell_angle_alpha                94.3619(12)
_cell_angle_beta                 114.0071(15)
_cell_angle_gamma                108.5552(13)
_cell_volume                     2161.74(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15053
_cell_measurement_temperature    348.00(10)
_cell_measurement_theta_max      66.5420
_cell_measurement_theta_min      3.2420
_shelx_estimated_absorpt_T_max   0.854
_shelx_estimated_absorpt_T_min   0.792
_exptl_absorpt_coefficient_mu    1.627
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25665
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.593
_diffrn_reflns_theta_max         66.593
_diffrn_reflns_theta_min         3.265
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      348.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     52.00 106.00   0.50    0.30    --   62.89  15.00   0.00  108
  2  ω     34.00  69.00   0.50    0.30    --   72.93-125.00 150.00   70
  3  ω     45.00  98.00   0.50    0.30    --   76.75-125.00  30.00  106
  4  ω     55.00  98.00   0.50    0.30    --   76.75-125.00 -90.00   86
  5  ω     42.00  98.00   0.50    0.30    --   76.75-125.00-180.00  112
  6  ω    -89.00 -53.00   0.50    0.30    --  -63.41 -15.00-180.00   72
  7  ω   -109.00 -63.00   0.50    0.30    --  -71.74 -15.00-180.00   92
  8  ω   -107.00 -63.00   0.50    0.30    --  -71.74 -15.00-120.00   88
  9  ω   -103.00 -64.00   0.50    0.30    --  -71.74 -15.00 -90.00   78
 10  ω   -120.00 -66.00   0.50    0.30    --  -76.23 -15.00 -30.00  108
 11  ω   -120.00 -85.00   0.50    0.30    --  -76.23 -15.00  30.00   70
 12  ω    -97.00 -62.00   0.50    0.30    --  -71.74 -15.00  30.00   70
 13  ω   -123.00 -77.00   0.50    0.30    --  -81.49 -15.00  90.00   92
 14  ω   -120.00 -79.00   0.50    0.30    --  -76.23 -15.00 120.00   82
 15  ω   -125.00 -83.00   0.50    0.30    --  -81.49 -15.00 -30.00   84
 16  ω   -121.00 -84.00   0.50    0.30    --  -81.49 -15.00-120.00   74
 17  ω   -122.00 -87.00   0.50    0.30    --  -81.49 -15.00-180.00   70
 18  ω   -102.00 -76.00   0.50    0.30    --  -81.49 125.00-180.00   52
 19  ω    -82.00 -43.00   0.50    0.30    --  -76.23 125.00-120.00   78
 20  ω    -68.00 -28.00   0.50    0.30    --  -63.41 125.00   0.00   80
 21  ω    -72.00 -42.00   0.50    0.30    --  -76.23 125.00 -30.00   60
 22  ω    -97.00 -50.00   0.50    0.30    --  -76.23 125.00  30.00   94
 23  ω    -73.00 -34.00   0.50    0.30    --  -76.23 125.00  60.00   78
 24  ω   -102.00 -69.00   0.50    0.30    --  -81.49 125.00  30.00   66
 25  ω    -66.00 -23.00   0.50    0.30    --  -63.41 125.00 120.00   86
 26  ω    -74.00 -29.00   0.50    0.30    --  -71.74 125.00 150.00   90
 27  ω   -102.00 -56.00   0.50    0.30    --  -81.49 125.00 120.00   92
 28  ω   -101.00 -75.00   0.50    0.30    --  -81.49 125.00  90.00   52
 29  ω   -102.00 -73.00   0.50    0.30    --  -81.49 125.00 150.00   58
 30  ω   -102.00 -58.00   0.50    0.30    --  -81.49 125.00   0.00   88
 31  ω   -101.00 -72.00   0.50    0.30    --  -81.49 125.00  60.00   58
 32  ω    -64.00 -39.00   0.50    0.30    --  -81.49 125.00 -60.00   50
 33  ω   -102.00 -71.00   0.50    0.30    --  -81.49 125.00 -60.00   62
 34  ω   -102.00 -51.00   0.50    0.30    --  -81.49 125.00 -90.00  102
 35  ω   -102.00 -77.00   0.50    0.30    --  -81.49 125.00-120.00   50
 36  ω   -102.00 -43.00   0.50    0.30    --  -81.49 125.00-150.00  118
 37  ω    -64.00 -39.00   0.50    0.30    --  -81.49 125.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0626925000
_diffrn_orient_matrix_UB_12      0.0605955000
_diffrn_orient_matrix_UB_13      -0.0587770000
_diffrn_orient_matrix_UB_21      0.0779455000
_diffrn_orient_matrix_UB_22      -0.0716045000
_diffrn_orient_matrix_UB_23      0.0180866000
_diffrn_orient_matrix_UB_31      -0.1006672000
_diffrn_orient_matrix_UB_32      -0.0867527000
_diffrn_orient_matrix_UB_33      -0.0957624000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6315
_reflns_number_total             7582
_reflns_odcompleteness_completeness 98.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7582
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0664
_refine_ls_restrained_S_all      1.111
_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)+(0.1180P)²+0.4225P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2045
_refine_ls_wR_factor_ref         0.2123
_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. Restrained distances
 C52-C53
 1.54 with sigma of 0.02
 C53-Cl2
 1.78 with sigma of 0.02
 C52-Cl1
 1.78 with sigma of 0.02
 C52A-Cl1A
 1.78 with sigma of 0.02
 C53A-Cl2A
 1.78 with sigma of 0.02
 C52A-C53A
 1.54 with sigma of 0.02
3. Rigid bond restraints
 C44, C46
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Others
 Sof(Cl2A)=Sof(C53A)=Sof(H53C)=Sof(H53D)=Sof(C52A)=Sof(H52C)=Sof(H52D)=
 Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C53)=Sof(H53A)=Sof(H53B)=
 FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C53(H53A,H53B), C53A(H53C,H53D), C52A(H52C,H52D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C5(H5), C10(H10), C20(H20), C39(H39), C34(H34), C15(H15),
 C36(H36), C25(H25), C29(H29), C18(H18), C38(H38), C37(H37), C32(H32), C17(H17),
  C22(H22), C16(H16), C24(H24), C31(H31), C30(H30), C23(H23)
5.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C47(H47A,H47B,H47C), C51(H51A,H51B,
 H51C), C49(H49A,H49B,H49C), C46(H46A,H46B,H46C), C45(H45A,H45B,H45C), C50(H50A,
 H50B,H50C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Cl1 Cl 0.0252(9) 0.1181(10) 0.6319(7) 0.273(5) Uani 0.469(11) 1 d D . P A 1
O1 O 0.73402(12) 0.49642(9) 0.75473(10) 0.0599(4) Uani 1 1 d . . . . .
Cl2 Cl -0.2389(8) -0.0290(7) 0.7222(8) 0.209(3) Uani 0.469(11) 1 d D . P A 1
C2 C 0.81808(16) 0.68454(13) 0.83199(14) 0.0529(4) Uani 1 1 d . . . . .
C12 C 0.65268(16) 0.38942(13) 0.73405(13) 0.0493(4) Uani 1 1 d . . . . .
C6 C 0.64928(16) 0.56021(13) 0.85393(13) 0.0487(4) Uani 1 1 d . . . . .
C11 C 0.66189(16) 0.31120(13) 0.67329(13) 0.0517(4) Uani 1 1 d . . . . .
C7 C 0.56704(16) 0.35985(13) 0.77001(13) 0.0481(4) Uani 1 1 d . . . . .
C1 C 0.73154(16) 0.57913(13) 0.81402(13) 0.0500(4) Uani 1 1 d . . . . .
C3 C 0.82078(17) 0.77215(14) 0.89152(14) 0.0569(5) Uani 1 1 d . . . . .
H3 H 0.878687 0.842774 0.904143 0.068 Uiso 1 1 calc R U . . .
C8 C 0.49066(16) 0.24835(13) 0.74428(13) 0.0522(4) Uani 1 1 d . . . . .
H8 H 0.433226 0.227313 0.768427 0.063 Uiso 1 1 calc R U . . .
C9 C 0.49610(17) 0.16702(13) 0.68430(14) 0.0537(4) Uani 1 1 d . . . . .
C27 C 0.75429(17) 0.34384(13) 0.63417(14) 0.0525(4) Uani 1 1 d . . . . .
C28 C 0.88084(18) 0.37403(15) 0.69843(15) 0.0588(5) Uani 1 1 d . . . . .
C13 C 0.90837(17) 0.70552(13) 0.79054(14) 0.0537(4) Uani 1 1 d . . . . .
C5 C 0.65609(16) 0.65097(13) 0.91267(13) 0.0522(4) Uani 1 1 d . . . . .
H5 H 0.601601 0.639409 0.939854 0.063 Uiso 1 1 calc R U . . .
C4 C 0.74039(17) 0.75840(13) 0.93292(14) 0.0540(4) Uani 1 1 d . . . . .
C41 C 0.55568(15) 0.44467(13) 0.83658(13) 0.0493(4) Uani 1 1 d . . . . .
C14 C 1.03429(18) 0.73393(13) 0.85482(15) 0.0570(5) Uani 1 1 d . . . . .
C40 C 0.71368(18) 0.34021(13) 0.53286(14) 0.0551(4) Uani 1 1 d . . . . .
C26 C 0.86879(19) 0.70279(15) 0.68920(15) 0.0607(5) Uani 1 1 d . . . . .
C10 C 0.58339(17) 0.20111(14) 0.64983(14) 0.0558(4) Uani 1 1 d . . . . .
H10 H 0.589359 0.148378 0.609713 0.067 Uiso 1 1 calc R U . . .
C42 C 0.42567(18) 0.44397(16) 0.78873(17) 0.0675(5) Uani 1 1 d . . . . .
H42A H 0.367252 0.371164 0.778173 0.101 Uiso 1 1 calc R U . . .
H42B H 0.409159 0.463816 0.726527 0.101 Uiso 1 1 calc R U . . .
H42C H 0.418761 0.496482 0.831374 0.101 Uiso 1 1 calc R U . . .
C19 C 1.12243(19) 0.76467(15) 0.81674(18) 0.0650(5) Uani 1 1 d . . . . .
C33 C 0.96755(19) 0.39840(17) 0.65882(17) 0.0664(5) Uani 1 1 d . . . . .
C35 C 0.8026(2) 0.36519(15) 0.49521(16) 0.0629(5) Uani 1 1 d . . . . .
C44 C 0.7418(2) 0.85433(15) 0.99814(16) 0.0646(5) Uani 1 1 d . U . . .
C21 C 0.9585(2) 0.73510(17) 0.65304(17) 0.0690(6) Uani 1 1 d . . . . .
C48 C 0.40985(19) 0.04540(14) 0.66001(16) 0.0643(5) Uani 1 1 d . . . . .
C20 C 1.0820(2) 0.76576(18) 0.71779(18) 0.0728(6) Uani 1 1 d . . . . .
H20 H 1.139725 0.787828 0.694022 0.087 Uiso 1 1 calc R U . . .
C39 C 0.5881(2) 0.31221(17) 0.46477(17) 0.0702(5) Uani 1 1 d . . . . .
H39 H 0.529116 0.296687 0.487533 0.084 Uiso 1 1 calc R U . . .
C43 C 0.5827(2) 0.41368(16) 0.93660(15) 0.0677(5) Uani 1 1 d . . . . .
H43A H 0.577994 0.467554 0.979662 0.101 Uiso 1 1 calc R U . . .
H43B H 0.663789 0.412393 0.965868 0.101 Uiso 1 1 calc R U . . .
H43C H 0.523157 0.341748 0.926700 0.101 Uiso 1 1 calc R U . . .
C34 C 0.9258(2) 0.39308(18) 0.55874(18) 0.0710(6) Uani 1 1 d . . . . .
H34 H 0.982324 0.408742 0.533464 0.085 Uiso 1 1 calc R U . . .
C15 C 1.0802(2) 0.73460(17) 0.95672(18) 0.0723(6) Uani 1 1 d . . . . .
H15 H 1.025144 0.714196 0.983172 0.087 Uiso 1 1 calc R U . . .
C36 C 0.7599(3) 0.35914(19) 0.39165(18) 0.0772(6) Uani 1 1 d . . . . .
H36 H 0.816584 0.375149 0.366520 0.093 Uiso 1 1 calc R U . . .
C25 C 0.7428(2) 0.6713(2) 0.61978(18) 0.0801(6) Uani 1 1 d . . . . .
H25 H 0.682420 0.649930 0.640922 0.096 Uiso 1 1 calc R U . . .
C29 C 0.9279(2) 0.3800(2) 0.80122(17) 0.0758(6) Uani 1 1 d . . . . .
H29 H 0.873705 0.364994 0.828795 0.091 Uiso 1 1 calc R U . . .
C18 C 1.2499(2) 0.7957(2) 0.8832(2) 0.0825(7) Uani 1 1 d . . . . .
H18 H 1.307615 0.816398 0.859308 0.099 Uiso 1 1 calc R U . . .
C38 C 0.5524(3) 0.3076(2) 0.36653(19) 0.0837(7) Uani 1 1 d . . . . .
H38 H 0.469760 0.289085 0.323337 0.100 Uiso 1 1 calc R U . . .
C37 C 0.6406(3) 0.3310(2) 0.33020(19) 0.0852(7) Uani 1 1 d . . . . .
H37 H 0.615368 0.326819 0.263129 0.102 Uiso 1 1 calc R U . . .
C32 C 1.0942(2) 0.4246(2) 0.7241(2) 0.0911(8) Uani 1 1 d . . . . .
H32 H 1.150905 0.439491 0.698974 0.109 Uiso 1 1 calc R U . . .
C17 C 1.2879(2) 0.7955(2) 0.9784(2) 0.0912(8) Uani 1 1 d . . . . .
H17 H 1.371433 0.816265 1.019991 0.109 Uiso 1 1 calc R U . . .
C22 C 0.9178(3) 0.7366(2) 0.5513(2) 0.0924(8) Uani 1 1 d . . . . .
H22 H 0.975648 0.759090 0.527645 0.111 Uiso 1 1 calc R U . . .
C16 C 1.2026(2) 0.7643(2) 1.0169(2) 0.0875(7) Uani 1 1 d . . . . .
H16 H 1.230042 0.763910 1.083427 0.105 Uiso 1 1 calc R U . . .
C47 C 0.8518(3) 0.9602(2) 1.0248(3) 0.1178(12) Uani 1 1 d . . . . .
H47A H 0.925751 0.945436 1.051418 0.177 Uiso 1 1 calc R U . . .
H47B H 0.855813 1.014626 1.073230 0.177 Uiso 1 1 calc R U . . .
H47C H 0.843713 0.987660 0.966783 0.177 Uiso 1 1 calc R U . . .
C51 C 0.4071(3) -0.0255(2) 0.5754(3) 0.1161(12) Uani 1 1 d . . . . .
H51A H 0.346596 -0.099038 0.558657 0.174 Uiso 1 1 calc R U . . .
H51B H 0.486664 -0.028852 0.594682 0.174 Uiso 1 1 calc R U . . .
H51C H 0.386287 0.006310 0.519055 0.174 Uiso 1 1 calc R U . . .
C24 C 0.7095(3) 0.6722(3) 0.5233(2) 0.1028(9) Uani 1 1 d . . . . .
H24 H 0.626533 0.649727 0.479149 0.123 Uiso 1 1 calc R U . . .
C49 C 0.2774(3) 0.0370(2) 0.6274(3) 0.1235(13) Uani 1 1 d . . . . .
H49A H 0.253060 0.070131 0.572318 0.185 Uiso 1 1 calc R U . . .
H49B H 0.272730 0.075112 0.681194 0.185 Uiso 1 1 calc R U . . .
H49C H 0.223284 -0.039646 0.608428 0.185 Uiso 1 1 calc R U . . .
C46 C 0.7534(3) 0.8248(2) 1.0967(2) 0.1119(11) Uani 1 1 d . U . . .
H46A H 0.684733 0.758330 1.084018 0.168 Uiso 1 1 calc R U . . .
H46B H 0.754031 0.884479 1.137827 0.168 Uiso 1 1 calc R U . . .
H46C H 0.828629 0.813238 1.129550 0.168 Uiso 1 1 calc R U . . .
C31 C 1.1333(3) 0.4284(3) 0.8200(2) 0.1097(10) Uani 1 1 d . . . . .
H31 H 1.216323 0.445175 0.860852 0.132 Uiso 1 1 calc R U . . .
C30 C 1.0486(3) 0.4069(3) 0.8601(2) 0.1008(9) Uani 1 1 d . . . . .
H30 H 1.076693 0.411362 0.927453 0.121 Uiso 1 1 calc R U . . .
C23 C 0.7983(3) 0.7064(3) 0.4890(2) 0.1077(10) Uani 1 1 d . . . . .
H23 H 0.773912 0.708012 0.422973 0.129 Uiso 1 1 calc R U . . .
C45 C 0.6224(3) 0.8695(3) 0.9486(3) 0.1401(16) Uani 1 1 d . . . . .
H45A H 0.614867 0.892123 0.888613 0.210 Uiso 1 1 calc R U . . .
H45B H 0.620577 0.925396 0.991879 0.210 Uiso 1 1 calc R U . . .
H45C H 0.555240 0.800785 0.933562 0.210 Uiso 1 1 calc R U . . .
C50 C 0.4487(4) 0.0010(2) 0.7503(3) 0.1441(16) Uani 1 1 d . . . . .
H50A H 0.396679 -0.075749 0.734782 0.216 Uiso 1 1 calc R U . . .
H50B H 0.441791 0.042163 0.801085 0.216 Uiso 1 1 calc R U . . .
H50C H 0.532663 0.008193 0.773011 0.216 Uiso 1 1 calc R U . . .
