# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

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

data_2j-danjing1_auto
_audit_block_doi                 10.5517/ccdc.csd.cc2d4w0g
_database_code_depnum_ccdc_archive 'CCDC 2209215'
loop_
_audit_author_name
_audit_author_address
'Sichen Tao'
;TJUT
China
;
_audit_update_record             
;
2022-09-24 deposited with the CCDC.	2023-01-20 downloaded from the CCDC.
;
_audit_creation_date             2022-07-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        1
_chemical_formula_moiety         '2(C24 H30 O4)'
_chemical_formula_sum            'C48 H60 O8'
_chemical_formula_weight         764.96
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   15.9821(4)
_cell_length_b                   14.8327(3)
_cell_length_c                   19.0411(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.264(2)
_cell_angle_gamma                90
_cell_volume                     4501.34(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21069
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.9240
_cell_measurement_theta_min      2.3210
_shelx_estimated_absorpt_T_max   0.976
_shelx_estimated_absorpt_T_min   0.948
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
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    1.129
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47701
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.500
_diffrn_reflns_theta_min         3.485
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     26.00  72.00   0.50    0.50    --   42.30 -54.00 -60.00   92
  2  ω    -35.00  -6.00   0.50    0.50    --   42.30 -82.00  90.00   58
  3  ω    -47.00  22.00   0.50    0.50    --   42.30 -54.00 -60.00  138
  4  ω    100.00 126.00   0.50    0.50    --   42.30  54.00  90.00   52
  5  ω     21.00  70.00   0.50    0.50    --   42.30 -82.00  90.00   98
  6  ω    -47.00  21.00   0.50    0.50    --   42.30 -77.00-120.00  136
  7  ω      5.00  34.00   0.50    0.50    --   42.30 -77.00 120.00   58
  8  ω    -44.00  68.00   0.50    0.50    --   42.30 -54.00 150.00  224
  9  ω     19.00  47.00   0.50    0.50    --   42.30  54.00  90.00   56
 10  ω    -40.00 -14.00   0.50    0.50    --   42.30 -82.00-150.00   52
 11  ω    -16.00  66.00   0.50    0.50    --   42.30 -65.00 -60.00  164
 12  ω    -36.00 -10.00   0.50    0.50    --   42.30 -82.00  30.00   52
 13  ω     77.00 102.00   0.50    0.50    --   42.30  77.00-180.00   50
 14  ω     28.00  53.00   0.50    0.50    --   42.30  77.00-180.00   50
 15  ω     29.00  70.00   0.50    0.50    --   42.30 -82.00 -84.05   82
 16  ω    -43.00   8.00   0.50    0.50    --   42.30 -82.00 -84.05  102
 17  ω    -47.00   1.00   0.50    0.50    --   42.30 -77.00 120.00   96
 18  ω     30.00  67.00   0.50    0.50    --   42.30 -82.00  60.00   74
 19  ω     51.00  94.00   0.50    0.50    --   42.30  54.00  90.00   86
 20  ω    -36.00  19.00   0.50    0.50    --   42.30 -77.00-180.00  110
 21  ω     37.00  65.00   0.50    0.50    --   42.30 -77.00-180.00   56
 22  ω     41.00  70.00   0.50    0.50    --   42.30 -82.00-150.00   58
 23  ω     18.00  43.00   0.50    0.50    --   42.30  43.00 120.00   50
 24  ω     41.00  66.00   0.50    0.50    --   42.30 -65.00-180.00   50
 25  ω     53.00  78.00   0.50    0.50    --   42.30  43.00 120.00   50
 26  ω     36.00  67.00   0.50    0.50    --   42.30 -82.00  30.00   62
 27  ω     36.00  61.00   0.50    0.50    --   42.30 -77.00 120.00   50
 28  ω     35.00  99.00   0.50    1.50    --   93.70 -82.00 120.00  128
 29  ω     13.00 118.00   0.50    1.50    --   93.70 -82.00   0.00  210
 30  ω    119.00 160.00   0.50    1.50    --   93.70  33.00 120.00   82
 31  ω     71.00  97.00   0.50    1.50    --   93.70 -82.00  69.96   52
 32  ω     64.00  90.00   0.50    1.50    --   93.70 -82.00  60.00   52
 33  ω     76.00 105.00   0.50    1.50    --   93.70  68.00-120.00   58