C52 C -0.0767(10) 0.1037(9) 0.6696(8) 0.105(3) Uani 0.469(11) 1 d D . P A 1
H52A H -0.040281 0.157853 0.731547 0.126 Uiso 0.469(11) 1 calc R U P A 1
H52B H -0.143266 0.120071 0.621941 0.126 Uiso 0.469(11) 1 calc R U P A 1
C53 C -0.1303(15) -0.0107(13) 0.6849(15) 0.143(5) Uani 0.469(11) 1 d D . P A 1
H53A H -0.063651 -0.026263 0.733261 0.172 Uiso 0.469(11) 1 calc R U P A 1
H53B H -0.164975 -0.064709 0.623163 0.172 Uiso 0.469(11) 1 calc R U P A 1
Cl2A Cl -0.2090(11) 0.0314(11) 0.7571(8) 0.245(4) Uani 0.531(11) 1 d D . P A 2
C53A C -0.1230(13) 0.0802(13) 0.7008(10) 0.188(7) Uani 0.531(11) 1 d D . P A 2
H53C H -0.173241 0.097930 0.641579 0.225 Uiso 0.531(11) 1 calc R U P A 2
H53D H -0.056352 0.149153 0.743990 0.225 Uiso 0.531(11) 1 calc R U P A 2
C52A C -0.0687(14) 0.0081(12) 0.6725(11) 0.210(11) Uani 0.531(11) 1 d D . P A 2
H52C H -0.132620 -0.058533 0.623404 0.252 Uiso 0.531(11) 1 calc R U P A 2
H52D H -0.019016 -0.013170 0.729617 0.252 Uiso 0.531(11) 1 calc R U P A 2
Cl1A Cl 0.0234(3) 0.0883(6) 0.6235(3) 0.176(2) Uani 0.531(11) 1 d D . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C52 1.600(11) . ?
O1 C12 1.3741(19) . ?
O1 C1 1.3741(19) . ?
Cl2 C53 1.670(15) . ?
C2 C1 1.391(2) . ?
C2 C3 1.390(2) . ?
C2 C13 1.499(2) . ?
C12 C11 1.394(2) . ?
C12 C7 1.385(2) . ?
C6 C1 1.390(2) . ?
C6 C5 1.389(2) . ?
C6 C41 1.526(2) . ?
C11 C27 1.498(2) . ?
C11 C10 1.388(2) . ?
C7 C8 1.392(2) . ?
C7 C41 1.529(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.390(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.388(2) . ?
C9 C10 1.391(2) . ?
C9 C48 1.535(2) . ?
C27 C28 1.415(3) . ?
C27 C40 1.407(3) . ?
C28 C33 1.436(3) . ?
C28 C29 1.418(3) . ?
C13 C14 1.412(3) . ?
C13 C26 1.411(3) . ?
C5 H5 0.9300 . ?
C5 C4 1.393(2) . ?
C4 C44 1.532(2) . ?
C41 C42 1.525(3) . ?
C41 C43 1.538(3) . ?
C14 C19 1.437(3) . ?
C14 C15 1.419(3) . ?
C40 C35 1.439(3) . ?
C40 C39 1.422(3) . ?
C26 C21 1.435(3) . ?
C26 C25 1.425(3) . ?
C10 H10 0.9300 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C19 C20 1.385(3) . ?
C19 C18 1.429(3) . ?
C33 C34 1.384(3) . ?
C33 C32 1.428(3) . ?
C35 C34 1.383(3) . ?
C35 C36 1.432(3) . ?
C44 C47 1.512(3) . ?
C44 C46 1.540(4) . ?
C44 C45 1.498(4) . ?
C21 C20 1.385(3) . ?
C21 C22 1.426(3) . ?
C48 C51 1.513(3) . ?
C48 C49 1.532(4) . ?
C48 C50 1.493(4) . ?
C20 H20 0.9300 . ?
C39 H39 0.9300 . ?
C39 C38 1.367(3) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C34 H34 0.9300 . ?
C15 H15 0.9300 . ?
C15 C16 1.362(3) . ?
C36 H36 0.9300 . ?
C36 C37 1.337(4) . ?
C25 H25 0.9300 . ?
C25 C24 1.357(4) . ?
C29 H29 0.9300 . ?
C29 C30 1.347(4) . ?
C18 H18 0.9300 . ?
C18 C17 1.332(4) . ?
C38 H38 0.9300 . ?
C38 C37 1.416(4) . ?
C37 H37 0.9300 . ?
C32 H32 0.9300 . ?
C32 C31 1.330(4) . ?
C17 H17 0.9300 . ?
C17 C16 1.411(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.338(4) . ?
C16 H16 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C24 H24 0.9300 . ?
C24 C23 1.405(4) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C31 H31 0.9300 . ?
C31 C30 1.419(4) . ?
C30 H30 0.9300 . ?
C23 H23 0.9300 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 C53 1.517(14) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
Cl2A C53A 1.666(15) . ?
C53A H53C 0.9700 . ?
C53A H53D 0.9700 . ?
C53A C52A 1.473(16) . ?
C52A H52C 0.9700 . ?
C52A H52D 0.9700 . ?
C52A Cl1A 1.764(15) . ?

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
C12 O1 C1 119.13(12) . . ?
C1 C2 C13 122.14(14) . . ?
C3 C2 C1 118.22(15) . . ?
C3 C2 C13 119.63(14) . . ?
O1 C12 C11 115.08(14) . . ?
O1 C12 C7 123.26(14) . . ?
C7 C12 C11 121.66(15) . . ?
C1 C6 C41 122.29(14) . . ?
C5 C6 C1 117.48(14) . . ?
C5 C6 C41 120.22(14) . . ?
C12 C11 C27 121.39(14) . . ?
C10 C11 C12 118.39(15) . . ?
C10 C11 C27 120.21(14) . . ?
C12 C7 C8 117.59(15) . . ?
C12 C7 C41 122.28(14) . . ?
C8 C7 C41 120.12(14) . . ?
O1 C1 C2 115.18(14) . . ?
O1 C1 C6 123.08(14) . . ?
C6 C1 C2 121.74(15) . . ?
C2 C3 H3 118.7 . . ?
C4 C3 C2 122.61(15) . . ?
C4 C3 H3 118.7 . . ?
C7 C8 H8 118.4 . . ?
C9 C8 C7 123.14(15) . . ?
C9 C8 H8 118.4 . . ?
C8 C9 C10 117.00(15) . . ?
C8 C9 C48 120.23(16) . . ?
C10 C9 C48 122.75(15) . . ?
C28 C27 C11 119.89(16) . . ?
C40 C27 C11 119.52(17) . . ?
C40 C27 C28 120.56(16) . . ?
C27 C28 C33 119.31(18) . . ?
C27 C28 C29 123.38(17) . . ?
C29 C28 C33 117.31(19) . . ?
C14 C13 C2 119.32(17) . . ?
C26 C13 C2 120.22(17) . . ?
C26 C13 C14 120.37(16) . . ?
C6 C5 H5 118.3 . . ?
C6 C5 C4 123.34(15) . . ?
C4 C5 H5 118.3 . . ?
C3 C4 C5 116.60(15) . . ?
C3 C4 C44 123.18(15) . . ?
C5 C4 C44 120.22(16) . . ?
C6 C41 C7 109.95(13) . . ?
C6 C41 C43 108.78(14) . . ?
C7 C41 C43 108.74(14) . . ?
C42 C41 C6 109.86(14) . . ?
C42 C41 C7 109.90(14) . . ?
C42 C41 C43 109.58(16) . . ?
C13 C14 C19 119.28(18) . . ?
C13 C14 C15 123.49(17) . . ?
C15 C14 C19 117.22(19) . . ?
C27 C40 C35 118.94(18) . . ?
C27 C40 C39 123.27(17) . . ?
C39 C40 C35 117.79(18) . . ?
C13 C26 C21 119.33(19) . . ?
C13 C26 C25 123.23(18) . . ?
C25 C26 C21 117.4(2) . . ?
C11 C10 C9 122.21(15) . . ?
C11 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C20 C19 C14 119.30(19) . . ?
C20 C19 C18 122.0(2) . . ?
C18 C19 C14 118.6(2) . . ?
C34 C33 C28 119.36(19) . . ?
C34 C33 C32 122.09(19) . . ?
C32 C33 C28 118.5(2) . . ?
C34 C35 C40 119.82(18) . . ?
C34 C35 C36 121.72(19) . . ?
C36 C35 C40 118.5(2) . . ?
C4 C44 C46 109.02(18) . . ?
C47 C44 C4 112.25(17) . . ?
C47 C44 C46 106.0(2) . . ?
C45 C44 C4 109.54(19) . . ?
C45 C44 C47 112.2(3) . . ?
C45 C44 C46 107.7(3) . . ?
C20 C21 C26 119.4(2) . . ?
C20 C21 C22 121.8(2) . . ?
C22 C21 C26 118.8(2) . . ?
C51 C48 C9 112.25(17) . . ?
C51 C48 C49 106.3(2) . . ?
C49 C48 C9 110.00(18) . . ?
C50 C48 C9 109.25(19) . . ?
C50 C48 C51 110.5(3) . . ?
C50 C48 C49 108.5(3) . . ?
C19 C20 H20 118.9 . . ?
C21 C20 C19 122.22(18) . . ?
C21 C20 H20 118.9 . . ?
C40 C39 H39 119.3 . . ?
C38 C39 C40 121.3(2) . . ?
C38 C39 H39 119.3 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C33 C34 H34 119.0 . . ?
C35 C34 C33 122.00(18) . . ?
C35 C34 H34 119.0 . . ?
C14 C15 H15 119.1 . . ?
C16 C15 C14 121.9(2) . . ?
C16 C15 H15 119.1 . . ?
C35 C36 H36 119.2 . . ?
C37 C36 C35 121.6(2) . . ?
C37 C36 H36 119.2 . . ?
C26 C25 H25 119.5 . . ?
C24 C25 C26 121.0(2) . . ?
C24 C25 H25 119.5 . . ?
C28 C29 H29 119.0 . . ?
C30 C29 C28 121.9(2) . . ?
C30 C29 H29 119.0 . . ?
C19 C18 H18 119.2 . . ?
C17 C18 C19 121.5(2) . . ?
C17 C18 H18 119.2 . . ?
C39 C38 H38 119.8 . . ?
C39 C38 C37 120.3(2) . . ?
C37 C38 H38 119.8 . . ?
C36 C37 C38 120.5(2) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C33 C32 H32 119.2 . . ?
C31 C32 C33 121.7(2) . . ?
C31 C32 H32 119.2 . . ?
C18 C17 H17 119.7 . . ?
C18 C17 C16 120.6(2) . . ?
C16 C17 H17 119.7 . . ?
C21 C22 H22 119.3 . . ?
C23 C22 C21 121.4(2) . . ?
C23 C22 H22 119.3 . . ?
C15 C16 C17 120.1(3) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C48 C51 H51A 109.5 . . ?
C48 C51 H51B 109.5 . . ?
C48 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C25 C24 H24 119.4 . . ?
C25 C24 C23 121.1(3) . . ?
C23 C24 H24 119.4 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C32 C31 H31 119.9 . . ?
C32 C31 C30 120.1(3) . . ?
C30 C31 H31 119.9 . . ?
C29 C30 C31 120.4(3) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C22 C23 C24 120.1(3) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
Cl1 C52 H52A 108.6 . . ?
Cl1 C52 H52B 108.6 . . ?
H52A C52 H52B 107.6 . . ?
C53 C52 Cl1 114.5(9) . . ?
C53 C52 H52A 108.6 . . ?
C53 C52 H52B 108.6 . . ?
Cl2 C53 H53A 108.4 . . ?
Cl2 C53 H53B 108.4 . . ?
C52 C53 Cl2 115.7(11) . . ?
C52 C53 H53A 108.4 . . ?
C52 C53 H53B 108.4 . . ?
H53A C53 H53B 107.4 . . ?
Cl2A C53A H53C 108.0 . . ?
Cl2A C53A H53D 108.0 . . ?
H53C C53A H53D 107.2 . . ?
C52A C53A Cl2A 117.4(13) . . ?
C52A C53A H53C 108.0 . . ?
C52A C53A H53D 108.0 . . ?
C53A C52A H52C 110.7 . . ?
C53A C52A H52D 110.7 . . ?
C53A C52A Cl1A 105.2(11) . . ?
H52C C52A H52D 108.8 . . ?
Cl1A C52A H52C 110.7 . . ?
Cl1A C52A H52D 110.7 . . ?

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
Cl1 C52 C53 Cl2 -178.9(11) . . . . ?
O1 C12 C11 C27 -0.2(3) . . . . ?
O1 C12 C11 C10 179.46(16) . . . . ?
O1 C12 C7 C8 -179.42(16) . . . . ?
O1 C12 C7 C41 0.0(3) . . . . ?
C2 C3 C4 C5 0.6(3) . . . . ?
C2 C3 C4 C44 -179.60(19) . . . . ?
C2 C13 C14 C19 -173.92(15) . . . . ?
C2 C13 C14 C15 5.7(3) . . . . ?
C2 C13 C26 C21 173.12(16) . . . . ?
C2 C13 C26 C25 -5.6(3) . . . . ?
C12 O1 C1 C2 179.23(16) . . . . ?
C12 O1 C1 C6 -0.6(3) . . . . ?
C12 C11 C27 C28 72.2(2) . . . . ?
C12 C11 C27 C40 -110.1(2) . . . . ?
C12 C11 C10 C9 0.4(3) . . . . ?
C12 C7 C8 C9 -0.5(3) . . . . ?
C12 C7 C41 C6 0.5(2) . . . . ?
C12 C7 C41 C42 121.53(19) . . . . ?
C12 C7 C41 C43 -118.53(19) . . . . ?
C6 C5 C4 C3 -0.4(3) . . . . ?
C6 C5 C4 C44 179.75(18) . . . . ?
C11 C12 C7 C8 0.7(3) . . . . ?
C11 C12 C7 C41 -179.91(17) . . . . ?
C11 C27 C28 C33 176.11(16) . . . . ?
C11 C27 C28 C29 -2.8(3) . . . . ?
C11 C27 C40 C35 -176.22(14) . . . . ?
C11 C27 C40 C39 3.4(3) . . . . ?
C7 C12 C11 C27 179.66(17) . . . . ?
C7 C12 C11 C10 -0.7(3) . . . . ?
C7 C8 C9 C10 0.3(3) . . . . ?
C7 C8 C9 C48 179.29(17) . . . . ?
C1 O1 C12 C11 179.94(16) . . . . ?
C1 O1 C12 C7 0.1(3) . . . . ?
C1 C2 C3 C4 -0.3(3) . . . . ?
C1 C2 C13 C14 -110.0(2) . . . . ?
C1 C2 C13 C26 73.4(2) . . . . ?
C1 C6 C5 C4 0.0(3) . . . . ?
C1 C6 C41 C7 -1.0(2) . . . . ?
C1 C6 C41 C42 -122.07(19) . . . . ?
C1 C6 C41 C43 117.99(19) . . . . ?
C3 C2 C1 O1 -179.93(17) . . . . ?
C3 C2 C1 C6 -0.1(3) . . . . ?
C3 C2 C13 C14 69.2(2) . . . . ?
C3 C2 C13 C26 -107.4(2) . . . . ?
C3 C4 C44 C47 -9.0(3) . . . . ?
C3 C4 C44 C46 -126.1(2) . . . . ?
C3 C4 C44 C45 116.4(3) . . . . ?
C8 C7 C41 C6 179.83(16) . . . . ?
C8 C7 C41 C42 -59.1(2) . . . . ?
C8 C7 C41 C43 60.8(2) . . . . ?
C8 C9 C10 C11 -0.3(3) . . . . ?
C8 C9 C48 C51 166.0(2) . . . . ?
C8 C9 C48 C49 47.9(3) . . . . ?
C8 C9 C48 C50 -71.0(3) . . . . ?
C27 C11 C10 C9 -179.89(18) . . . . ?
C27 C28 C33 C34 0.7(3) . . . . ?
C27 C28 C33 C32 -177.7(2) . . . . ?
C27 C28 C29 C30 178.6(2) . . . . ?
C27 C40 C35 C34 -0.5(3) . . . . ?
C27 C40 C35 C36 178.80(16) . . . . ?
C27 C40 C39 C38 -178.74(18) . . . . ?
C28 C27 C40 C35 1.4(2) . . . . ?
C28 C27 C40 C39 -178.99(16) . . . . ?
C28 C33 C34 C35 0.2(3) . . . . ?
C28 C33 C32 C31 -0.9(4) . . . . ?
C28 C29 C30 C31 -1.1(5) . . . . ?
C13 C2 C1 O1 -0.8(3) . . . . ?
C13 C2 C1 C6 179.08(18) . . . . ?
C13 C2 C3 C4 -179.52(18) . . . . ?
C13 C14 C19 C20 0.0(3) . . . . ?
C13 C14 C19 C18 178.59(17) . . . . ?
C13 C14 C15 C16 -178.88(19) . . . . ?
C13 C26 C21 C20 1.6(3) . . . . ?
C13 C26 C21 C22 -177.31(19) . . . . ?
C13 C26 C25 C24 178.7(2) . . . . ?
C5 C6 C1 O1 -179.93(17) . . . . ?
C5 C6 C1 C2 0.2(3) . . . . ?
C5 C6 C41 C7 -179.89(16) . . . . ?
C5 C6 C41 C42 59.0(2) . . . . ?
C5 C6 C41 C43 -60.9(2) . . . . ?
C5 C4 C44 C47 170.8(2) . . . . ?
C5 C4 C44 C46 53.8(3) . . . . ?
C5 C4 C44 C45 -63.8(3) . . . . ?
C41 C6 C1 O1 1.1(3) . . . . ?
C41 C6 C1 C2 -178.70(17) . . . . ?
C41 C6 C5 C4 178.99(17) . . . . ?
C41 C7 C8 C9 -179.93(17) . . . . ?
C14 C13 C26 C21 -3.4(3) . . . . ?
C14 C13 C26 C25 177.90(18) . . . . ?
C14 C19 C20 C21 -1.9(3) . . . . ?
C14 C19 C18 C17 0.6(3) . . . . ?
C14 C15 C16 C17 0.0(4) . . . . ?
C40 C27 C28 C33 -1.5(3) . . . . ?
C40 C27 C28 C29 179.55(18) . . . . ?
C40 C35 C34 C33 -0.3(3) . . . . ?
C40 C35 C36 C37 0.0(3) . . . . ?
C40 C39 C38 C37 -0.1(3) . . . . ?
C26 C13 C14 C19 2.6(2) . . . . ?
C26 C13 C14 C15 -177.70(17) . . . . ?
C26 C21 C20 C19 1.1(3) . . . . ?
C26 C21 C22 C23 -1.5(4) . . . . ?
C26 C25 C24 C23 -1.4(5) . . . . ?
C10 C11 C27 C28 -107.4(2) . . . . ?
C10 C11 C27 C40 70.2(2) . . . . ?