 34  ω      5.00 183.00   0.50    1.50    --   93.70  -8.00 120.00  356
 35  ω     20.00  63.00   0.50    1.50    --   93.70 -82.00 -30.00   86
 36  ω      4.00  33.00   0.50    1.50    --   93.70 -82.00  69.96   58
 37  ω     14.00  74.00   0.50    1.50    --   93.70 -82.00  26.60  120
 38  ω     12.00  95.00   0.50    1.50    --   93.70 -82.00 150.00  166
 39  ω     75.00 102.00   0.50    1.50    --   93.70 -82.00-120.00   54
 40  ω      8.00  98.00   0.50    1.50    --   93.70 -82.00 -90.00  180
 41  ω      4.00  92.00   0.50    1.50    --   93.70 -59.00  30.00  176
 42  ω    100.00 128.00   0.50    1.50    --   93.70 -33.00  60.00   56
 43  ω     77.00 102.00   0.50    1.50    --   93.70 -82.00  76.17   50
 44  ω    120.00 183.00   0.50    1.50    --   93.70  68.00-150.00  126
 45  ω     81.00 115.00   0.50    1.50    --   93.70  68.00-150.00   68
 46  ω     27.00 101.00   0.50    1.50    --   93.70 -82.00 -60.00  148
 47  ω     60.00 100.00   0.50    1.50    --   93.70 -82.00-150.00   80
 48  ω      9.00  86.00   0.50    1.50    --   93.70 -33.00  60.00  154
 49  ω     82.00 108.00   0.50    1.50    --   93.70 -82.00 -30.00   52
 50  ω     73.00  98.00   0.50    1.50    --   93.70 -82.00  30.00   50
 51  ω     11.00  37.00   0.50    1.50    --   93.70 -82.00-150.00   52
 52  ω      5.00 113.00   0.50    1.50    --   93.70 -59.00 150.00  216
 53  ω     10.00 128.00   0.50    1.50    --   93.70  25.00  30.00  236
 54  ω     73.00 105.00   0.50    1.50    --   93.70 -82.00 165.60   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro II AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0148726000
_diffrn_orient_matrix_UB_12      0.0827751000
_diffrn_orient_matrix_UB_13      -0.0481922000
_diffrn_orient_matrix_UB_21      -0.0650606000
_diffrn_orient_matrix_UB_22      -0.0537148000
_diffrn_orient_matrix_UB_23      -0.0468520000
_diffrn_orient_matrix_UB_31      -0.0699894000
_diffrn_orient_matrix_UB_32      0.0322964000
_diffrn_orient_matrix_UB_33      0.0454205000
_diffrn_oxdiff_digest_frames     
;
01d50762f83e0d74199b9cde2f4bb13fc300029b762
;
_diffrn_oxdiff_digest_hkl        
;
01802e3c27259397ef9a5c07a918ecbc675c39
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed 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                6313
_reflns_number_total             8230
_reflns_odcompleteness_completeness 99.92
_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 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         8230
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0946
_refine_ls_restrained_S_all      1.221
_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)+(0.1662P)²+1.5640P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2749
_refine_ls_wR_factor_ref         0.2958
_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, All O(H) groups
2. Restrained distances
 O4-C24
 1.35 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
O4 \\sim C24 \\sim C21: within 2.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
C22 \\sim C21 \\sim C20: within 2.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
4.a Riding coordinates:
 O7(H7), O3(H3)
4.b Ternary CH refined with riding coordinates:
 C33(H33), C12(H12)
4.c Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C40(H40A,H40B), C35(H35A,H35B), C36(H36A,H36B), C15(H15A,
 H15B), C16(H16A,H16B), C11(H11A,H11B), C10(H10A,H10B)
4.d Aromatic/amide H refined with riding coordinates:
 C29(H29), C28(H28), C32(H32), C31(H31), C47(H47), C46(H46), C44(H44),
 C43(H43), C7(H7A), C8(H8), C4(H4), C5(H5), C23(H23), C22(H22), C20(H20),
 C19(H19)
4.e Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C37(H37A,H37B,H37C), C25(H25A,H25B,H25C), C48(H48A,H48B,
 H48C), C17(H17A,H17B,H17C), C9(H9A,H9B,H9C), C1(H1A,H1B,H1C), C24(H24A,H24B,
 H24C)
;
_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
O7 O 0.45035(12) 0.93337(12) 0.59310(9) 0.0561(5) Uani 1 1 d . . . . .