C10 C9 C48 C51 -15.1(3) . . . . ?
C10 C9 C48 C49 -133.2(2) . . . . ?
C10 C9 C48 C50 107.9(3) . . . . ?
C19 C14 C15 C16 0.8(3) . . . . ?
C19 C18 C17 C16 0.2(4) . . . . ?
C33 C28 C29 C30 -0.3(4) . . . . ?
C33 C32 C31 C30 -0.5(5) . . . . ?
C35 C40 C39 C38 0.8(3) . . . . ?
C35 C36 C37 C38 0.8(4) . . . . ?
C21 C26 C25 C24 0.0(4) . . . . ?
C21 C22 C23 C24 0.0(5) . . . . ?
C48 C9 C10 C11 -179.21(18) . . . . ?
C20 C19 C18 C17 179.2(2) . . . . ?
C20 C21 C22 C23 179.7(3) . . . . ?
C39 C40 C35 C34 179.87(17) . . . . ?
C39 C40 C35 C36 -0.8(3) . . . . ?
C39 C38 C37 C36 -0.8(4) . . . . ?
C34 C33 C32 C31 -179.3(3) . . . . ?
C34 C35 C36 C37 179.3(2) . . . . ?
C15 C14 C19 C20 -179.69(17) . . . . ?
C15 C14 C19 C18 -1.1(3) . . . . ?
C36 C35 C34 C33 -179.59(19) . . . . ?
C25 C26 C21 C20 -179.7(2) . . . . ?
C25 C26 C21 C22 1.4(3) . . . . ?
C25 C24 C23 C22 1.5(5) . . . . ?
C29 C28 C33 C34 179.70(19) . . . . ?
C29 C28 C33 C32 1.3(3) . . . . ?
C18 C19 C20 C21 179.6(2) . . . . ?
C18 C17 C16 C15 -0.5(4) . . . . ?
C32 C33 C34 C35 178.5(2) . . . . ?
C32 C31 C30 C29 1.5(5) . . . . ?
C22 C21 C20 C19 179.9(2) . . . . ?
Cl2A C53A C52A Cl1A -176.1(9) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.654
_oxdiff_exptl_absorpt_empirical_full_min 0.331
####################################################################### 
# 
# 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_210414e_0m
_database_code_depnum_ccdc_archive 'CCDC 2180359'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2022-06-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2021-04-21
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H4 Cl2, C51 H46 O'
_chemical_formula_sum            'C53 H50 Cl2 O'
_chemical_formula_weight         773.83
_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 0.0137 0.0067 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3281 0.5435 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.8128(4)
_cell_length_b                   12.9995(4)
_cell_length_c                   15.1372(4)
_cell_angle_alpha                93.8220(10)
_cell_angle_beta                 114.4420(10)
_cell_angle_gamma                108.3770(10)
_cell_volume                     2120.80(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    293.0
_cell_measurement_theta_max      56.94
_cell_measurement_theta_min      2.87
_shelx_estimated_absorpt_T_max   0.899
_shelx_estimated_absorpt_T_min   0.853
_exptl_absorpt_coefficient_mu    1.091
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.5861
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1070 before and 0.0451 after correction.
The Ratio of minimum to maximum transmission is 0.7802.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             820
_exptl_crystal_preparation       'Solvent evaporation'
_exptl_crystal_recrystallization_method 'Solvent evaporation'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23188
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.031
_diffrn_reflns_theta_min         2.865
_diffrn_ambient_temperature      293.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_source                   ?
_diffrn_source_current           3.57
_diffrn_source_power             0.2497215
_diffrn_source_voltage           69.95
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6619
_reflns_number_total             8459
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0125(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         8459
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0519
_refine_ls_restrained_S_all      1.101
_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)+(0.0887P)²+0.2795P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.1653
_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. Restrained distances
 C52-C53 \\sim C52A-C53A
 with sigma of 0.02
 C52-Cl2 \\sim C52A-Cl2A
 with sigma of 0.02
 C53-Cl2 \\sim C53A-Cl2A
 with sigma of 0.04
 C53-Cl1 \\sim C53A-Cl1A
 with sigma of 0.02
 C52-Cl1 \\sim C52A-Cl1A
 with sigma of 0.04
3. Others
 Sof(Cl1A)=Sof(Cl2A)=Sof(C52A)=Sof(H52C)=Sof(H52D)=Sof(C53A)=Sof(H53C)=
 Sof(H53D)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C53)=Sof(H53A)=Sof(H53B)=
 FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C53(H53A,H53B), C52A(H52C,H52D), C53A(H53C,H53D)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C8(H8), C10(H10), C16(H16), C17(H17), C18(H18), C19(H19),
 C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C40(H40), C41(H41), C42(H42),
  C43(H43), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50)
4.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
Cl1 Cl 0.9803(4) 0.8939(4) 1.3749(3) 0.1414(13) Uani 0.590(7) 1 d D . P A 1
Cl2 Cl 1.2420(4) 1.0234(4) 1.2689(4) 0.1458(13) Uani 0.590(7) 1 d D . P A 1
C52 C 1.1336(6) 1.0100(5) 1.3098(5) 0.0936(17) Uani 0.590(7) 1 d D . P A 1
H52A H 1.1711 1.0682 1.3715 0.112 Uiso 0.590(7) 1 calc R U P A 1
H52B H 1.0643 1.0249 1.2591 0.112 Uiso 0.590(7) 1 calc R U P A 1
C53 C 1.0810(4) 0.8987(4) 1.3311(4) 0.0815(14) Uani 0.590(7) 1 d D . P A 1
H53A H 1.1498 0.8819 1.3803 0.098 Uiso 0.590(7) 1 calc R U P A 1
H53B H 1.0394 0.8403 1.2690 0.098 Uiso 0.590(7) 1 calc R U P A 1
Cl1A Cl 0.9808(4) 0.9203(6) 1.3769(4) 0.1378(19) Uani 0.410(7) 1 d D . P A 2
Cl2A Cl 1.2161(8) 0.9679(7) 1.2427(6) 0.161(2) Uani 0.410(7) 1 d D . P A 2
C52A C 1.1286(8) 0.9165(8) 1.2981(6) 0.119(3) Uani 0.410(7) 1 d D . P A 2
H52C H 1.0586 0.8481 1.2519 0.143 Uiso 0.410(7) 1 calc R U P A 2
H52D H 1.1787 0.8944 1.3577 0.143 Uiso 0.410(7) 1 calc R U P A 2
C53A C 1.0775(8) 0.9911(8) 1.3295(6) 0.107(3) Uani 0.410(7) 1 d D . P A 2
H53C H 1.0306 1.0175 1.2717 0.128 Uiso 0.410(7) 1 calc R U P A 2
H53D H 1.1460 1.0568 1.3810 0.128 Uiso 0.410(7) 1 calc R U P A 2
O1 O 0.73473(9) 0.49637(7) 0.75510(7) 0.0452(3) Uani 1 1 d . . . . .
C1 C 0.82018(12) 0.68440(11) 0.83406(10) 0.0402(3) Uani 1 1 d . . . . .
C2 C 0.82348(13) 0.77236(11) 0.89466(10) 0.0424(3) Uani 1 1 d . . . . .
H2 H 0.8827 0.8448 0.9077 0.051 Uiso 1 1 calc R U . . .
C3 C 0.74284(13) 0.75746(11) 0.93665(10) 0.0401(3) Uani 1 1 d . . . . .
C4 C 0.65833(12) 0.65035(11) 0.91574(10) 0.0398(3) Uani 1 1 d . . . . .
H4 H 0.6026 0.6383 0.9437 0.048 Uiso 1 1 calc R U . . .
C5 C 0.65063(12) 0.55948(10) 0.85596(9) 0.0372(3) Uani 1 1 d . . . . .
C6 C 0.55649(12) 0.44375(10) 0.83798(9) 0.0371(3) Uani 1 1 d . . . . .
C7 C 0.56681(12) 0.35916(10) 0.77040(9) 0.0364(3) Uani 1 1 d . . . . .
C8 C 0.48965(12) 0.24754(11) 0.74364(10) 0.0393(3) Uani 1 1 d . . . . .
H8 H 0.4308 0.2259 0.7684 0.047 Uiso 1 1 calc R U . . .
C9 C 0.49401(12) 0.16612(11) 0.68272(10) 0.0394(3) Uani 1 1 d . . . . .
C10 C 0.58144(13) 0.20047(11) 0.64765(10) 0.0413(3) Uani 1 1 d . . . . .
H10 H 0.5868 0.1467 0.6058 0.050 Uiso 1 1 calc R U . . .
C11 C 0.66096(12) 0.31085(11) 0.67194(10) 0.0389(3) Uani 1 1 d . . . . .
C12 C 0.65266(12) 0.38903(10) 0.73372(9) 0.0375(3) Uani 1 1 d . . . . .
C13 C 0.73298(12) 0.57868(10) 0.81566(10) 0.0380(3) Uani 1 1 d . . . . .
C14 C 0.91005(13) 0.70628(10) 0.79184(10) 0.0404(3) Uani 1 1 d . . . . .
C15 C 1.03696(13) 0.73594(11) 0.85671(11) 0.0430(3) Uani 1 1 d . . . . .
C16 C 1.08421(15) 0.73682(13) 0.96033(12) 0.0545(4) Uani 1 1 d . . . . .
H16 H 1.0282 0.7149 0.9877 0.065 Uiso 1 1 calc R U . . .
C17 C 1.20755(17) 0.76829(15) 1.02077(14) 0.0657(5) Uani 1 1 d . . . . .
H17 H 1.2364 0.7684 1.0896 0.079 Uiso 1 1 calc R U . . .
C18 C 1.29308(17) 0.80082(16) 0.98215(15) 0.0676(5) Uani 1 1 d . . . . .
H18 H 1.3791 0.8230 1.0252 0.081 Uiso 1 1 calc R U . . .
C19 C 1.25351(16) 0.80055(14) 0.88482(15) 0.0625(4) Uani 1 1 d . . . . .
H19 H 1.3123 0.8224 0.8600 0.075 Uiso 1 1 calc R U . . .
C20 C 1.12496(14) 0.76809(12) 0.81796(12) 0.0486(4) Uani 1 1 d . . . . .
C21 C 1.08347(15) 0.76911(13) 0.71783(12) 0.0543(4) Uani 1 1 d . . . . .
H21 H 1.1423 0.7925 0.6932 0.065 Uiso 1 1 calc R U . . .
C22 C 0.95863(15) 0.73708(13) 0.65243(12) 0.0511(4) Uani 1 1 d . . . . .
C23 C 0.91680(19) 0.73848(16) 0.54984(13) 0.0674(5) Uani 1 1 d . . . . .
H23 H 0.9757 0.7620 0.5253 0.081 Uiso 1 1 calc R U . . .
C24 C 0.7961(2) 0.70736(19) 0.48681(14) 0.0776(6) Uani 1 1 d . . . . .
H24 H 0.7705 0.7088 0.4185 0.093 Uiso 1 1 calc R U . . .
C25 C 0.70670(19) 0.67226(19) 0.52202(14) 0.0750(5) Uani 1 1 d . . . . .
H25 H 0.6212 0.6491 0.4768 0.090 Uiso 1 1 calc R U . . .
C26 C 0.74206(16) 0.67146(15) 0.61960(12) 0.0583(4) Uani 1 1 d . . . . .
H26 H 0.6808 0.6489 0.6419 0.070 Uiso 1 1 calc R U . . .
C27 C 0.86904(14) 0.70364(11) 0.68949(11) 0.0452(3) Uani 1 1 d . . . . .
C28 C 0.74496(14) 0.85333(11) 1.00301(11) 0.0467(3) Uani 1 1 d . . . . .
C29 C 0.6244(2) 0.87053(19) 0.95143(17) 0.0917(7) Uani 1 1 d . . . . .
H29A H 0.6159 0.8911 0.8884 0.138 Uiso 1 1 calc R U . . .
H29B H 0.6241 0.9302 0.9944 0.138 Uiso 1 1 calc R U . . .
H29C H 0.5551 0.8014 0.9381 0.138 Uiso 1 1 calc R U . . .
C30 C 0.7581(2) 0.82324(16) 1.10205(13) 0.0739(5) Uani 1 1 d . . . . .
H30A H 0.6867 0.7566 1.0897 0.111 Uiso 1 1 calc R U . . .
H30B H 0.7619 0.8852 1.1454 0.111 Uiso 1 1 calc R U . . .
H30C H 0.8342 0.8087 1.1346 0.111 Uiso 1 1 calc R U . . .
C31 C 0.8538(2) 0.96093(14) 1.02743(17) 0.0785(6) Uani 1 1 d . . . . .
H31A H 0.9312 0.9480 1.0582 0.118 Uiso 1 1 calc R U . . .
H31B H 0.8550 1.0182 1.0738 0.118 Uiso 1 1 calc R U . . .
H31C H 0.8454 0.9859 0.9660 0.118 Uiso 1 1 calc R U . . .
C32 C 0.58285(16) 0.41046(12) 0.93852(11) 0.0504(4) Uani 1 1 d . . . . .
H32A H 0.6667 0.4102 0.9698 0.076 Uiso 1 1 calc R U . . .
H32B H 0.5228 0.3359 0.9274 0.076 Uiso 1 1 calc R U . . .
H32C H 0.5758 0.4641 0.9823 0.076 Uiso 1 1 calc R U . . .
C33 C 0.42547(13) 0.44442(12) 0.78932(12) 0.0502(4) Uani 1 1 d . . . . .
H33A H 0.4190 0.4988 0.8328 0.075 Uiso 1 1 calc R U . . .
H33B H 0.3654 0.3702 0.7790 0.075 Uiso 1 1 calc R U . . .
H33C H 0.4082 0.4647 0.7249 0.075 Uiso 1 1 calc R U . . .
C34 C 0.40717(14) 0.04453(11) 0.65791(11) 0.0460(3) Uani 1 1 d . . . . .
C35 C 0.27428(17) 0.03658(16) 0.62495(17) 0.0772(6) Uani 1 1 d . . . . .
H35A H 0.2190 -0.0418 0.6061 0.116 Uiso 1 1 calc R U . . .
H35B H 0.2488 0.0705 0.5677 0.116 Uiso 1 1 calc R U . . .
H35C H 0.2698 0.0760 0.6800 0.116 Uiso 1 1 calc R U . . .
C36 C 0.4486(2) -0.00212(16) 0.74986(15) 0.0850(7) Uani 1 1 d . . . . .
H36A H 0.4395 0.0375 0.8020 0.127 Uiso 1 1 calc R U . . .
H36B H 0.5355 0.0075 0.7738 0.127 Uiso 1 1 calc R U . . .
H36C H 0.3974 -0.0815 0.7333 0.127 Uiso 1 1 calc R U . . .
C37 C 0.4063(2) -0.02722(14) 0.57344(15) 0.0734(5) Uani 1 1 d . . . . .
H37A H 0.3450 -0.1027 0.5567 0.110 Uiso 1 1 calc R U . . .
H37B H 0.4885 -0.0301 0.5946 0.110 Uiso 1 1 calc R U . . .
H37C H 0.3848 0.0050 0.5148 0.110 Uiso 1 1 calc R U . . .
C38 C 0.75339(13) 0.34340(10) 0.63246(10) 0.0398(3) Uani 1 1 d . . . . .
C39 C 0.88044(13) 0.37315(11) 0.69715(11) 0.0438(3) Uani 1 1 d . . . . .
C40 C 0.92767(15) 0.37874(14) 0.80164(12) 0.0564(4) Uani 1 1 d . . . . .
H40 H 0.8723 0.3640 0.8300 0.068 Uiso 1 1 calc R U . . .
C41 C 1.04986(17) 0.40468(18) 0.86117(14) 0.0736(5) Uani 1 1 d . . . . .
H41 H 1.0791 0.4087 0.9306 0.088 Uiso 1 1 calc R U . . .
C42 C 1.13418(17) 0.42575(19) 0.82092(15) 0.0777(6) Uani 1 1 d . . . . .
H42 H 1.2194 0.4423 0.8632 0.093 Uiso 1 1 calc R U . . .
C43 C 1.09449(16) 0.42249(16) 0.72300(15) 0.0674(5) Uani 1 1 d . . . . .
H43 H 1.1524 0.4375 0.6971 0.081 Uiso 1 1 calc R U . . .
C44 C 0.96722(14) 0.39691(13) 0.65759(12) 0.0498(4) Uani 1 1 d . . . . .
C45 C 0.92521(15) 0.39170(13) 0.55614(12) 0.0536(4) Uani 1 1 d . . . . .
H45 H 0.9832 0.4075 0.5302 0.064 Uiso 1 1 calc R U . . .
C46 C 0.80083(15) 0.36408(12) 0.49165(11) 0.0477(4) Uani 1 1 d . . . . .
C47 C 0.75776(18) 0.35745(14) 0.38712(13) 0.0594(4) Uani 1 1 d . . . . .
H47 H 0.8157 0.3737 0.3613 0.071 Uiso 1 1 calc R U . . .
C48 C 0.6372(2) 0.32880(15) 0.32482(13) 0.0647(5) Uani 1 1 d . . . . .
H48 H 0.6108 0.3239 0.2555 0.078 Uiso 1 1 calc R U . . .
C49 C 0.54892(18) 0.30580(15) 0.36160(13) 0.0640(4) Uani 1 1 d . . . . .
H49 H 0.4638 0.2864 0.3170 0.077 Uiso 1 1 calc R U . . .
C50 C 0.58565(15) 0.31144(13) 0.46066(12) 0.0530(4) Uani 1 1 d . . . . .
H50 H 0.5254 0.2963 0.4842 0.064 Uiso 1 1 calc R U . . .
C51 C 0.71233(13) 0.33953(11) 0.52987(10) 0.0419(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
Cl1 C53 1.663(6) . ?
Cl2 C52 1.709(7) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C52 C53 1.509(7) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
Cl1A C53A 1.733(11) . ?
Cl2A C52A 1.670(12) . ?
C52A H52C 0.9900 . ?
C52A H52D 0.9900 . ?
C52A C53A 1.480(10) . ?
C53A H53C 0.9900 . ?
C53A H53D 0.9900 . ?
O1 C12 1.3749(15) . ?
O1 C13 1.3738(14) . ?
C1 C2 1.3957(18) . ?
C1 C13 1.3921(18) . ?
C1 C14 1.4975(17) . ?