H7 H 0.476969 0.980156 0.589324 0.084 Uiso 1 1 d R . . . .
O6 O 0.35420(18) 0.49309(16) 0.73138(19) 0.1075(10) Uani 1 1 d . . . . .
O5 O 0.25024(19) 0.5780(2) 0.7599(2) 0.1264(13) Uani 1 1 d . . . . .
O8 O 0.7967(2) 0.7250(2) 0.45378(15) 0.1076(10) Uani 1 1 d . . . . .
C30 C 0.45266(16) 0.79010(16) 0.65344(12) 0.0483(6) Uani 1 1 d . . . . .
C29 C 0.36914(17) 0.79985(18) 0.66693(14) 0.0558(6) Uani 1 1 d . . . . .
H29 H 0.341893 0.854337 0.657250 0.067 Uiso 1 1 calc R . . . .
C28 C 0.32597(18) 0.7288(2) 0.69479(16) 0.0620(7) Uani 1 1 d . . . . .
H28 H 0.270260 0.736514 0.704540 0.074 Uiso 1 1 calc R . . . .
C27 C 0.36471(18) 0.64670(18) 0.70826(15) 0.0583(7) Uani 1 1 d . . . . .
C32 C 0.44818(18) 0.63655(19) 0.69429(16) 0.0626(7) Uani 1 1 d . . . . .
H32 H 0.475197 0.581747 0.703169 0.075 Uiso 1 1 calc R . . . .
C31 C 0.49108(18) 0.70770(19) 0.66723(16) 0.0595(7) Uani 1 1 d . . . . .
H31 H 0.547002 0.700160 0.658067 0.071 Uiso 1 1 calc R . . . .
C33 C 0.50420(16) 0.86524(17) 0.62528(13) 0.0504(6) Uani 1 1 d . . . . .
H33 H 0.537322 0.839842 0.588762 0.061 Uiso 1 1 calc R . . . .
C34 C 0.56446(17) 0.90346(18) 0.68240(13) 0.0534(6) Uani 1 1 d . . . . .
C38 C 0.64687(19) 0.8930(2) 0.68014(16) 0.0686(8) Uani 1 1 d . . . . .
C39 C 0.7101(2) 0.9182(3) 0.74149(19) 0.0849(10) Uani 1 1 d . . . . .
H39A H 0.680075 0.936092 0.781668 0.102 Uiso 1 1 calc R . . . .
H39B H 0.743959 0.865840 0.755039 0.102 Uiso 1 1 calc R . . . .
C40 C 0.7650(3) 0.9919(4) 0.7225(2) 0.1106(15) Uani 1 1 d . . . . .
H40A H 0.731236 1.044732 0.710214 0.133 Uiso 1 1 calc R . . . .
H40B H 0.793763 0.974618 0.681452 0.133 Uiso 1 1 calc R . . . .
C41 C 0.8317(3) 1.0161(4) 0.7846(2) 0.1210(18) Uani 1 1 d . . . . .
H41A H 0.863919 1.067332 0.771549 0.181 Uiso 1 1 calc GR . . . .
H41B H 0.868425 0.965666 0.794015 0.181 Uiso 1 1 calc GR . . . .
H41C H 0.803505 1.030228 0.825968 0.181 Uiso 1 1 calc GR . . . .
C35 C 0.52343(19) 0.95016(19) 0.74197(14) 0.0594(7) Uani 1 1 d . . . . .
H35A H 0.468363 0.970857 0.724011 0.071 Uiso 1 1 calc R . . . .
H35B H 0.556388 1.003121 0.755512 0.071 Uiso 1 1 calc R . . . .