C2 H2 0.9500 . ?
C2 C3 1.3938(18) . ?
C3 C4 1.3851(18) . ?
C3 C28 1.5338(17) . ?
C4 H4 0.9500 . ?
C4 C5 1.3906(17) . ?
C5 C6 1.5238(17) . ?
C5 C13 1.3908(17) . ?
C6 C7 1.5254(17) . ?
C6 C32 1.5402(18) . ?
C6 C33 1.5321(19) . ?
C7 C8 1.3901(18) . ?
C7 C12 1.3907(17) . ?
C8 H8 0.9500 . ?
C8 C9 1.3870(18) . ?
C9 C10 1.3944(18) . ?
C9 C34 1.5309(18) . ?
C10 H10 0.9500 . ?
C10 C11 1.3893(18) . ?
C11 C12 1.3938(17) . ?
C11 C38 1.4974(17) . ?
C14 C15 1.411(2) . ?
C14 C27 1.409(2) . ?
C15 C16 1.426(2) . ?
C15 C20 1.4397(19) . ?
C16 H16 0.9500 . ?
C16 C17 1.359(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.411(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.344(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.428(2) . ?
C20 C21 1.386(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.388(2) . ?
C22 C23 1.421(2) . ?
C22 C27 1.4395(19) . ?
C23 H23 0.9500 . ?
C23 C24 1.341(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.419(3) . ?
C25 H25 0.9500 . ?
C25 C26 1.356(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.424(2) . ?
C28 C29 1.513(3) . ?
C28 C30 1.530(2) . ?
C28 C31 1.521(2) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.529(2) . ?
C34 C36 1.514(2) . ?
C34 C37 1.525(2) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.411(2) . ?
C38 C51 1.4099(19) . ?
C39 C40 1.428(2) . ?
C39 C44 1.4315(18) . ?
C40 H40 0.9500 . ?
C40 C41 1.355(2) . ?
C41 H41 0.9500 . ?
C41 C42 1.412(3) . ?
C42 H42 0.9500 . ?
C42 C43 1.346(3) . ?
C43 H43 0.9500 . ?
C43 C44 1.424(2) . ?
C44 C45 1.390(2) . ?
C45 H45 0.9500 . ?
C45 C46 1.388(2) . ?
C46 C47 1.430(2) . ?
C46 C51 1.4358(18) . ?
C47 H47 0.9500 . ?
C47 C48 1.341(3) . ?
C48 H48 0.9500 . ?
C48 C49 1.417(3) . ?
C49 H49 0.9500 . ?
C49 C50 1.362(2) . ?
C50 H50 0.9500 . ?
C50 C51 1.426(2) . ?

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
Cl2 C52 H52A 108.2 . . ?
Cl2 C52 H52B 108.2 . . ?
H52A C52 H52B 107.4 . . ?
C53 C52 Cl2 116.2(5) . . ?
C53 C52 H52A 108.2 . . ?
C53 C52 H52B 108.2 . . ?
Cl1 C53 H53A 108.9 . . ?
Cl1 C53 H53B 108.9 . . ?
C52 C53 Cl1 113.3(5) . . ?
C52 C53 H53A 108.9 . . ?
C52 C53 H53B 108.9 . . ?
H53A C53 H53B 107.7 . . ?
Cl2A C52A H52C 108.2 . . ?
Cl2A C52A H52D 108.2 . . ?
H52C C52A H52D 107.3 . . ?
C53A C52A Cl2A 116.5(9) . . ?
C53A C52A H52C 108.2 . . ?
C53A C52A H52D 108.2 . . ?
Cl1A C53A H53C 109.7 . . ?
Cl1A C53A H53D 109.7 . . ?
C52A C53A Cl1A 109.8(8) . . ?
C52A C53A H53C 109.7 . . ?
C52A C53A H53D 109.7 . . ?
H53C C53A H53D 108.2 . . ?
C13 O1 C12 119.04(9) . . ?
C2 C1 C14 119.39(11) . . ?
C13 C1 C2 118.23(11) . . ?
C13 C1 C14 122.38(11) . . ?
C1 C2 H2 118.9 . . ?
C3 C2 C1 122.22(12) . . ?
C3 C2 H2 118.9 . . ?
C2 C3 C28 122.84(12) . . ?
C4 C3 C2 116.85(11) . . ?
C4 C3 C28 120.31(11) . . ?
C3 C4 H4 118.2 . . ?
C3 C4 C5 123.53(12) . . ?
C5 C4 H4 118.2 . . ?
C4 C5 C6 120.37(11) . . ?
C4 C5 C13 117.43(11) . . ?
C13 C5 C6 122.19(11) . . ?
C5 C6 C7 110.12(10) . . ?
C5 C6 C32 109.09(11) . . ?
C5 C6 C33 109.76(11) . . ?
C7 C6 C32 108.85(10) . . ?
C7 C6 C33 109.60(11) . . ?
C33 C6 C32 109.40(11) . . ?
C8 C7 C6 120.37(11) . . ?
C8 C7 C12 117.34(11) . . ?
C12 C7 C6 122.29(11) . . ?
C7 C8 H8 118.2 . . ?
C9 C8 C7 123.50(12) . . ?
C9 C8 H8 118.2 . . ?
C8 C9 C10 116.90(11) . . ?
C8 C9 C34 120.40(11) . . ?
C10 C9 C34 122.69(11) . . ?
C9 C10 H10 118.9 . . ?
C11 C10 C9 122.12(11) . . ?
C11 C10 H10 118.9 . . ?
C10 C11 C12 118.47(11) . . ?
C10 C11 C38 120.03(11) . . ?
C12 C11 C38 121.50(11) . . ?
O1 C12 C7 123.09(11) . . ?
O1 C12 C11 115.24(10) . . ?
C7 C12 C11 121.67(11) . . ?
O1 C13 C1 115.01(11) . . ?
O1 C13 C5 123.25(11) . . ?
C5 C13 C1 121.73(11) . . ?
C15 C14 C1 119.14(12) . . ?
C27 C14 C1 120.22(12) . . ?
C27 C14 C15 120.53(12) . . ?
C14 C15 C16 123.39(13) . . ?
C14 C15 C20 119.22(13) . . ?
C16 C15 C20 117.39(14) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 C15 121.55(15) . . ?
C17 C16 H16 119.2 . . ?
C16 C17 H17 119.7 . . ?
C16 C17 C18 120.55(17) . . ?
C18 C17 H17 119.7 . . ?
C17 C18 H18 119.8 . . ?
C19 C18 C17 120.38(16) . . ?
C19 C18 H18 119.8 . . ?
C18 C19 H19 119.3 . . ?
C18 C19 C20 121.39(15) . . ?
C20 C19 H19 119.3 . . ?
C19 C20 C15 118.73(14) . . ?
C21 C20 C15 119.46(14) . . ?
C21 C20 C19 121.79(14) . . ?
C20 C21 H21 119.0 . . ?
C20 C21 C22 122.02(13) . . ?
C22 C21 H21 119.0 . . ?
C21 C22 C23 121.69(14) . . ?
C21 C22 C27 119.37(14) . . ?
C23 C22 C27 118.93(15) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 C22 121.55(16) . . ?
C24 C23 H23 119.2 . . ?
C23 C24 H24 120.0 . . ?
C23 C24 C25 120.07(17) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 119.7 . . ?
C26 C25 C24 120.63(18) . . ?
C26 C25 H25 119.7 . . ?
C25 C26 H26 119.3 . . ?
C25 C26 C27 121.46(15) . . ?
C27 C26 H26 119.3 . . ?
C14 C27 C22 119.31(13) . . ?
C14 C27 C26 123.33(13) . . ?
C26 C27 C22 117.34(13) . . ?
C29 C28 C3 109.07(13) . . ?
C29 C28 C30 108.92(16) . . ?
C29 C28 C31 110.18(16) . . ?
C30 C28 C3 109.29(12) . . ?
C31 C28 C3 112.27(12) . . ?
C31 C28 C30 107.04(14) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C6 C32 H32A 109.5 . . ?
C6 C32 H32B 109.5 . . ?
C6 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C6 C33 H33A 109.5 . . ?
C6 C33 H33B 109.5 . . ?
C6 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C9 110.27(12) . . ?
C36 C34 C9 108.93(13) . . ?
C36 C34 C35 109.25(16) . . ?
C36 C34 C37 108.81(15) . . ?
C37 C34 C9 112.29(12) . . ?
C37 C34 C35 107.22(14) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 C11 119.96(12) . . ?
C51 C38 C11 119.68(12) . . ?
C51 C38 C39 120.31(12) . . ?
C38 C39 C40 122.92(12) . . ?
C38 C39 C44 119.57(13) . . ?
C40 C39 C44 117.50(13) . . ?
C39 C40 H40 119.3 . . ?
C41 C40 C39 121.37(15) . . ?
C41 C40 H40 119.3 . . ?
C40 C41 H41 119.7 . . ?
C40 C41 C42 120.60(17) . . ?
C42 C41 H41 119.7 . . ?
C41 C42 H42 119.8 . . ?
C43 C42 C41 120.34(17) . . ?
C43 C42 H42 119.8 . . ?
C42 C43 H43 119.4 . . ?
C42 C43 C44 121.16(15) . . ?
C44 C43 H43 119.4 . . ?
C43 C44 C39 119.02(14) . . ?
C45 C44 C39 119.45(14) . . ?
C45 C44 C43 121.50(14) . . ?
C44 C45 H45 119.1 . . ?
C46 C45 C44 121.74(13) . . ?
C46 C45 H45 119.1 . . ?
C45 C46 C47 121.58(14) . . ?
C45 C46 C51 119.61(13) . . ?
C47 C46 C51 118.80(15) . . ?
C46 C47 H47 119.3 . . ?
C48 C47 C46 121.37(15) . . ?
C48 C47 H47 119.3 . . ?
C47 C48 H48 119.8 . . ?
C47 C48 C49 120.50(15) . . ?
C49 C48 H48 119.8 . . ?
C48 C49 H49 119.9 . . ?
C50 C49 C48 120.22(17) . . ?
C50 C49 H49 119.9 . . ?
C49 C50 H50 119.2 . . ?
C49 C50 C51 121.58(15) . . ?
C51 C50 H50 119.2 . . ?
C38 C51 C46 119.29(13) . . ?
C38 C51 C50 123.19(12) . . ?
C50 C51 C46 117.52(13) . . ?

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
Cl2 C52 C53 Cl1 177.7(4) . . . . ?
Cl2A C52A C53A Cl1A 175.7(6) . . . . ?
C1 C2 C3 C4 0.2(2) . . . . ?
C1 C2 C3 C28 -179.74(13) . . . . ?
C1 C14 C15 C16 5.81(19) . . . . ?
C1 C14 C15 C20 -173.68(12) . . . . ?
C1 C14 C27 C22 173.06(12) . . . . ?
C1 C14 C27 C26 -5.6(2) . . . . ?
C2 C1 C13 O1 179.71(12) . . . . ?
C2 C1 C13 C5 -0.1(2) . . . . ?
C2 C1 C14 C15 68.18(17) . . . . ?
C2 C1 C14 C27 -108.11(15) . . . . ?
C2 C3 C4 C5 -0.1(2) . . . . ?
C2 C3 C28 C29 115.25(18) . . . . ?
C2 C3 C28 C30 -125.77(16) . . . . ?
C2 C3 C28 C31 -7.2(2) . . . . ?
C3 C4 C5 C6 178.91(12) . . . . ?
C3 C4 C5 C13 0.0(2) . . . . ?
C4 C3 C28 C29 -64.63(19) . . . . ?
C4 C3 C28 C30 54.35(18) . . . . ?
C4 C3 C28 C31 172.96(15) . . . . ?
C4 C5 C6 C7 -179.95(12) . . . . ?
C4 C5 C6 C32 -60.55(16) . . . . ?
C4 C5 C6 C33 59.30(16) . . . . ?
C4 C5 C13 O1 -179.68(12) . . . . ?
C4 C5 C13 C1 0.1(2) . . . . ?
C5 C6 C7 C8 -179.98(11) . . . . ?
C5 C6 C7 C12 0.44(17) . . . . ?
C6 C5 C13 O1 1.5(2) . . . . ?
C6 C5 C13 C1 -178.79(12) . . . . ?
C6 C7 C8 C9 -179.87(12) . . . . ?
C6 C7 C12 O1 0.0(2) . . . . ?
C6 C7 C12 C11 -179.93(12) . . . . ?
C7 C8 C9 C10 0.1(2) . . . . ?
C7 C8 C9 C34 179.05(12) . . . . ?
C8 C7 C12 O1 -179.58(12) . . . . ?
C8 C7 C12 C11 0.5(2) . . . . ?
C8 C9 C10 C11 -0.1(2) . . . . ?
C8 C9 C34 C35 48.20(18) . . . . ?
C8 C9 C34 C36 -71.69(18) . . . . ?
C8 C9 C34 C37 167.71(14) . . . . ?
C9 C10 C11 C12 0.3(2) . . . . ?
C9 C10 C11 C38 179.89(12) . . . . ?
C10 C9 C34 C35 -132.86(16) . . . . ?
C10 C9 C34 C36 107.24(17) . . . . ?
C10 C9 C34 C37 -13.4(2) . . . . ?
C10 C11 C12 O1 179.58(12) . . . . ?
C10 C11 C12 C7 -0.5(2) . . . . ?
C10 C11 C38 C39 -108.20(15) . . . . ?
C10 C11 C38 C51 69.08(17) . . . . ?
C11 C38 C39 C40 -2.8(2) . . . . ?
C11 C38 C39 C44 175.82(12) . . . . ?
C11 C38 C51 C46 -176.08(11) . . . . ?
C11 C38 C51 C50 3.49(19) . . . . ?
C12 O1 C13 C1 179.32(11) . . . . ?
C12 O1 C13 C5 -0.92(19) . . . . ?
C12 C7 C8 C9 -0.3(2) . . . . ?
C12 C11 C38 C39 71.42(17) . . . . ?
C12 C11 C38 C51 -111.29(15) . . . . ?
C13 O1 C12 C7 0.18(19) . . . . ?
C13 O1 C12 C11 -179.89(11) . . . . ?
C13 C1 C2 C3 -0.1(2) . . . . ?
C13 C1 C14 C15 -111.42(15) . . . . ?
C13 C1 C14 C27 72.29(18) . . . . ?
C13 C5 C6 C7 -1.14(17) . . . . ?
C13 C5 C6 C32 118.27(14) . . . . ?
C13 C5 C6 C33 -121.88(14) . . . . ?
C14 C1 C2 C3 -179.68(13) . . . . ?
C14 C1 C13 O1 -0.68(19) . . . . ?
C14 C1 C13 C5 179.56(13) . . . . ?
C14 C15 C16 C17 -178.54(14) . . . . ?
C14 C15 C20 C19 178.50(13) . . . . ?
C14 C15 C20 C21 -0.1(2) . . . . ?
C15 C14 C27 C22 -3.2(2) . . . . ?
C15 C14 C27 C26 178.19(13) . . . . ?
C15 C16 C17 C18 -0.3(3) . . . . ?
C15 C20 C21 C22 -1.8(2) . . . . ?
C16 C15 C20 C19 -1.0(2) . . . . ?
C16 C15 C20 C21 -179.65(13) . . . . ?
C16 C17 C18 C19 -0.3(3) . . . . ?
C17 C18 C19 C20 0.2(3) . . . . ?
C18 C19 C20 C15 0.4(2) . . . . ?
C18 C19 C20 C21 179.04(15) . . . . ?
C19 C20 C21 C22 179.64(14) . . . . ?
C20 C15 C16 C17 1.0(2) . . . . ?
C20 C21 C22 C23 179.92(15) . . . . ?
C20 C21 C22 C27 1.2(2) . . . . ?
C21 C22 C23 C24 179.93(18) . . . . ?
C21 C22 C27 C14 1.3(2) . . . . ?
C21 C22 C27 C26 -179.99(14) . . . . ?
C22 C23 C24 C25 0.2(3) . . . . ?
C23 C22 C27 C14 -177.47(14) . . . . ?
C23 C22 C27 C26 1.2(2) . . . . ?
C23 C24 C25 C26 1.1(3) . . . . ?
C24 C25 C26 C27 -1.1(3) . . . . ?
C25 C26 C27 C14 178.62(16) . . . . ?
C25 C26 C27 C22 0.0(2) . . . . ?
C27 C14 C15 C16 -177.91(13) . . . . ?
C27 C14 C15 C20 2.60(19) . . . . ?
C27 C22 C23 C24 -1.3(3) . . . . ?
C28 C3 C4 C5 179.74(13) . . . . ?
C32 C6 C7 C8 60.47(16) . . . . ?
C32 C6 C7 C12 -119.11(14) . . . . ?
C33 C6 C7 C8 -59.14(16) . . . . ?
C33 C6 C7 C12 121.28(14) . . . . ?
C34 C9 C10 C11 -179.02(13) . . . . ?
C38 C11 C12 O1 -0.05(19) . . . . ?
C38 C11 C12 C7 179.89(12) . . . . ?
C38 C39 C40 C41 178.19(16) . . . . ?
C38 C39 C44 C43 -177.52(14) . . . . ?
C38 C39 C44 C45 0.8(2) . . . . ?
C39 C38 C51 C46 1.19(19) . . . . ?
C39 C38 C51 C50 -179.23(12) . . . . ?
C39 C40 C41 C42 -0.8(3) . . . . ?
C39 C44 C45 C46 0.1(2) . . . . ?
C40 C39 C44 C43 1.2(2) . . . . ?
C40 C39 C44 C45 179.55(14) . . . . ?
C40 C41 C42 C43 1.3(3) . . . . ?
C41 C42 C43 C44 -0.6(3) . . . . ?
C42 C43 C44 C39 -0.7(3) . . . . ?
C42 C43 C44 C45 -179.00(18) . . . . ?
C43 C44 C45 C46 178.36(15) . . . . ?
C44 C39 C40 C41 -0.5(2) . . . . ?
C44 C45 C46 C47 -179.21(14) . . . . ?
C44 C45 C46 C51 -0.3(2) . . . . ?
C45 C46 C47 C48 178.80(15) . . . . ?
C45 C46 C51 C38 -0.3(2) . . . . ?
C45 C46 C51 C50 -179.91(13) . . . . ?
C46 C47 C48 C49 1.0(3) . . . . ?