C36 C 0.5131(3) 0.8941(3) 0.80805(16) 0.0797(9) Uani 1 1 d . . . . .
H36A H 0.478405 0.841918 0.795850 0.096 Uiso 1 1 calc R . . . .
H36B H 0.567605 0.872719 0.826806 0.096 Uiso 1 1 calc R . . . .
C37 C 0.4732(4) 0.9487(4) 0.8636(2) 0.128(2) Uani 1 1 d . . . . .
H37A H 0.422367 0.975722 0.843427 0.192 Uiso 1 1 calc GR . . . .
H37B H 0.511291 0.995048 0.880786 0.192 Uiso 1 1 calc GR . . . .
H37C H 0.460574 0.909964 0.901773 0.192 Uiso 1 1 calc GR . . . .
C26 C 0.3160(2) 0.5714(2) 0.7361(2) 0.0754(9) Uani 1 1 d . . . . .
C25 C 0.3106(4) 0.4148(3) 0.7554(4) 0.153(3) Uani 1 1 d . . . . .
H25A H 0.264399 0.400499 0.722118 0.230 Uiso 1 1 calc GR . . . .
H25B H 0.289875 0.427296 0.800441 0.230 Uiso 1 1 calc GR . . . .
H25C H 0.348501 0.364545 0.759591 0.230 Uiso 1 1 calc GR . . . .
C42 C 0.68544(18) 0.8507(2) 0.61910(16) 0.0654(7) Uani 1 1 d . . . . .
C47 C 0.7213(2) 0.7660(3) 0.62461(19) 0.0776(9) Uani 1 1 d . . . . .
H47 H 0.720987 0.735098 0.667072 0.093 Uiso 1 1 calc R . . . .
C46 C 0.7574(3) 0.7263(3) 0.5692(2) 0.0871(10) Uani 1 1 d . . . . .
H46 H 0.781088 0.669204 0.574708 0.104 Uiso 1 1 calc R . . . .
C45 C 0.7588(2) 0.7703(3) 0.50538(19) 0.0789(9) Uani 1 1 d . . . . .
C44 C 0.7224(2) 0.8539(3) 0.49752(18) 0.0772(9) Uani 1 1 d . . . . .
H44 H 0.721834 0.883946 0.454632 0.093 Uiso 1 1 calc R . . . .
C43 C 0.6861(2) 0.8932(2) 0.55434(18) 0.0737(8) Uani 1 1 d . . . . .
H43 H 0.661638 0.949864 0.548644 0.088 Uiso 1 1 calc R . . . .
C48 C 0.8001(4) 0.7669(5) 0.3877(2) 0.148(2) Uani 1 1 d . . . . .
H48A H 0.835052 0.732063 0.359016 0.222 Uiso 1 1 calc GR . . . .
H48B H 0.823012 0.826399 0.393995 0.222 Uiso 1 1 calc GR . . . .
H48C H 0.744553 0.770714 0.364934 0.222 Uiso 1 1 calc GR . . . .
O3 O 0.46452(13) 0.90895(12) 0.44782(9) 0.0597(5) Uani 1 1 d . . . . .
H3 H 0.449447 0.912373 0.487969 0.090 Uiso 1 1 d R . . . .
O2 O 0.48967(16) 0.7731(2) 0.08882(11) 0.0917(8) Uani 1 1 d . . . . .
O1 O 0.62107(17) 0.7658(3) 0.13394(14) 0.1139(11) Uani 1 1 d . . . . .
C6 C 0.44763(16) 0.82832(17) 0.33920(12) 0.0486(6) Uani 1 1 d . . . . .
C7 C 0.39559(18) 0.7980(2) 0.28232(14) 0.0603(7) Uani 1 1 d . . . . .
H7A H 0.338679 0.789725 0.287405 0.072 Uiso 1 1 calc R . . . .
C8 C 0.42742(19) 0.7801(2) 0.21852(14) 0.0648(7) Uani 1 1 d . . . . .
H8 H 0.391563 0.761157 0.180686 0.078 Uiso 1 1 calc R . . . .
C3 C 0.51190(18) 0.7899(2) 0.21017(14) 0.0583(7) Uani 1 1 d . . . . .
C4 C 0.56492(18) 0.8179(2) 0.26722(14) 0.0601(7) Uani 1 1 d . . . . .
H4 H 0.622143 0.823889 0.262471 0.072 Uiso 1 1 calc R . . . .
C5 C 0.53272(16) 0.83680(18) 0.33096(13) 0.0540(6) Uani 1 1 d . . . . .
H5 H 0.568619 0.855485 0.368846 0.065 Uiso 1 1 calc R . . . .
C12 C 0.40919(16) 0.84981(17) 0.40717(12) 0.0495(6) Uani 1 1 d . . . . .
H12 H 0.356051 0.881443 0.395913 0.059 Uiso 1 1 calc R . . . .
C13 C 0.39138(17) 0.76549(17) 0.44896(12) 0.0507(6) Uani 1 1 d . . . . .
C14 C 0.31389(18) 0.74676(18) 0.46665(14) 0.0558(6) Uani 1 1 d . . . . .
C15 C 0.2921(2) 0.6670(2) 0.51161(17) 0.0712(8) Uani 1 1 d . . . . .
H15A H 0.343904 0.637733 0.528983 0.085 Uiso 1 1 calc R . . . .
H15B H 0.265158 0.689345 0.552125 0.085 Uiso 1 1 calc R . . . .
C16 C 0.2358(3) 0.5972(2) 0.4751(2) 0.0908(11) Uani 1 1 d . . . . .
H16A H 0.264725 0.568795 0.437933 0.109 Uiso 1 1 calc R . . . .
H16B H 0.185813 0.626297 0.453707 0.109 Uiso 1 1 calc R . . . .
C17 C 0.2103(3) 0.5250(3) 0.5273(3) 0.1181(17) Uani 1 1 d . . . . .
H17A H 0.170965 0.484186 0.503735 0.177 Uiso 1 1 calc GR . . . .
H17B H 0.184934 0.553479 0.565665 0.177 Uiso 1 1 calc GR . . . .
H17C H 0.259221 0.492260 0.545045 0.177 Uiso 1 1 calc GR . . . .
C11 C 0.46865(19) 0.70938(19) 0.46998(15) 0.0597(7) Uani 1 1 d . . . . .
H11A H 0.465171 0.689045 0.518088 0.072 Uiso 1 1 calc R . . . .
H11B H 0.517713 0.747762 0.469175 0.072 Uiso 1 1 calc R . . . .
C10 C 0.4814(2) 0.6272(2) 0.42368(19) 0.0762(9) Uani 1 1 d . . . . .
H10A H 0.435914 0.584853 0.428304 0.091 Uiso 1 1 calc R . . . .
H10B H 0.480067 0.645916 0.374793 0.091 Uiso 1 1 calc R . . . .
C9 C 0.5639(3) 0.5815(3) 0.4441(3) 0.1091(14) Uani 1 1 d . . . . .
H9A H 0.568539 0.527882 0.416358 0.164 Uiso 1 1 calc GR . . . .
H9B H 0.566490 0.565756 0.493074 0.164 Uiso 1 1 calc GR . . . .
H9C H 0.609170 0.621684 0.435703 0.164 Uiso 1 1 calc GR . . . .
C2 C 0.5479(2) 0.7755(3) 0.14188(16) 0.0718(8) Uani 1 1 d . . . . .
C1 C 0.5183(3) 0.7617(5) 0.01916(18) 0.128(2) Uani 1 1 d . . . . .
H1A H 0.472703 0.772961 -0.015429 0.193 Uiso 1 1 calc GR . . . .
H1B H 0.538203 0.701141 0.014008 0.193 Uiso 1 1 calc GR . . . .
H1C H 0.563026 0.803342 0.012626 0.193 Uiso 1 1 calc GR . . . .
C18 C 0.24048(18) 0.80604(19) 0.44607(15) 0.0585(7) Uani 1 1 d . . . . .
C23 C 0.2236(2) 0.8806(2) 0.4867(2) 0.0764(9) Uani 1 1 d . . . . .
H23 H 0.257976 0.893614 0.527027 0.092 Uiso 1 1 calc R . . . .