C47 C46 C51 C38 178.61(12) . . . . ?
C47 C46 C51 C50 -0.98(19) . . . . ?
C47 C48 C49 C50 -0.7(3) . . . . ?
C48 C49 C50 C51 -0.4(2) . . . . ?
C49 C50 C51 C38 -178.32(14) . . . . ?
C49 C50 C51 C46 1.3(2) . . . . ?
C51 C38 C39 C40 179.89(13) . . . . ?
C51 C38 C39 C44 -1.4(2) . . . . ?
C51 C46 C47 C48 -0.1(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_mo_210513a_0m
_database_code_depnum_ccdc_archive 'CCDC 2180357'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2022-06-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2021-12-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_chemical_formula_moiety         'C51 H46 O, C H2 Br2'
_chemical_formula_sum            'C52 H48 Br2 O'
_chemical_formula_weight         848.767
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Br -0.28346 2.55990 17.17890 5.23580 5.63770 3.98510 2.17230 16.57960 0.26090
41.43280 2.95569992065
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_symmetry_Int_Tables_number      2
_cell_length_a                   12.795(9)
_cell_length_b                   13.079(9)
_cell_length_c                   14.955(10)
_cell_angle_alpha                93.844(9)
_cell_angle_beta                 114.095(9)
_cell_angle_gamma                108.298(9)
_cell_volume                     2113(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1206
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.64
_cell_measurement_theta_min      2.77
_exptl_absorpt_coefficient_mu    1.955
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3725
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1269 before and 0.0605 after correction.
The Ratio of minimum to maximum transmission is 0.4997.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_meas      .
_exptl_crystal_description       needle
_exptl_crystal_F_000             875.508
_exptl_crystal_preparation       'solvent evaporation'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_diffrn_reflns_av_R_equivalents  0.1067
_diffrn_reflns_av_unetI/netI     0.2191
_diffrn_reflns_Laue_measured_fraction_full 0.9882
_diffrn_reflns_Laue_measured_fraction_max 0.9882
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16640
_diffrn_reflns_point_group_measured_fraction_full 0.9882
_diffrn_reflns_point_group_measured_fraction_max 0.9882
_diffrn_reflns_theta_full        25.0270
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.68
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9882
_diffrn_measured_fraction_theta_max 0.9882
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -15
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                2454
_reflns_number_total             7384
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_refine_diff_density_max         1.0356
_refine_diff_density_min         -0.8903
_refine_diff_density_rms         0.1594
_refine_ls_d_res_high            0.8400
_refine_ls_d_res_low             12.0990
_refine_ls_goodness_of_fit_ref   0.9525
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    98
_refine_ls_number_parameters     551
_refine_ls_number_reflns         7384
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.2441
_refine_ls_R_factor_gt           0.0907
_refine_ls_restrained_S_all      0.9508
_refine_ls_shift/su_max          0.0027
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1485P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2321
_refine_ls_wR_factor_ref         0.3248
_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. Restrained distances
 C52-Br1 = C52-Br2 = C52a-Br2a = C52a-Br1a
 1.94 with sigma of 0.02
 Br1-Br2 \\sim Br1a-Br2a
 with sigma of 0.04
 C44-C46 \\sim C44-C46a
 with sigma of 0.02
 C44-C47 \\sim C44-C47a
 with sigma of 0.02
 C44-C45 \\sim C44-C45a
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C47) \\sim Ueq, Uanis(C47a) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C45a) = Uanis(C45)
Uanis(C46a) = Uanis(C46)
4. Others
 Sof(Br1a)=Sof(C52a)=Sof(H52c)=Sof(H52d)=Sof(Br2a)=1-FVAR(1)
 Sof(Br1)=Sof(C52)=Sof(H52a)=Sof(H52b)=Sof(Br2)=FVAR(1)
 Sof(C45a)=Sof(H45d)=Sof(H45e)=Sof(H45f)=Sof(C46a)=Sof(H46d)=Sof(H46e)=
 Sof(H46f)=Sof(C47a)=Sof(H47d)=Sof(H47e)=Sof(H47f)=1-FVAR(2)
 Sof(C46)=Sof(H46a)=Sof(H46b)=Sof(H46c)=Sof(C47)=Sof(H47a)=Sof(H47b)=Sof(H47c)=
 Sof(C45)=Sof(H45a)=Sof(H45b)=Sof(H45c)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C52(H52a,H52b), C52a(H52c,H52d)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11), C15(H15), C16(H16), C17(H17), C18(H18),
 C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C29(H29), C30(H30), C31(H31),
  C32(H32), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41)
5.c Idealised Me refined as rotating group:
 C42(H42a,H42b,H42c), C43(H43a,H43b,H43c), C46(H46a,H46b,H46c), C47(H47a,H47b,
 H47c), C49(H49a,H49b,H49c), C50(H50a,H50b,H50c), C51(H51a,H51b,H51c), C45(H45a,
 H45b,H45c), C45a(H45d,H45e,H45f), C46a(H46d,H46e,H46f), C47a(H47d,H47e,H47f)
;
_atom_sites_solution_primary     direct
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_disorder_group
O1 O 0.7663(4) 0.0030(3) 0.2473(3) 0.0449(12) Uani 1.000000 . . .
C1 C 0.8478(5) 0.1099(5) 0.2677(5) 0.0388(16) Uani 1.000000 . . .
C2 C 0.8383(6) 0.1871(5) 0.3282(5) 0.0394(16) Uani 1.000000 . . .
C3 C 0.9159(6) 0.2970(5) 0.3495(5) 0.0432(17) Uani 1.000000 . . .
H3 H 0.9097(6) 0.3499(5) 0.3898(5) 0.052(2) Uiso 1.000000 R . .
C4 C 1.0031(6) 0.3312(5) 0.3128(5) 0.0400(16) Uani 1.000000 . . .
C5 C 1.0064(5) 0.2486(5) 0.2523(5) 0.0403(16) Uani 1.000000 . . .
H5 H 1.0632(5) 0.2686(5) 0.2267(5) 0.048(2) Uiso 1.000000 R . .
C6 C 0.9303(5) 0.1375(5) 0.2273(4) 0.0341(15) Uani 1.000000 . . .
C7 C 0.9409(5) 0.0535(5) 0.1606(5) 0.0356(15) Uani 1.000000 . . .
C8 C 0.8487(5) -0.0613(5) 0.1453(4) 0.0333(15) Uani 1.000000 . . .
C9 C 0.8421(6) -0.1524(5) 0.0857(5) 0.0412(16) Uani 1.000000 . . .
H9 H 0.8970(6) -0.1411(5) 0.0581(5) 0.049(2) Uiso 1.000000 R . .
C10 C 0.7569(6) -0.2600(5) 0.0653(5) 0.0399(16) Uani 1.000000 . . .
C11 C 0.6786(6) -0.2726(5) 0.1097(5) 0.0418(16) Uani 1.000000 . . .
H11 H 0.6216(6) -0.3429(5) 0.0988(5) 0.050(2) Uiso 1.000000 R . .
C12 C 0.6816(5) -0.1846(5) 0.1700(5) 0.0359(15) Uani 1.000000 . . .
C13 C 0.7670(5) -0.0798(5) 0.1857(5) 0.0369(16) Uani 1.000000 . . .
C53 C 0.7038(7) 0.1382(5) 0.5144(6) 0.0503(19) Uani 1.000000 . . .
C15 C 0.7519(9) 0.1451(6) 0.6210(7) 0.070(2) Uani 1.000000 . . .
H15 H 0.6972(9) 0.1282(6) 0.6488(7) 0.084(3) Uiso 1.000000 R . .
C16 C 0.8712(10) 0.1748(7) 0.6803(7) 0.075(2) Uani 1.000000 . . .
H16 H 0.8985(10) 0.1814(7) 0.7491(7) 0.091(3) Uiso 1.000000 R . .
C17 C 0.9592(8) 0.1971(6) 0.6416(7) 0.070(2) Uani 1.000000 . . .
H17 H 1.0427(8) 0.2161(6) 0.6840(7) 0.084(3) Uiso 1.000000 R . .
C18 C 0.9179(7) 0.1897(5) 0.5418(6) 0.0549(19) Uani 1.000000 . . .
H18 H 0.9751(7) 0.2043(5) 0.5164(6) 0.066(2) Uiso 1.000000 R . .
C19 C 0.7909(6) 0.1605(5) 0.4735(6) 0.0454(18) Uani 1.000000 . . .
C20 C 0.7483(6) 0.1571(5) 0.3704(5) 0.0398(16) Uani 1.000000 . . .
C21 C 0.6219(6) 0.1270(5) 0.3067(5) 0.0439(17) Uani 1.000000 . . .
C22 C 0.5713(7) 0.1181(6) 0.2020(6) 0.066(2) Uani 1.000000 . . .
H22 H 0.6241(7) 0.1306(6) 0.1724(6) 0.079(3) Uiso 1.000000 R . .
C23 C 0.4506(8) 0.0926(8) 0.1430(7) 0.086(3) Uani 1.000000 . . .
H23 H 0.4208(8) 0.0875(8) 0.0742(7) 0.104(3) Uiso 1.000000 R . .
C24 C 0.3683(8) 0.0732(7) 0.1879(8) 0.088(3) Uani 1.000000 . . .
H24 H 0.2847(8) 0.0570(7) 0.1480(8) 0.105(3) Uiso 1.000000 R . .
C25 C 0.4093(7) 0.0781(7) 0.2837(8) 0.070(2) Uani 1.000000 . . .
H25 H 0.3535(7) 0.0640(7) 0.3105(8) 0.084(3) Uiso 1.000000 R . .
C26 C 0.5354(7) 0.1042(5) 0.3487(6) 0.0539(19) Uani 1.000000 . . .
C27 C 0.5786(7) 0.1098(6) 0.4508(6) 0.058(2) Uani 1.000000 . . .
H27 H 0.5229(7) 0.0943(6) 0.4777(6) 0.070(2) Uiso 1.000000 R . .
C28 C 0.5424(7) -0.2367(5) 0.3537(6) 0.0508(19) Uani 1.000000 . . .
C29 C 0.5853(9) -0.2406(6) 0.4574(6) 0.068(2) Uani 1.000000 . . .
H29 H 0.5279(9) -0.2655(6) 0.4819(6) 0.082(3) Uiso 1.000000 R . .
C30 C 0.7030(9) -0.2100(7) 0.5190(6) 0.079(3) Uani 1.000000 . . .
H30 H 0.7278(9) -0.2117(7) 0.5865(6) 0.095(3) Uiso 1.000000 R . .
C31 C 0.7925(8) -0.1744(7) 0.4840(6) 0.078(3) Uani 1.000000 . . .
H31 H 0.8759(8) -0.1521(7) 0.5286(6) 0.093(3) Uiso 1.000000 R . .
C32 C 0.7583(7) -0.1725(6) 0.3872(6) 0.0567(19) Uani 1.000000 . . .
H32 H 0.8188(7) -0.1504(6) 0.3655(6) 0.068(2) Uiso 1.000000 R . .
C33 C 0.6318(6) -0.2035(5) 0.3159(5) 0.0457(17) Uani 1.000000 . . .
C34 C 0.5922(6) -0.2043(5) 0.2134(5) 0.0430(17) Uani 1.000000 . . .
C35 C 0.4645(6) -0.2337(5) 0.1469(5) 0.0429(17) Uani 1.000000 . . .
C36 C 0.4198(7) -0.2339(5) 0.0435(6) 0.058(2) Uani 1.000000 . . .
H36 H 0.4751(7) -0.2135(5) 0.0165(6) 0.070(2) Uiso 1.000000 R . .
C37 C 0.2985(8) -0.2632(6) -0.0162(6) 0.069(2) Uani 1.000000 . . .
H37 H 0.2705(8) -0.2623(6) -0.0841(6) 0.083(3) Uiso 1.000000 R . .
C38 C 0.2122(7) -0.2955(6) 0.0238(7) 0.071(2) Uani 1.000000 . . .
H38 H 0.1282(7) -0.3172(6) -0.0184(7) 0.086(3) Uiso 1.000000 R . .
C39 C 0.2515(7) -0.2949(6) 0.1215(7) 0.065(2) Uani 1.000000 . . .
H39 H 0.1943(7) -0.3137(6) 0.1468(7) 0.078(3) Uiso 1.000000 R . .
C40 C 0.3788(6) -0.2661(5) 0.1877(6) 0.0495(18) Uani 1.000000 . . .
C41 C 0.4180(7) -0.2673(6) 0.2880(6) 0.057(2) Uani 1.000000 . . .
H41 H 0.3600(7) -0.2889(6) 0.3123(6) 0.069(2) Uiso 1.000000 R . .
C42 C 0.9129(7) 0.0834(5) 0.0577(5) 0.057(2) Uani 1.000000 . . .
H42a H 0.8296(14) 0.080(3) 0.0259(15) 0.085(3) Uiso 1.000000 GR . .
H42b H 0.969(3) 0.1566(14) 0.0668(6) 0.085(3) Uiso 1.000000 GR . .
H42c H 0.923(4) 0.032(2) 0.0160(12) 0.085(3) Uiso 1.000000 GR . .
C43 C 1.0730(6) 0.0531(5) 0.2101(6) 0.055(2) Uani 1.000000 . . .
H43a H 1.1312(7) 0.1242(12) 0.217(3) 0.083(3) Uiso 1.000000 GR . .
H43b H 1.0913(14) 0.037(3) 0.2754(13) 0.083(3) Uiso 1.000000 GR . .
H43c H 1.0786(12) -0.003(2) 0.1689(16) 0.083(3) Uiso 1.000000 GR . .
C44 C 1.0876(6) 0.4514(5) 0.3377(5) 0.0494(18) Uani 1.000000 D . .
C46 C 1.218(9) 0.467(19) 0.353(15) 0.11(2) Uani 0.48(6) D . 1
C47 C 1.022(4) 0.505(2) 0.256(2) 0.099(10) Uani 0.48(6) D U 1
C48 C 0.7554(6) -0.3540(5) 0.0005(5) 0.0497(18) Uani 1.000000 . . .
C49 C 0.8779(9) -0.3692(8) 0.0485(9) 0.136(5) Uani 1.000000 . . .
H49a H 0.9434(13) -0.303(3) 0.056(6) 0.204(7) Uiso 1.000000 GR . .
H49b H 0.892(4) -0.386(7) 0.113(3) 0.204(7) Uiso 1.000000 GR . .
H49c H 0.876(3) -0.429(5) 0.006(3) 0.204(7) Uiso 1.000000 GR . .
C50 C 0.7401(10) -0.3274(7) -0.1012(7) 0.112(4) Uani 1.000000 . . .
H50a H 0.663(3) -0.318(6) -0.135(2) 0.169(6) Uiso 1.000000 GR . .
H50b H 0.807(4) -0.261(3) -0.0909(8) 0.169(6) Uiso 1.000000 GR . .
H50c H 0.741(7) -0.387(3) -0.142(2) 0.169(6) Uiso 1.000000 GR . .
C51 C 0.6488(9) -0.4613(6) -0.0221(8) 0.115(4) Uani 1.000000 . . .
H51a H 0.650(4) -0.478(3) 0.0398(8) 0.173(6) Uiso 1.000000 GR . .
H51b H 0.5722(10) -0.454(2) -0.063(5) 0.173(6) Uiso 1.000000 GR . .
H51c H 0.657(4) -0.5200(14) -0.058(5) 0.173(6) Uiso 1.000000 GR . .
Br1 Br 0.5096(5) 0.4486(7) 0.3700(4) 0.154(2) Uani 0.492(9) D . 1
C52 C 0.6036(16) 0.5208(12) 0.3224(13) 0.085(6) Uani 0.492(9) D . 1
H52a H 0.5566(16) 0.5538(12) 0.2728(13) 0.102(7) Uiso 0.492(9) R . 1
H52b H 0.6708(16) 0.5812(12) 0.3768(13) 0.102(7) Uiso 0.492(9) R . 1
C45 C 1.110(12) 0.522(11) 0.431(5) 0.109(13) Uani 0.48(6) D . 1
Br2 Br 0.6787(6) 0.4482(7) 0.2595(4) 0.168(3) Uani 0.492(9) D . 1
Br1a Br 0.5209(7) 0.3893(7) 0.3603(5) 0.200(3) Uani 0.508(9) D . 2
C52a C 0.6189(19) 0.3862(13) 0.3077(18) 0.120(8) Uani 0.508(9) D . 2
H52c H 0.6782(19) 0.3572(13) 0.3500(18) 0.143(10) Uiso 0.508(9) R . 2
H52d H 0.5702(19) 0.3348(13) 0.2427(18) 0.143(10) Uiso 0.508(9) R . 2
Br2a Br 0.7080(6) 0.5249(6) 0.2900(5) 0.187(3) Uani 0.508(9) D . 2
C45a C 1.081(11) 0.519(10) 0.417(5) 0.109(13) Uani 0.52(6) D . 2
C46a C 1.222(8) 0.454(17) 0.376(14) 0.11(2) Uani 0.52(6) D . 2
C47a C 1.064(2) 0.4929(15) 0.2408(12) 0.059(8) Uani 0.52(6) D U 2
H46a H 1.267(10) 0.544(19) 0.37(2) 0.17(3) Uiso 0.48(6) GR . 1
H46b H 1.256(11) 0.43(2) 0.407(18) 0.17(3) Uiso 0.48(6) GR . 1
H46c H 1.213(9) 0.43(2) 0.292(16) 0.17(3) Uiso 0.48(6) GR . 1
H47a H 0.945(7) 0.499(10) 0.255(7) 0.149(15) Uiso 0.48(6) GR . 1
H47b H 1.073(7) 0.582(3) 0.270(6) 0.149(15) Uiso 0.48(6) GR . 1
H47c H 1.008(12) 0.469(8) 0.192(3) 0.149(15) Uiso 0.48(6) GR . 1
H45a H 1.15(2) 0.598(11) 0.433(9) 0.16(2) Uiso 0.48(6) GR . 1
H45b H 1.032(12) 0.512(17) 0.431(9) 0.16(2) Uiso 0.48(6) GR . 1
H45c H 1.160(18) 0.501(14) 0.488(5) 0.16(2) Uiso 0.48(6) GR . 1
H45d H 1.05(2) 0.473(11) 0.456(10) 0.16(2) Uiso 0.52(6) GR . 2
H45e H 1.161(11) 0.574(15) 0.460(10) 0.16(2) Uiso 0.52(6) GR . 2
H45f H 1.024(15) 0.555(14) 0.386(5) 0.16(2) Uiso 0.52(6) GR . 2
H46d H 1.279(8) 0.529(17) 0.400(17) 0.17(3) Uiso 0.52(6) GR . 2
H46e H 1.240(10) 0.42(2) 0.429(16) 0.17(3) Uiso 0.52(6) GR . 2
H46f H 1.229(9) 0.42(2) 0.321(14) 0.17(3) Uiso 0.52(6) GR . 2
H47d H 0.985(4) 0.499(7) 0.213(4) 0.088(12) Uiso 0.52(6) GR . 2
H47e H 1.127(5) 0.564(3) 0.2552(17) 0.088(12) Uiso 0.52(6) GR . 2
H47f H 1.066(8) 0.442(4) 0.193(3) 0.088(12) Uiso 0.52(6) GR . 2


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 1.379(6) . ?