C22 C 0.1559(3) 0.9357(3) 0.4676(3) 0.1002(11) Uani 1 1 d . U . . .
H22 H 0.145707 0.986416 0.494394 0.120 Uiso 1 1 calc R . . . .
C21 C 0.1032(3) 0.9155(3) 0.4087(3) 0.1107(11) Uani 1 1 d . U . . .
C20 C 0.1172(3) 0.8415(3) 0.3700(3) 0.1011(11) Uani 1 1 d . U . . .
H20 H 0.080502 0.826760 0.331535 0.121 Uiso 1 1 calc R . . . .
C19 C 0.1859(2) 0.7881(3) 0.38753(18) 0.0756(9) Uani 1 1 d . . . . .
H19 H 0.196029 0.738563 0.359455 0.091 Uiso 1 1 calc R . . . .
O4 O 0.0338(2) 0.9643(3) 0.3848(3) 0.1644(14) Uani 1 1 d D U . . .
C24 C 0.0279(4) 1.0519(3) 0.4019(4) 0.167(2) Uani 1 1 d D U . . .
H24A H -0.022807 1.076575 0.379497 0.251 Uiso 1 1 calc GR . . . .
H24B H 0.075308 1.083975 0.386424 0.251 Uiso 1 1 calc GR . . . .
H24C H 0.026922 1.057613 0.452081 0.251 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
O7 H7 0.8200 . ?
O7 C33 1.435(3) . ?
O6 C26 1.318(4) . ?
O6 C25 1.446(4) . ?
O5 C26 1.179(4) . ?
O8 C45 1.368(4) . ?
O8 C48 1.409(6) . ?
C30 C29 1.385(4) . ?
C30 C31 1.384(4) . ?
C30 C33 1.508(3) . ?
C29 H29 0.9300 . ?
C29 C28 1.387(4) . ?
C28 H28 0.9300 . ?
C28 C27 1.382(4) . ?
C27 C32 1.388(4) . ?
C27 C26 1.482(4) . ?
C32 H32 0.9300 . ?
C32 C31 1.379(4) . ?
C31 H31 0.9300 . ?
C33 H33 0.9800 . ?
C33 C34 1.509(4) . ?
C34 C38 1.330(4) . ?
C34 C35 1.519(4) . ?
C38 C39 1.533(5) . ?
C38 C42 1.494(4) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.464(6) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 C41 1.573(6) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C36 1.527(4) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 C37 1.510(5) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C42 C47 1.382(5) . ?
C42 C43 1.385(5) . ?
C47 H47 0.9300 . ?
C47 C46 1.373(5) . ?
C46 H46 0.9300 . ?
C46 C45 1.381(6) . ?
C45 C44 1.374(5) . ?
C44 H44 0.9300 . ?
C44 C43 1.392(5) . ?
C43 H43 0.9300 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
O3 H3 0.8200 . ?
O3 C12 1.431(3) . ?
O2 C2 1.322(4) . ?
O2 C1 1.445(4) . ?
O1 C2 1.199(4) . ?
C6 C7 1.390(4) . ?
C6 C5 1.386(4) . ?
C6 C12 1.507(3) . ?
C7 H7A 0.9300 . ?
C7 C8 1.377(4) . ?
C8 H8 0.9300 . ?
C8 C3 1.379(4) . ?
C3 C4 1.391(4) . ?
C3 C2 1.476(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.382(4) . ?
C5 H5 0.9300 . ?
C12 H12 0.9800 . ?
C12 C13 1.521(3) . ?
C13 C14 1.337(4) . ?
C13 C11 1.518(4) . ?
C14 C15 1.516(4) . ?
C14 C18 1.495(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.508(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.536(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C10 1.526(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.508(5) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C18 C23 1.388(4) . ?
C18 C19 1.389(4) . ?
C23 H23 0.9300 . ?
C23 C22 1.383(5) . ?
C22 H22 0.9300 . ?
C22 C21 1.383(7) . ?
C21 C20 1.351(7) . ?
C21 O4 1.374(5) . ?
C20 H20 0.9300 . ?
C20 C19 1.374(5) . ?
C19 H19 0.9300 . ?
O4 C24 1.344(2) . ?
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
C33 O7 H7 109.6 . . ?
C26 O6 C25 116.7(3) . . ?
C45 O8 C48 118.3(4) . . ?
C29 C30 C33 123.2(2) . . ?
C31 C30 C29 118.5(2) . . ?
C31 C30 C33 118.3(2) . . ?
C30 C29 H29 119.8 . . ?
C30 C29 C28 120.4(2) . . ?
C28 C29 H29 119.8 . . ?
C29 C28 H28 119.6 . . ?
C27 C28 C29 120.8(3) . . ?
C27 C28 H28 119.6 . . ?
C28 C27 C32 118.9(2) . . ?
C28 C27 C26 119.4(3) . . ?
C32 C27 C26 121.7(3) . . ?
C27 C32 H32 120.0 . . ?
C31 C32 C27 120.0(3) . . ?
C31 C32 H32 120.0 . . ?
C30 C31 H31 119.3 . . ?
C32 C31 C30 121.4(3) . . ?
C32 C31 H31 119.3 . . ?
O7 C33 C30 110.3(2) . . ?
O7 C33 H33 107.8 . . ?
O7 C33 C34 111.9(2) . . ?
C30 C33 H33 107.8 . . ?
C30 C33 C34 111.0(2) . . ?
C34 C33 H33 107.8 . . ?
C33 C34 C35 115.0(2) . . ?
C38 C34 C33 120.9(2) . . ?
C38 C34 C35 124.1(3) . . ?
C34 C38 C39 123.0(3) . . ?
C34 C38 C42 122.8(3) . . ?
C42 C38 C39 114.1(3) . . ?
C38 C39 H39A 109.3 . . ?
C38 C39 H39B 109.3 . . ?
H39A C39 H39B 108.0 . . ?
C40 C39 C38 111.5(3) . . ?
C40 C39 H39A 109.3 . . ?
C40 C39 H39B 109.3 . . ?
C39 C40 H40A 109.3 . . ?
C39 C40 H40B 109.3 . . ?
C39 C40 C41 111.7(4) . . ?
H40A C40 H40B 107.9 . . ?
C41 C40 H40A 109.3 . . ?
C41 C40 H40B 109.3 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C34 C35 H35A 108.2 . . ?
C34 C35 H35B 108.2 . . ?
C34 C35 C36 116.5(2) . . ?
H35A C35 H35B 107.3 . . ?
C36 C35 H35A 108.2 . . ?
C36 C35 H35B 108.2 . . ?
C35 C36 H36A 109.4 . . ?
C35 C36 H36B 109.4 . . ?
H36A C36 H36B 108.0 . . ?
C37 C36 C35 111.2(3) . . ?
C37 C36 H36A 109.4 . . ?
C37 C36 H36B 109.4 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O6 C26 C27 112.4(3) . . ?
O5 C26 O6 122.0(3) . . ?
O5 C26 C27 125.6(3) . . ?
O6 C25 H25A 109.5 . . ?
O6 C25 H25B 109.5 . . ?
O6 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C47 C42 C38 121.0(3) . . ?
C47 C42 C43 116.8(3) . . ?
C43 C42 C38 122.2(3) . . ?
C42 C47 H47 119.1 . . ?
C46 C47 C42 121.9(4) . . ?
C46 C47 H47 119.1 . . ?
C47 C46 H46 119.7 . . ?
C47 C46 C45 120.6(4) . . ?
C45 C46 H46 119.7 . . ?
O8 C45 C46 115.9(4) . . ?
O8 C45 C44 124.9(4) . . ?
C44 C45 C46 119.2(3) . . ?
C45 C44 H44 120.3 . . ?
C45 C44 C43 119.4(3) . . ?
C43 C44 H44 120.3 . . ?
C42 C43 C44 122.2(3) . . ?
C42 C43 H43 118.9 . . ?
C44 C43 H43 118.9 . . ?
O8 C48 H48A 109.5 . . ?
O8 C48 H48B 109.5 . . ?
O8 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C12 O3 H3 109.2 . . ?
C2 O2 C1 116.9(3) . . ?