O1 C13 1.379(6) . ?
C1 C2 1.378(8) . ?
C1 C6 1.386(8) . ?
C2 C3 1.392(8) . ?
C2 C20 1.491(8) . ?
C3 C4 1.402(8) . ?
C4 C5 1.384(8) . ?
C4 C44 1.518(8) . ?
C5 C6 1.393(7) . ?
C6 C7 1.509(8) . ?
C7 C8 1.524(8) . ?
C7 C42 1.539(9) . ?
C7 C43 1.546(8) . ?
C8 C9 1.398(7) . ?
C8 C13 1.375(8) . ?
C9 C10 1.404(8) . ?
C10 C11 1.388(8) . ?
C10 C48 1.504(8) . ?
C11 C12 1.394(8) . ?
C12 C13 1.391(8) . ?
C12 C34 1.498(8) . ?
C53 C15 1.440(10) . ?
C53 C19 1.441(9) . ?
C53 C27 1.394(9) . ?
C15 C16 1.321(11) . ?
C16 C17 1.427(11) . ?
C17 C18 1.349(10) . ?
C18 C19 1.426(9) . ?
C19 C20 1.401(9) . ?
C20 C21 1.404(9) . ?
C21 C22 1.409(10) . ?
C21 C26 1.447(9) . ?
C22 C23 1.341(10) . ?
C23 C24 1.435(12) . ?
C24 C25 1.297(11) . ?
C25 C26 1.412(10) . ?
C26 C27 1.382(10) . ?
C28 C29 1.429(10) . ?
C28 C33 1.437(9) . ?
C28 C41 1.390(9) . ?
C29 C30 1.311(10) . ?
C30 C31 1.411(11) . ?
C31 C32 1.335(10) . ?
C32 C33 1.429(9) . ?
C33 C34 1.402(9) . ?
C34 C35 1.427(9) . ?
C35 C36 1.412(9) . ?
C35 C40 1.428(9) . ?
C36 C37 1.343(10) . ?
C37 C38 1.426(10) . ?
C38 C39 1.335(10) . ?
C39 C40 1.422(10) . ?
C40 C41 1.378(10) . ?
C44 C46 1.54(3) . ?
C44 C47 1.53(2) . ?
C44 C45 1.48(3) . ?
C44 C45a 1.48(3) . ?
C44 C46a 1.56(3) . ?
C44 C47a 1.529(16) . ?
C48 C49 1.519(11) . ?
C48 C50 1.530(11) . ?
C48 C51 1.518(9) . ?
Br1 C52 1.710(14) . ?
C52 Br2 1.975(13) . ?
Br1a C52a 1.739(16) . ?
C52a Br2a 1.917(15) . ?

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
C13 O1 C1 119.5(4) . . ?
C2 C1 O1 115.2(5) . . ?
C6 C1 O1 122.0(5) . . ?
C6 C1 C2 122.8(5) . . ?
C3 C2 C1 117.9(5) . . ?
C20 C2 C1 122.5(5) . . ?
C20 C2 C3 119.6(5) . . ?
C4 C3 C2 122.7(6) . . ?
C5 C4 C3 115.7(5) . . ?
C44 C4 C3 121.8(6) . . ?
C44 C4 C5 122.5(5) . . ?
C6 C5 C4 124.4(5) . . ?
C5 C6 C1 116.5(5) . . ?
C7 C6 C1 123.0(5) . . ?
C7 C6 C5 120.4(5) . . ?
C8 C7 C6 110.1(5) . . ?
C42 C7 C6 109.3(5) . . ?
C42 C7 C8 108.9(5) . . ?
C43 C7 C6 109.6(5) . . ?
C43 C7 C8 109.1(5) . . ?
C43 C7 C42 109.7(5) . . ?
C9 C8 C7 120.0(5) . . ?
C13 C8 C7 122.5(5) . . ?
C13 C8 C9 117.4(5) . . ?
C10 C9 C8 123.4(6) . . ?
C11 C10 C9 115.9(5) . . ?
C48 C10 C9 120.3(5) . . ?
C48 C10 C11 123.7(6) . . ?
C12 C11 C10 122.9(6) . . ?
C13 C12 C11 118.2(5) . . ?
C34 C12 C11 119.8(5) . . ?
C34 C12 C13 122.0(5) . . ?
C8 C13 O1 122.7(5) . . ?
C12 C13 O1 115.1(5) . . ?
C12 C13 C8 122.2(5) . . ?
C19 C53 C15 117.3(7) . . ?
C27 C53 C15 122.9(7) . . ?
C27 C53 C19 119.8(7) . . ?
C16 C15 C53 122.0(7) . . ?
C17 C16 C15 121.8(8) . . ?
C18 C17 C16 118.2(8) . . ?
C19 C18 C17 123.2(7) . . ?
C18 C19 C53 117.6(7) . . ?
C20 C19 C53 119.1(7) . . ?
C20 C19 C18 123.3(6) . . ?
C19 C20 C2 119.7(6) . . ?
C21 C20 C2 119.6(6) . . ?
C21 C20 C19 120.7(6) . . ?
C22 C21 C20 124.2(6) . . ?
C26 C21 C20 119.6(7) . . ?
C26 C21 C22 116.3(7) . . ?
C23 C22 C21 123.1(7) . . ?
C24 C23 C22 118.9(8) . . ?
C25 C24 C23 120.7(8) . . ?
C26 C25 C24 122.5(7) . . ?
C25 C26 C21 118.5(7) . . ?
C27 C26 C21 119.2(7) . . ?
C27 C26 C25 122.3(7) . . ?
C26 C27 C53 121.6(7) . . ?
C33 C28 C29 118.3(7) . . ?
C41 C28 C29 122.5(7) . . ?
C41 C28 C33 119.2(7) . . ?
C30 C29 C28 121.9(8) . . ?
C31 C30 C29 120.6(8) . . ?
C32 C31 C30 120.4(8) . . ?
C33 C32 C31 122.1(7) . . ?
C32 C33 C28 116.5(6) . . ?
C34 C33 C28 119.7(7) . . ?
C34 C33 C32 123.8(6) . . ?
C33 C34 C12 120.5(6) . . ?
C35 C34 C12 118.6(6) . . ?
C35 C34 C33 120.7(6) . . ?
C36 C35 C34 123.0(6) . . ?
C40 C35 C34 117.7(6) . . ?
C40 C35 C36 119.3(6) . . ?
C37 C36 C35 120.8(7) . . ?
C38 C37 C36 120.3(8) . . ?
C39 C38 C37 120.4(7) . . ?
C40 C39 C38 121.5(7) . . ?
C39 C40 C35 117.7(7) . . ?
C41 C40 C35 121.4(7) . . ?
C41 C40 C39 120.9(7) . . ?
C40 C41 C28 121.3(6) . . ?
C46 C44 C4 113(8) . . ?
C47 C44 C4 107.5(11) . . ?
C47 C44 C46 114(6) . . ?
C45 C44 C4 116(6) . . ?
C45 C44 C46 104(10) . . ?
C45 C44 C47 102(5) . . ?
C45a C44 C4 112(6) . . ?
C45a C44 C46 116(10) . . ?
C45a C44 C47 93(4) . . ?
C45a C44 C45 13(8) . . ?
C46a C44 C4 107(7) . . ?
C46a C44 C46 14(11) . . ?
C46a C44 C47 128(5) . . ?
C46a C44 C45 97(9) . . ?
C46a C44 C45a 110(9) . . ?
C47a C44 C4 109.6(8) . . ?
C47a C44 C46 89(6) . . ?
C47a C44 C47 27.3(12) . . ?
C47a C44 C45 121(5) . . ?
C47a C44 C45a 116(5) . . ?
C47a C44 C46a 103(5) . . ?
C49 C48 C10 110.4(6) . . ?
C50 C48 C10 110.0(6) . . ?
C50 C48 C49 106.5(7) . . ?
C51 C48 C10 112.6(6) . . ?
C51 C48 C49 110.8(7) . . ?
C51 C48 C50 106.4(7) . . ?
Br2 C52 Br1 121.4(8) . . ?
Br2a C52a Br1a 116.0(9) . . ?

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 -178.4(5) . . . . ?
O1 C1 C2 C20 1.2(7) . . . . ?
O1 C1 C6 C5 179.0(6) . . . . ?
O1 C1 C6 C7 -1.8(7) . . . . ?
O1 C13 C8 C7 -3.4(7) . . . . ?
O1 C13 C8 C9 178.7(6) . . . . ?
O1 C13 C12 C11 -179.0(5) . . . . ?
O1 C13 C12 C34 2.6(7) . . . . ?
C1 C2 C3 C4 -0.6(7) . . . . ?
C1 C2 C20 C19 108.9(6) . . . . ?
C1 C2 C20 C21 -71.9(7) . . . . ?
C1 C6 C5 C4 -0.9(7) . . . . ?
C1 C6 C7 C8 0.5(7) . . . . ?
C1 C6 C7 C42 120.1(6) . . . . ?
C1 C6 C7 C43 -119.6(6) . . . . ?
C2 C3 C4 C5 0.8(7) . . . . ?
C2 C3 C4 C44 -179.5(6) . . . . ?
C2 C20 C19 C53 176.1(5) . . . . ?
C2 C20 C19 C18 -1.2(7) . . . . ?
C2 C20 C21 C22 2.9(7) . . . . ?
C2 C20 C21 C26 -176.4(5) . . . . ?
C3 C4 C5 C6 -0.0(7) . . . . ?
C3 C4 C44 C46 143(8) . . . . ?
C3 C4 C44 C47 -90(2) . . . . ?
C3 C4 C44 C45 23(5) . . . . ?
C3 C4 C44 C45a 10(4) . . . . ?
C3 C4 C44 C46a 130(7) . . . . ?
C3 C4 C44 C47a -119.2(15) . . . . ?
C4 C5 C6 C7 180.0(6) . . . . ?
C5 C6 C7 C8 179.6(5) . . . . ?
C5 C6 C7 C42 -60.8(6) . . . . ?
C5 C6 C7 C43 59.5(6) . . . . ?
C6 C7 C8 C9 179.9(5) . . . . ?
C6 C7 C8 C13 2.0(6) . . . . ?
C7 C8 C9 C10 -177.8(5) . . . . ?
C7 C8 C13 C12 178.9(6) . . . . ?
C8 C9 C10 C11 -1.1(7) . . . . ?
C8 C9 C10 C48 -180.0(6) . . . . ?
C8 C13 C12 C11 -1.1(7) . . . . ?
C8 C13 C12 C34 -179.5(6) . . . . ?
C9 C10 C11 C12 0.9(7) . . . . ?
C9 C10 C48 C49 61.7(8) . . . . ?
C9 C10 C48 C50 -55.5(7) . . . . ?
C9 C10 C48 C51 -173.9(7) . . . . ?
C10 C11 C12 C13 0.1(8) . . . . ?
C10 C11 C12 C34 178.6(6) . . . . ?
C11 C12 C34 C33 106.2(6) . . . . ?
C11 C12 C34 C35 -68.2(6) . . . . ?
C12 C34 C33 C28 -171.9(5) . . . . ?
C12 C34 C33 C32 7.2(7) . . . . ?
C12 C34 C35 C36 -6.8(6) . . . . ?
C12 C34 C35 C40 172.0(5) . . . . ?
C53 C15 C16 C17 -2.8(8) . . . . ?
C53 C19 C18 C17 0.0(7) . . . . ?
C53 C19 C20 C21 -3.1(7) . . . . ?
C53 C27 C26 C21 0.7(8) . . . . ?
C53 C27 C26 C25 -178.5(7) . . . . ?
C15 C16 C17 C18 1.6(9) . . . . ?
C16 C17 C18 C19 -0.2(9) . . . . ?
C17 C18 C19 C20 177.4(6) . . . . ?
C18 C19 C20 C21 179.6(6) . . . . ?
C19 C20 C21 C22 -177.9(6) . . . . ?
C19 C20 C21 C26 2.8(7) . . . . ?
C20 C21 C22 C23 -177.9(7) . . . . ?
C20 C21 C26 C25 177.7(6) . . . . ?
C20 C21 C26 C27 -1.6(7) . . . . ?
C21 C22 C23 C24 0.0(9) . . . . ?
C21 C26 C25 C24 0.5(8) . . . . ?
C22 C23 C24 C25 -1.4(10) . . . . ?
C23 C24 C25 C26 1.1(11) . . . . ?
C24 C25 C26 C27 179.7(8) . . . . ?
C28 C29 C30 C31 -1.7(9) . . . . ?
C28 C33 C32 C31 0.2(7) . . . . ?
C28 C33 C34 C35 2.4(7) . . . . ?
C28 C41 C40 C35 0.1(8) . . . . ?
C28 C41 C40 C39 -178.4(6) . . . . ?
C29 C30 C31 C32 -0.7(10) . . . . ?
C30 C31 C32 C33 1.4(10) . . . . ?
C31 C32 C33 C34 -178.9(7) . . . . ?
C32 C33 C34 C35 -178.5(6) . . . . ?
C33 C34 C35 C36 178.8(6) . . . . ?
C33 C34 C35 C40 -2.4(6) . . . . ?
C34 C35 C36 C37 179.4(6) . . . . ?
C34 C35 C40 C39 179.7(6) . . . . ?
C34 C35 C40 C41 1.1(7) . . . . ?
C35 C36 C37 C38 -0.5(8) . . . . ?
C35 C40 C39 C38 2.3(7) . . . . ?
C36 C37 C38 C39 1.4(9) . . . . ?
C37 C38 C39 C40 -2.3(9) . . . . ?
C38 C39 C40 C41 -179.1(7) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
C52 Br1 1 1.9400 0.0200 0.2304
C52 Br2 1 1.9400 0.0200 -0.0355
C52a Br1a 1 1.9400 0.0200 0.2008
C52a Br2a 1 1.9400 0.0200 0.0234

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_id
C44 C46 1 2
C44 C47 1 3
C44 C45 1 4
C44 C45a 1 4
C44 C46a 1 2
C44 C47a 1 3
Br1 Br2 1 1
Br1a Br2a 1 1

loop_
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
_restr_equal_distance_class_average
_restr_equal_distance_class_esd
_restr_equal_distance_class_diff_max
1 0.0400 3.1587 0.0569 0.0569
2 0.0200 1.5487 0.0136 0.0136
3 0.0200 1.5283 0.0005 0.0005
4 0.0200 1.4839 0.0001 0.0001

loop_
_restr_U_iso_atom_site_label
_restr_U_iso_weight_param
C47 0.0100
C47a 0.0100

####################################################################### 
# 
# 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_20220506-lqy318k
_database_code_depnum_ccdc_archive 'CCDC 2180372'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/D3SC05533G 2024
loop_
_audit_author_name
_audit_author_address
'Qiuyan Liao'
;Wuhan University
China
;
_audit_update_record             
;
2022-06-20 deposited with the CCDC.	2024-02-14 downloaded from the CCDC.
;
_audit_creation_date             2022-05-31
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H4 Cl2, C51 H46 O'
_chemical_formula_sum            'C53 H50 Cl2 O'
_chemical_formula_weight         773.83
_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'
Cl Cl 0.3639 0.7018 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.84138(18)
_cell_length_b                   13.04491(19)
_cell_length_c                   15.1875(2)
_cell_angle_alpha                94.0644(12)
_cell_angle_beta                 114.2372(15)
_cell_angle_gamma                108.4420(13)
_cell_volume                     2140.65(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16000
_cell_measurement_temperature    318.00(10)
_cell_measurement_theta_max      66.5350
_cell_measurement_theta_min      3.2390
_shelx_estimated_absorpt_T_max   0.853
_shelx_estimated_absorpt_T_min   0.791
_exptl_absorpt_coefficient_mu    1.643
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25395
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.598
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_min         3.281
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      318.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     30.00  62.00   0.50    0.30    --   62.89-125.00  60.00   64
  2  ω     46.00  71.00   0.50    0.30    --   76.75-125.00  60.00   50
  3  ω     72.00  98.00   0.50    0.30    --   76.75-125.00  90.00   52
  4  ω     67.00  98.00   0.50    0.30    --   76.75-125.00  30.00   62
  5  ω     22.00  67.00   0.50    0.30    --   62.89-125.00 -30.00   90
  6  ω     44.00  98.00   0.50    0.30    --   76.75-125.00-180.00  108
  7  ω     45.00  98.00   0.50    0.30    --   76.75-125.00 -60.00  106
  8  ω     55.00  95.00   0.50    0.30    --   62.89  15.00 150.00   80
  9  ω     52.00 102.00   0.50    0.30    --   62.89  15.00  30.00  100
 10  ω   -101.00 -48.00   0.50    0.30    --  -81.49 125.00  30.00  106
 11  ω    -73.00 -42.00   0.50    0.30    --  -71.74 125.00 150.00   62
 12  ω    -73.00 -47.00   0.50    0.30    --  -76.43 125.00  60.00   52
 13  ω    -65.00 -39.00   0.50    0.30    --  -81.49 125.00  60.00   52
 14  ω    -75.00 -29.00   0.50    0.30    --  -71.74 125.00   0.00   92
 15  ω   -101.00 -72.00   0.50    0.30    --  -81.49 125.00  60.00   58
 16  ω    -74.00 -48.00   0.50    0.30    --  -76.43 125.00 -90.00   52
 17  ω   -102.00 -48.00   0.50    0.30    --  -81.49 125.00 -90.00  108
 18  ω   -102.00 -53.00   0.50    0.30    --  -81.49 125.00-120.00   98
 19  ω    -97.00 -34.00   0.50    0.30    --  -76.43 125.00-180.00  126
 20  ω   -101.00 -57.00   0.50    0.30    --  -81.49 125.00-180.00   88
 21  ω   -102.00 -76.00   0.50    0.30    --  -81.49 125.00-150.00   52
 22  ω    -72.00 -39.00   0.50    0.30    --  -81.49 125.00 -60.00   66
 23  ω   -102.00 -76.00   0.50    0.30    --  -81.49 125.00 -60.00   52
 24  ω   -102.00 -74.00   0.50    0.30    --  -81.49 125.00   0.00   56
 25  ω   -101.00 -76.00   0.50    0.30    --  -81.49 125.00  90.00   50
 26  ω    -77.00 -43.00   0.50    0.30    --  -81.49 125.00 120.00   68
 27  ω   -102.00 -72.00   0.50    0.30    --  -81.49 125.00 150.00   60
 28  ω   -101.00 -56.00   0.50    0.30    --  -63.72 -15.00 120.00   90
 29  ω    -95.00 -69.00   0.50    0.30    --  -71.74 -15.00  90.00   52
 30  ω   -101.00 -62.00   0.50    0.30    --  -71.74 -15.00 -90.00   78
 31  ω   -101.00 -70.00   0.50    0.30    --  -71.74 -15.00-120.00   62
 32  ω   -107.00 -56.00   0.50    0.30    --  -63.72 -15.00-180.00  102
 33  ω    -89.00 -63.00   0.50    0.30    --  -71.74 -15.00-150.00   52
 34  ω   -120.00 -77.00   0.50    0.30    --  -76.43 -15.00 -30.00   86
 35  ω   -104.00 -75.00   0.50    0.30    --  -81.49 -15.00-150.00   58
 36  ω   -123.00 -82.00   0.50    0.30    --  -81.49 -15.00   0.00   82
 37  ω   -113.00 -66.00   0.50    0.30    --  -76.43 -15.00  30.00   94
 38  ω   -125.00 -77.00   0.50    0.30    --  -81.49 -15.00  90.00   96
 39  ω   -125.00 -76.00   0.50    0.30    --  -81.49 -15.00 150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0609592000
_diffrn_orient_matrix_UB_12      0.0629762000
_diffrn_orient_matrix_UB_13      -0.0592412000
_diffrn_orient_matrix_UB_21      0.0799107000
_diffrn_orient_matrix_UB_22      -0.0703387000
_diffrn_orient_matrix_UB_23      0.0170115000
_diffrn_orient_matrix_UB_31      -0.1006246000
_diffrn_orient_matrix_UB_32      -0.0864081000
_diffrn_orient_matrix_UB_33      -0.0963339000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6448
_reflns_number_total             7502
_reflns_odcompleteness_completeness 98.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7502
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0578
_refine_ls_restrained_S_all      1.085
_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)+(0.0970P)²+0.4640P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.1764
_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. Restrained distances
 C52-C53
 1.54 with sigma of 0.02
 C53-Cl2
 1.78 with sigma of 0.02
 C52-Cl1
 1.78 with sigma of 0.02
 C52A-Cl1A
 1.78 with sigma of 0.02
 C53A-Cl2A
 1.78 with sigma of 0.02
 C52A-C53A
 1.54 with sigma of 0.02
3. Others
 Sof(Cl2A)=Sof(C53A)=Sof(H53C)=Sof(H53D)=Sof(C52A)=Sof(H52C)=Sof(H52D)=
 Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C53)=Sof(H53A)=Sof(H53B)=
 FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C53(H53A,H53B), C53A(H53C,H53D), C52A(H52C,H52D)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C5(H5), C10(H10), C20(H20), C39(H39), C34(H34), C15(H15),
 C36(H36), C25(H25), C29(H29), C18(H18), C38(H38), C37(H37), C32(H32), C17(H17),
  C22(H22), C16(H16), C24(H24), C31(H31), C30(H30), C23(H23)
4.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C47(H47A,H47B,H47C), C51(H51A,H51B,
 H51C), C49(H49A,H49B,H49C), C46(H46A,H46B,H46C), C45(H45A,H45B,H45C), C50(H50A,
 H50B,H50C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Cl1 Cl 0.0216(5) 0.1109(7) 0.6277(4) 0.201(3) Uani 0.519(10) 1 d D . P A 1
O1 O 0.73435(10) 0.49647(8) 0.75491(9) 0.0510(3) Uani 1 1 d . . . . .
Cl2 Cl -0.2408(6) -0.0263(5) 0.7272(6) 0.171(2) Uani 0.519(10) 1 d D . P A 1
C2 C 0.81918(14) 0.68462(12) 0.83309(12) 0.0449(4) Uani 1 1 d . . . . .
C12 C 0.65262(14) 0.38915(11) 0.73386(11) 0.0421(3) Uani 1 1 d . . . . .
C6 C 0.65026(14) 0.55998(12) 0.85519(11) 0.0416(3) Uani 1 1 d . . . . .
C11 C 0.66147(14) 0.31103(12) 0.67263(12) 0.0437(3) Uani 1 1 d . . . . .
C7 C 0.56691(14) 0.35949(12) 0.77020(11) 0.0413(3) Uani 1 1 d . . . . .
C1 C 0.73234(14) 0.57880(12) 0.81490(12) 0.0427(3) Uani 1 1 d . . . . .
C3 C 0.82225(15) 0.77216(12) 0.89318(12) 0.0483(4) Uani 1 1 d . . . . .
H3 H 0.880212 0.842889 0.905896 0.058 Uiso 1 1 calc R U . . .
C8 C 0.49008(14) 0.24795(12) 0.74390(12) 0.0441(4) Uani 1 1 d . . . . .
H8 H 0.432460 0.226875 0.767999 0.053 Uiso 1 1 calc R U . . .
C9 C 0.49508(14) 0.16662(12) 0.68357(12) 0.0451(4) Uani 1 1 d . . . . .
C27 C 0.75377(15) 0.34361(12) 0.63327(12) 0.0446(4) Uani 1 1 d . . . . .
C28 C 0.88036(15) 0.37358(13) 0.69766(13) 0.0499(4) Uani 1 1 d . . . . .
C13 C 0.90930(15) 0.70593(11) 0.79124(12) 0.0456(4) Uani 1 1 d . . . . .
C5 C 0.65730(14) 0.65057(12) 0.91420(12) 0.0443(4) Uani 1 1 d . . . . .
H5 H 0.602562 0.638876 0.941280 0.053 Uiso 1 1 calc R U . . .
C4 C 0.74188(15) 0.75800(12) 0.93504(12) 0.0459(4) Uani 1 1 d . . . . .
C41 C 0.55605(14) 0.44414(11) 0.83722(11) 0.0418(3) Uani 1 1 d . . . . .
C14 C 1.03556(15) 0.73497(12) 0.85561(13) 0.0485(4) Uani 1 1 d . . . . .
C40 C 0.71282(16) 0.33976(12) 0.53122(13) 0.0472(4) Uani 1 1 d . . . . .
C26 C 0.86875(16) 0.70308(13) 0.68922(13) 0.0513(4) Uani 1 1 d . . . . .
C10 C 0.58236(15) 0.20076(12) 0.64867(12) 0.0467(4) Uani 1 1 d . . . . .
H10 H 0.587859 0.148061 0.608031 0.056 Uiso 1 1 calc R U . . .
C42 C 0.42569(15) 0.44425(14) 0.78907(15) 0.0573(4) Uani 1 1 d . . . . .
H42A H 0.367083 0.371649 0.779138 0.086 Uiso 1 1 calc R U . . .
H42B H 0.408756 0.463704 0.726222 0.086 Uiso 1 1 calc R U . . .
H42C H 0.419295 0.497461 0.831589 0.086 Uiso 1 1 calc R U . . .
C19 C 1.12354(16) 0.76633(13) 0.81723(15) 0.0555(4) Uani 1 1 d . . . . .
C33 C 0.96717(17) 0.39754(15) 0.65810(15) 0.0575(4) Uani 1 1 d . . . . .
C35 C 0.80165(18) 0.36454(13) 0.49314(14) 0.0541(4) Uani 1 1 d . . . . .
C44 C 0.74355(17) 0.85364(13) 1.00093(13) 0.0536(4) Uani 1 1 d . . . . .
C21 C 0.95833(18) 0.73592(15) 0.65252(14) 0.0584(4) Uani 1 1 d . . . . .
C48 C 0.40833(16) 0.04495(12) 0.65888(13) 0.0535(4) Uani 1 1 d . . . . .
C20 C 1.08248(18) 0.76730(15) 0.71756(15) 0.0619(5) Uani 1 1 d . . . . .
H20 H 1.140056 0.789710 0.693542 0.074 Uiso 1 1 calc R U . . .
C39 C 0.58681(18) 0.31182(15) 0.46253(14) 0.0600(4) Uani 1 1 d . . . . .
H39 H 0.527897 0.296795 0.485501 0.072 Uiso 1 1 calc R U . . .
C43 C 0.58296(19) 0.41191(14) 0.93781(13) 0.0571(4) Uani 1 1 d . . . . .
H43A H 0.576358 0.464647 0.980598 0.086 Uiso 1 1 calc R U . . .
H43B H 0.664900 0.411884 0.968033 0.086 Uiso 1 1 calc R U . . .
H43C H 0.524356 0.339127 0.927391 0.086 Uiso 1 1 calc R U . . .
C34 C 0.92540(18) 0.39223(15) 0.55728(15) 0.0606(5) Uani 1 1 d . . . . .
H34 H 0.982065 0.407692 0.532006 0.073 Uiso 1 1 calc R U . . .
C15 C 1.08248(18) 0.73596(15) 0.95869(15) 0.0616(5) Uani 1 1 d . . . . .
H15 H 1.027666 0.715279 0.985508 0.074 Uiso 1 1 calc R U . . .
C36 C 0.7586(2) 0.35793(16) 0.38916(16) 0.0667(5) Uani 1 1 d . . . . .
H36 H 0.815198 0.373527 0.363823 0.080 Uiso 1 1 calc R U . . .
C25 C 0.74233(19) 0.67128(18) 0.61945(15) 0.0673(5) Uani 1 1 d . . . . .
H25 H 0.682172 0.649462 0.640920 0.081 Uiso 1 1 calc R U . . .
C29 C 0.92769(18) 0.37929(17) 0.80156(15) 0.0645(5) Uani 1 1 d . . . . .
H29 H 0.873581 0.364610 0.829321 0.077 Uiso 1 1 calc R U . . .
C18 C 1.25160(19) 0.79803(17) 0.88384(19) 0.0710(6) Uani 1 1 d . . . . .
H18 H 1.309164 0.819043 0.859685 0.085 Uiso 1 1 calc R U . . .
C38 C 0.5505(2) 0.30658(18) 0.36391(16) 0.0722(5) Uani 1 1 d . . . . .
H38 H 0.467490 0.287702 0.320497 0.087 Uiso 1 1 calc R U . . .
C37 C 0.6387(2) 0.32980(18) 0.32728(16) 0.0734(6) Uani 1 1 d . . . . .
H37 H 0.613167 0.325484 0.259811 0.088 Uiso 1 1 calc R U . . .
C32 C 1.09436(19) 0.4233(2) 0.72342(19) 0.0780(6) Uani 1 1 d . . . . .
H32 H 1.150978 0.437889 0.698113 0.094 Uiso 1 1 calc R U . . .
C17 C 1.2906(2) 0.79812(19) 0.9806(2) 0.0775(6) Uani 1 1 d . . . . .
H17 H 1.374413 0.819296 1.022471 0.093 Uiso 1 1 calc R U . . .
C22 C 0.9168(2) 0.7373(2) 0.55034(17) 0.0778(6) Uani 1 1 d . . . . .
H22 H 0.974496 0.760000 0.526457 0.093 Uiso 1 1 calc R U . . .
C16 C 1.2052(2) 0.76634(18) 1.01878(18) 0.0746(6) Uani 1 1 d . . . . .
H16 H 1.232977 0.766132 1.085749 0.089 Uiso 1 1 calc R U . . .
C47 C 0.8532(3) 0.96078(16) 1.0264(2) 0.0940(8) Uani 1 1 d . . . . .
H47A H 0.928306 0.947617 1.056412 0.141 Uiso 1 1 calc R U . . .
H47B H 0.854554 1.016704 1.071911 0.141 Uiso 1 1 calc R U . . .
H47C H 0.846031 0.985597 0.966888 0.141 Uiso 1 1 calc R U . . .
C51 C 0.4070(3) -0.02663(17) 0.5746(2) 0.0896(8) Uani 1 1 d . . . . .
H51A H 0.346436 -0.100228 0.557851 0.134 Uiso 1 1 calc R U . . .
H51B H 0.486944 -0.030003 0.595087 0.134 Uiso 1 1 calc R U . . .
H51C H 0.386681 0.005159 0.517677 0.134 Uiso 1 1 calc R U . . .
C24 C 0.7079(2) 0.6721(2) 0.52261(17) 0.0870(7) Uani 1 1 d . . . . .
H24 H 0.624619 0.649531 0.478446 0.104 Uiso 1 1 calc R U . . .
C49 C 0.2756(2) 0.03667(19) 0.6264(2) 0.0971(9) Uani 1 1 d . . . . .
H49A H 0.250593 0.069484 0.570514 0.146 Uiso 1 1 calc R U . . .
H49B H 0.271398 0.075354 0.680237 0.146 Uiso 1 1 calc R U . . .
H49C H 0.221744 -0.040015 0.608091 0.146 Uiso 1 1 calc R U . . .
C46 C 0.7559(3) 0.82429(19) 1.09966(17) 0.0889(7) Uani 1 1 d . . . . .
H46A H 0.686007 0.759098 1.087486 0.133 Uiso 1 1 calc R U . . .
H46B H 0.759261 0.885087 1.141651 0.133 Uiso 1 1 calc R U . . .
H46C H 0.830172 0.810299 1.131727 0.133 Uiso 1 1 calc R U . . .
C31 C 1.1337(2) 0.4270(2) 0.8207(2) 0.0918(8) Uani 1 1 d . . . . .
H31 H 1.216864 0.443676 0.861936 0.110 Uiso 1 1 calc R U . . .
C30 C 1.0493(2) 0.4055(2) 0.86082(18) 0.0848(7) Uani 1 1 d . . . . .
H30 H 1.077623 0.409483 0.928487 0.102 Uiso 1 1 calc R U . . .
C23 C 0.7968(3) 0.7069(2) 0.48769(18) 0.0904(7) Uani 1 1 d . . . . .
H23 H 0.772069 0.708626 0.421220 0.109 Uiso 1 1 calc R U . . .
C45 C 0.6235(3) 0.8701(2) 0.9502(2) 0.1124(11) Uani 1 1 d . . . . .
H45A H 0.616222 0.892425 0.889690 0.169 Uiso 1 1 calc R U . . .
H45B H 0.622014 0.926603 0.993162 0.169 Uiso 1 1 calc R U . . .
H45C H 0.555862 0.801691 0.935282 0.169 Uiso 1 1 calc R U . . .
C50 C 0.4486(3) -0.00070(19) 0.7500(2) 0.1089(10) Uani 1 1 d . . . . .
H50A H 0.398194 -0.078190 0.733868 0.163 Uiso 1 1 calc R U . . .
H50B H 0.439824 0.038591 0.800738 0.163 Uiso 1 1 calc R U . . .
H50C H 0.533411 0.008359 0.773435 0.163 Uiso 1 1 calc R U . . .
C52 C -0.0791(7) 0.1018(6) 0.6683(6) 0.090(2) Uani 0.519(10) 1 d D . P A 1
H52A H -0.040569 0.159347 0.728548 0.108 Uiso 0.519(10) 1 calc R U P A 1
H52B H -0.146514 0.116956 0.619423 0.108 Uiso 0.519(10) 1 calc R U P A 1
C53 C -0.1324(10) -0.0091(9) 0.6903(9) 0.112(3) Uani 0.519(10) 1 d D . P A 1
H53A H -0.064736 -0.022065 0.741114 0.134 Uiso 0.519(10) 1 calc R U P A 1
H53B H -0.166425 -0.066480 0.630778 0.134 Uiso 0.519(10) 1 calc R U P A 1
Cl2A Cl -0.2132(9) 0.0316(9) 0.7569(7) 0.199(3) Uani 0.481(10) 1 d D . P A 2
C53A C -0.1253(11) 0.0826(10) 0.7016(8) 0.155(5) Uani 0.481(10) 1 d D . P A 2
H53C H -0.173823 0.104053 0.643450 0.187 Uiso 0.481(10) 1 calc R U P A 2
H53D H -0.056629 0.149434 0.746785 0.187 Uiso 0.481(10) 1 calc R U P A 2
C52A C -0.0754(12) 0.0078(10) 0.6707(9) 0.150(6) Uani 0.481(10) 1 d D . P A 2
H52C H -0.141839 -0.056575 0.620136 0.180 Uiso 0.481(10) 1 calc R U P A 2
H52D H -0.028492 -0.017286 0.726903 0.180 Uiso 0.481(10) 1 calc R U P A 2
Cl1A Cl 0.0211(3) 0.0853(6) 0.6231(3) 0.1515(18) Uani 0.481(10) 1 d D . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C52 1.623(8) . ?
O1 C12 1.3767(17) . ?
O1 C1 1.3720(17) . ?
Cl2 C53 1.662(10) . ?
C2 C1 1.394(2) . ?
C2 C3 1.390(2) . ?
C2 C13 1.499(2) . ?
C12 C11 1.394(2) . ?
C12 C7 1.387(2) . ?
C6 C1 1.390(2) . ?
C6 C5 1.387(2) . ?
C6 C41 1.5282(19) . ?
C11 C27 1.497(2) . ?
C11 C10 1.390(2) . ?
C7 C8 1.391(2) . ?
C7 C41 1.526(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.392(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.387(2) . ?
C9 C10 1.393(2) . ?
C9 C48 1.535(2) . ?
C27 C28 1.411(2) . ?
C27 C40 1.409(2) . ?
C28 C33 1.434(2) . ?
C28 C29 1.426(3) . ?
C13 C14 1.409(2) . ?
C13 C26 1.411(2) . ?
C5 H5 0.9300 . ?
C5 C4 1.391(2) . ?
C4 C44 1.532(2) . ?
C41 C42 1.528(2) . ?
C41 C43 1.543(2) . ?
C14 C19 1.437(2) . ?
C14 C15 1.425(3) . ?
C40 C35 1.440(2) . ?
C40 C39 1.424(3) . ?
C26 C21 1.437(2) . ?
C26 C25 1.425(3) . ?
C10 H10 0.9300 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C19 C20 1.386(3) . ?
C19 C18 1.429(3) . ?
C33 C34 1.387(3) . ?
C33 C32 1.428(3) . ?
C35 C34 1.386(3) . ?
C35 C36 1.428(3) . ?
C44 C47 1.522(3) . ?
C44 C46 1.531(3) . ?
C44 C45 1.508(3) . ?
C21 C20 1.386(3) . ?
C21 C22 1.423(3) . ?
C48 C51 1.521(3) . ?
C48 C49 1.531(3) . ?
C48 C50 1.503(3) . ?
C20 H20 0.9300 . ?
C39 H39 0.9300 . ?
C39 C38 1.363(3) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C34 H34 0.9300 . ?
C15 H15 0.9300 . ?
C15 C16 1.358(3) . ?
C36 H36 0.9300 . ?
C36 C37 1.339(3) . ?
C25 H25 0.9300 . ?
C25 C24 1.353(3) . ?
C29 H29 0.9300 . ?
C29 C30 1.353(3) . ?
C18 H18 0.9300 . ?
C18 C17 1.343(3) . ?
C38 H38 0.9300 . ?
C38 C37 1.418(3) . ?
C37 H37 0.9300 . ?
C32 H32 0.9300 . ?
C32 C31 1.343(3) . ?
C17 H17 0.9300 . ?
C17 C16 1.407(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.339(3) . ?
C16 H16 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C24 H24 0.9300 . ?
C24 C23 1.412(3) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C31 H31 0.9300 . ?
C31 C30 1.413(3) . ?
C30 H30 0.9300 . ?
C23 H23 0.9300 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 C53 1.518(11) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
Cl2A C53A 1.674(14) . ?
C53A H53C 0.9700 . ?
C53A H53D 0.9700 . ?
C53A C52A 1.469(14) . ?
C52A H52C 0.9700 . ?
C52A H52D 0.9700 . ?
C52A Cl1A 1.768(13) . ?

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 C12 119.10(11) . . ?
C1 C2 C13 122.13(13) . . ?
C3 C2 C1 118.29(14) . . ?
C3 C2 C13 119.57(13) . . ?
O1 C12 C11 115.15(12) . . ?
O1 C12 C7 123.13(13) . . ?
C7 C12 C11 121.71(13) . . ?
C1 C6 C41 122.06(12) . . ?
C5 C6 C1 117.60(13) . . ?
C5 C6 C41 120.33(13) . . ?
C12 C11 C27 121.48(13) . . ?
C10 C11 C12 118.40(13) . . ?
C10 C11 C27 120.13(13) . . ?
C12 C7 C8 117.46(13) . . ?
C12 C7 C41 122.30(12) . . ?
C8 C7 C41 120.24(13) . . ?
O1 C1 C2 115.17(13) . . ?
O1 C1 C6 123.30(12) . . ?
C6 C1 C2 121.53(13) . . ?
C2 C3 H3 118.7 . . ?
C2 C3 C4 122.52(13) . . ?
C4 C3 H3 118.7 . . ?
C7 C8 H8 118.3 . . ?
C9 C8 C7 123.31(14) . . ?
C9 C8 H8 118.3 . . ?
C8 C9 C10 117.00(13) . . ?
C8 C9 C48 120.31(14) . . ?
C10 C9 C48 122.69(13) . . ?
C28 C27 C11 119.91(14) . . ?
C40 C27 C11 119.58(14) . . ?
C40 C27 C28 120.46(14) . . ?
C27 C28 C33 119.50(16) . . ?
C27 C28 C29 123.19(15) . . ?
C29 C28 C33 117.29(16) . . ?
C14 C13 C2 119.36(15) . . ?
C14 C13 C26 120.44(14) . . ?
C26 C13 C2 120.10(15) . . ?
C6 C5 H5 118.3 . . ?
C6 C5 C4 123.50(14) . . ?
C4 C5 H5 118.3 . . ?
C3 C4 C44 123.19(13) . . ?
C5 C4 C3 116.55(13) . . ?
C5 C4 C44 120.26(14) . . ?
C6 C41 C43 108.75(12) . . ?
C7 C41 C6 110.10(11) . . ?
C7 C41 C42 109.81(13) . . ?
C7 C41 C43 108.76(13) . . ?
C42 C41 C6 109.88(12) . . ?
C42 C41 C43 109.52(14) . . ?
C13 C14 C19 119.38(16) . . ?
C13 C14 C15 123.44(15) . . ?
C15 C14 C19 117.19(16) . . ?
C27 C40 C35 119.09(16) . . ?
C27 C40 C39 123.31(15) . . ?
C39 C40 C35 117.60(16) . . ?
C13 C26 C21 119.25(16) . . ?
C13 C26 C25 123.44(15) . . ?
C25 C26 C21 117.29(17) . . ?
C11 C10 C9 122.12(14) . . ?
C11 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C20 C19 C14 119.34(16) . . ?
C20 C19 C18 121.88(17) . . ?
C18 C19 C14 118.77(18) . . ?
C34 C33 C28 119.42(17) . . ?
C34 C33 C32 121.63(17) . . ?
C32 C33 C28 118.93(18) . . ?
C34 C35 C40 119.63(16) . . ?
C34 C35 C36 121.82(17) . . ?
C36 C35 C40 118.55(18) . . ?
C47 C44 C4 112.17(15) . . ?
C47 C44 C46 106.49(18) . . ?
C46 C44 C4 109.48(15) . . ?
C45 C44 C4 109.28(16) . . ?
C45 C44 C47 111.0(2) . . ?
C45 C44 C46 108.3(2) . . ?
C20 C21 C26 119.41(17) . . ?
C20 C21 C22 121.82(17) . . ?
C22 C21 C26 118.76(18) . . ?
C51 C48 C9 112.33(14) . . ?
C51 C48 C49 107.06(18) . . ?
C49 C48 C9 110.29(15) . . ?
C50 C48 C9 109.04(16) . . ?
C50 C48 C51 109.3(2) . . ?
C50 C48 C49 108.8(2) . . ?
C19 C20 C21 122.10(16) . . ?
C19 C20 H20 119.0 . . ?
C21 C20 H20 119.0 . . ?
C40 C39 H39 119.2 . . ?
C38 C39 C40 121.55(18) . . ?
C38 C39 H39 119.2 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C33 C34 H34 119.1 . . ?
C35 C34 C33 121.88(15) . . ?
C35 C34 H34 119.1 . . ?
C14 C15 H15 119.1 . . ?
C16 C15 C14 121.71(18) . . ?
C16 C15 H15 119.1 . . ?
C35 C36 H36 119.2 . . ?
C37 C36 C35 121.60(19) . . ?
C37 C36 H36 119.2 . . ?
C26 C25 H25 119.3 . . ?
C24 C25 C26 121.38(19) . . ?
C24 C25 H25 119.3 . . ?
C28 C29 H29 119.2 . . ?
C30 C29 C28 121.68(18) . . ?
C30 C29 H29 119.2 . . ?
C19 C18 H18 119.3 . . ?
C17 C18 C19 121.42(19) . . ?
C17 C18 H18 119.3 . . ?
C39 C38 H38 119.9 . . ?
C39 C38 C37 120.2(2) . . ?
C37 C38 H38 119.9 . . ?
C36 C37 C38 120.46(19) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C33 C32 H32 119.4 . . ?
C31 C32 C33 121.19(19) . . ?
C31 C32 H32 119.4 . . ?
C18 C17 H17 119.8 . . ?
C18 C17 C16 120.3(2) . . ?
C16 C17 H17 119.8 . . ?
C21 C22 H22 119.2 . . ?
C23 C22 C21 121.7(2) . . ?
C23 C22 H22 119.2 . . ?
C15 C16 C17 120.6(2) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C48 C51 H51A 109.5 . . ?
C48 C51 H51B 109.5 . . ?
C48 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C25 C24 H24 119.5 . . ?
C25 C24 C23 120.9(2) . . ?
C23 C24 H24 119.5 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C32 C31 H31 119.8 . . ?
C32 C31 C30 120.4(2) . . ?
C30 C31 H31 119.8 . . ?
C29 C30 C31 120.5(2) . . ?
C29 C30 H30 119.7 . . ?
C31 C30 H30 119.7 . . ?
C22 C23 C24 119.9(2) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
Cl1 C52 H52A 108.4 . . ?
Cl1 C52 H52B 108.4 . . ?
H52A C52 H52B 107.5 . . ?
C53 C52 Cl1 115.5(7) . . ?
C53 C52 H52A 108.4 . . ?
C53 C52 H52B 108.4 . . ?
Cl2 C53 H53A 107.8 . . ?
Cl2 C53 H53B 107.8 . . ?
C52 C53 Cl2 118.1(8) . . ?
C52 C53 H53A 107.8 . . ?
C52 C53 H53B 107.8 . . ?
H53A C53 H53B 107.1 . . ?
Cl2A C53A H53C 108.2 . . ?
Cl2A C53A H53D 108.2 . . ?
H53C C53A H53D 107.4 . . ?
C52A C53A Cl2A 116.2(11) . . ?
C52A C53A H53C 108.2 . . ?
C52A C53A H53D 108.2 . . ?
C53A C52A H52C 110.4 . . ?
C53A C52A H52D 110.4 . . ?
C53A C52A Cl1A 106.5(10) . . ?
H52C C52A H52D 108.6 . . ?
Cl1A C52A H52C 110.4 . . ?
Cl1A C52A H52D 110.4 . . ?

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
Cl1 C52 C53 Cl2 -177.2(7) . . . . ?
O1 C12 C11 C27 -0.2(2) . . . . ?
O1 C12 C11 C10 179.60(14) . . . . ?
O1 C12 C7 C8 -179.58(14) . . . . ?
O1 C12 C7 C41 0.0(2) . . . . ?
C2 C3 C4 C5 0.3(3) . . . . ?
C2 C3 C4 C44 -179.65(16) . . . . ?
C2 C13 C14 C19 -173.75(13) . . . . ?
C2 C13 C14 C15 5.8(2) . . . . ?
C2 C13 C26 C21 173.04(14) . . . . ?
C2 C13 C26 C25 -5.6(2) . . . . ?
C12 O1 C1 C2 179.31(14) . . . . ?
C12 O1 C1 C6 -0.8(2) . . . . ?
C12 C11 C27 C28 71.8(2) . . . . ?
C12 C11 C27 C40 -110.74(17) . . . . ?
C12 C11 C10 C9 0.2(3) . . . . ?
C12 C7 C8 C9 -0.3(2) . . . . ?
C12 C7 C41 C6 0.3(2) . . . . ?
C12 C7 C41 C42 121.42(16) . . . . ?
C12 C7 C41 C43 -118.75(16) . . . . ?
C6 C5 C4 C3 0.0(3) . . . . ?
C6 C5 C4 C44 179.95(15) . . . . ?
C11 C12 C7 C8 0.5(2) . . . . ?
C11 C12 C7 C41 -179.93(14) . . . . ?
C11 C27 C28 C33 175.89(14) . . . . ?
C11 C27 C28 C29 -2.7(2) . . . . ?
C11 C27 C40 C35 -176.14(13) . . . . ?
C11 C27 C40 C39 3.5(2) . . . . ?
C7 C12 C11 C27 179.72(15) . . . . ?
C7 C12 C11 C10 -0.5(2) . . . . ?
C7 C8 C9 C10 0.0(2) . . . . ?
C7 C8 C9 C48 179.21(15) . . . . ?
C1 O1 C12 C11 -179.84(14) . . . . ?
C1 O1 C12 C7 0.3(2) . . . . ?
C1 C2 C3 C4 -0.3(3) . . . . ?
C1 C2 C13 C14 -110.70(17) . . . . ?
C1 C2 C13 C26 72.9(2) . . . . ?
C1 C6 C5 C4 -0.3(2) . . . . ?
C1 C6 C41 C7 -0.9(2) . . . . ?
C1 C6 C41 C42 -121.92(17) . . . . ?
C1 C6 C41 C43 118.22(17) . . . . ?
C3 C2 C1 O1 179.89(15) . . . . ?
C3 C2 C1 C6 0.0(2) . . . . ?
C3 C2 C13 C14 68.4(2) . . . . ?
C3 C2 C13 C26 -107.95(18) . . . . ?
C3 C4 C44 C47 -7.9(3) . . . . ?
C3 C4 C44 C46 -125.9(2) . . . . ?
C3 C4 C44 C45 115.6(2) . . . . ?
C8 C7 C41 C6 179.84(14) . . . . ?
C8 C7 C41 C42 -59.06(19) . . . . ?
C8 C7 C41 C43 60.77(19) . . . . ?
C8 C9 C10 C11 0.0(2) . . . . ?
C8 C9 C48 C51 167.09(18) . . . . ?
C8 C9 C48 C49 47.7(2) . . . . ?
C8 C9 C48 C50 -71.6(2) . . . . ?
C27 C11 C10 C9 180.00(15) . . . . ?
C27 C28 C33 C34 0.8(2) . . . . ?
C27 C28 C33 C32 -177.47(17) . . . . ?
C27 C28 C29 C30 178.25(19) . . . . ?
C27 C40 C35 C34 -0.3(2) . . . . ?
C27 C40 C35 C36 178.62(14) . . . . ?
C27 C40 C39 C38 -178.51(16) . . . . ?
C28 C27 C40 C35 1.3(2) . . . . ?
C28 C27 C40 C39 -179.03(14) . . . . ?
C28 C33 C34 C35 0.1(3) . . . . ?
C28 C33 C32 C31 -0.9(3) . . . . ?
C28 C29 C30 C31 -0.8(4) . . . . ?
C13 C2 C1 O1 -1.0(2) . . . . ?
C13 C2 C1 C6 179.20(15) . . . . ?
C13 C2 C3 C4 -179.50(16) . . . . ?
C13 C14 C19 C20 -0.1(2) . . . . ?
C13 C14 C19 C18 178.59(15) . . . . ?
C13 C14 C15 C16 -178.83(17) . . . . ?
C13 C26 C21 C20 1.5(2) . . . . ?
C13 C26 C21 C22 -177.30(16) . . . . ?
C13 C26 C25 C24 178.52(19) . . . . ?
C5 C6 C1 O1 -179.60(15) . . . . ?
C5 C6 C1 C2 0.2(2) . . . . ?
C5 C6 C41 C7 179.96(14) . . . . ?
C5 C6 C41 C42 58.89(19) . . . . ?
C5 C6 C41 C43 -60.97(19) . . . . ?
C5 C4 C44 C47 172.14(19) . . . . ?
C5 C4 C44 C46 54.2(2) . . . . ?
C5 C4 C44 C45 -64.3(2) . . . . ?
C41 C6 C1 O1 1.2(2) . . . . ?
C41 C6 C1 C2 -178.98(14) . . . . ?
C41 C6 C5 C4 178.97(15) . . . . ?
C41 C7 C8 C9 -179.84(15) . . . . ?
C14 C13 C26 C21 -3.3(2) . . . . ?
C14 C13 C26 C25 178.05(16) . . . . ?
C14 C19 C20 C21 -1.8(3) . . . . ?
C14 C19 C18 C17 0.5(3) . . . . ?
C14 C15 C16 C17 0.0(3) . . . . ?
C40 C27 C28 C33 -1.5(2) . . . . ?
C40 C27 C28 C29 179.85(15) . . . . ?
C40 C35 C34 C33 -0.4(3) . . . . ?
C40 C35 C36 C37 0.2(3) . . . . ?
C40 C39 C38 C37 -0.4(3) . . . . ?
C26 C13 C14 C19 2.6(2) . . . . ?
C26 C13 C14 C15 -177.84(15) . . . . ?
C26 C21 C20 C19 1.1(3) . . . . ?
C26 C21 C22 C23 -1.3(3) . . . . ?
C26 C25 C24 C23 -1.3(4) . . . . ?
C10 C11 C27 C28 -107.96(18) . . . . ?
C10 C11 C27 C40 69.5(2) . . . . ?
C10 C9 C48 C51 -13.8(3) . . . . ?
C10 C9 C48 C49 -133.1(2) . . . . ?
C10 C9 C48 C50 107.5(2) . . . . ?
C19 C14 C15 C16 0.7(3) . . . . ?
C19 C18 C17 C16 0.2(3) . . . . ?
C33 C28 C29 C30 -0.4(3) . . . . ?
C33 C32 C31 C30 -0.2(4) . . . . ?
C35 C40 C39 C38 1.2(2) . . . . ?
C35 C36 C37 C38 0.6(3) . . . . ?
C21 C26 C25 C24 -0.1(3) . . . . ?
C21 C22 C23 C24 -0.1(4) . . . . ?
C48 C9 C10 C11 -179.15(15) . . . . ?
C20 C19 C18 C17 179.16(19) . . . . ?
C20 C21 C22 C23 179.9(2) . . . . ?
C39 C40 C35 C34 179.96(15) . . . . ?
C39 C40 C35 C36 -1.1(2) . . . . ?
C39 C38 C37 C36 -0.5(3) . . . . ?
C34 C33 C32 C31 -179.2(2) . . . . ?
C34 C35 C36 C37 179.17(18) . . . . ?
C15 C14 C19 C20 -179.62(15) . . . . ?
C15 C14 C19 C18 -1.0(2) . . . . ?
C36 C35 C34 C33 -179.30(17) . . . . ?
C25 C26 C21 C20 -179.83(17) . . . . ?
C25 C26 C21 C22 1.4(3) . . . . ?
C25 C24 C23 C22 1.4(4) . . . . ?
C29 C28 C33 C34 179.51(17) . . . . ?
C29 C28 C33 C32 1.2(3) . . . . ?
C18 C19 C20 C21 179.56(17) . . . . ?
C18 C17 C16 C15 -0.5(3) . . . . ?
C32 C33 C34 C35 178.37(18) . . . . ?
C32 C31 C30 C29 1.1(4) . . . . ?
C22 C21 C20 C19 179.85(18) . . . . ?
Cl2A C53A C52A Cl1A -176.1(7) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.861
_oxdiff_exptl_absorpt_empirical_full_min 0.335