C7 C6 C12 118.6(2) . . ?
C5 C6 C7 118.4(2) . . ?
C5 C6 C12 122.9(2) . . ?
C6 C7 H7A 119.6 . . ?
C8 C7 C6 120.7(3) . . ?
C8 C7 H7A 119.6 . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C3 120.7(3) . . ?
C3 C8 H8 119.7 . . ?
C8 C3 C4 119.1(2) . . ?
C8 C3 C2 122.4(3) . . ?
C4 C3 C2 118.5(3) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.1(3) . . ?
C5 C4 H4 119.9 . . ?
C6 C5 H5 119.6 . . ?
C4 C5 C6 120.9(2) . . ?
C4 C5 H5 119.5 . . ?
O3 C12 C6 108.6(2) . . ?
O3 C12 H12 108.4 . . ?
O3 C12 C13 110.69(19) . . ?
C6 C12 H12 108.4 . . ?
C6 C12 C13 112.3(2) . . ?
C13 C12 H12 108.4 . . ?
C14 C13 C12 121.1(2) . . ?
C14 C13 C11 124.8(2) . . ?
C11 C13 C12 114.1(2) . . ?
C13 C14 C15 124.1(3) . . ?
C13 C14 C18 122.4(2) . . ?
C18 C14 C15 113.5(2) . . ?
C14 C15 H15A 108.4 . . ?
C14 C15 H15B 108.4 . . ?
H15A C15 H15B 107.5 . . ?
C16 C15 C14 115.4(3) . . ?
C16 C15 H15A 108.4 . . ?
C16 C15 H15B 108.4 . . ?
C15 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
C15 C16 C17 111.0(4) . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C13 C11 H11A 108.5 . . ?
C13 C11 H11B 108.5 . . ?
C13 C11 C10 115.2(2) . . ?
H11A C11 H11B 107.5 . . ?
C10 C11 H11A 108.5 . . ?
C10 C11 H11B 108.5 . . ?
C11 C10 H10A 109.4 . . ?
C11 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C9 C10 C11 111.2(3) . . ?
C9 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
C10 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O2 C2 C3 112.3(3) . . ?
O1 C2 O2 122.6(3) . . ?
O1 C2 C3 125.2(3) . . ?
O2 C1 H1A 109.5 . . ?
O2 C1 H1B 109.5 . . ?
O2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C23 C18 C14 120.3(3) . . ?
C23 C18 C19 117.6(3) . . ?
C19 C18 C14 122.1(3) . . ?
C18 C23 H23 119.8 . . ?
C22 C23 C18 120.3(4) . . ?
C22 C23 H23 119.8 . . ?
C23 C22 H22 119.9 . . ?
C23 C22 C21 120.2(4) . . ?
C21 C22 H22 119.9 . . ?
C20 C21 C22 120.2(4) . . ?
C20 C21 O4 114.2(5) . . ?
O4 C21 C22 125.6(5) . . ?
C21 C20 H20 120.1 . . ?
C21 C20 C19 119.8(5) . . ?
C19 C20 H20 120.1 . . ?
C18 C19 H19 119.1 . . ?
C20 C19 C18 121.8(4) . . ?
C20 C19 H19 119.1 . . ?
C24 O4 C21 119.9(6) . . ?
O4 C24 H24A 109.5 . . ?
O4 C24 H24B 109.5 . . ?
O4 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
O7 C33 C34 C38 -123.6(3) . . . . ?
O7 C33 C34 C35 58.6(3) . . . . ?
O8 C45 C44 C43 -179.6(3) . . . . ?
C30 C29 C28 C27 -1.3(5) . . . . ?
C30 C33 C34 C38 112.8(3) . . . . ?
C30 C33 C34 C35 -65.1(3) . . . . ?
C29 C30 C31 C32 -0.5(4) . . . . ?
C29 C30 C33 O7 -19.5(3) . . . . ?
C29 C30 C33 C34 105.1(3) . . . . ?
C29 C28 C27 C32 0.8(5) . . . . ?
C29 C28 C27 C26 -178.2(3) . . . . ?
C28 C27 C32 C31 -0.2(5) . . . . ?
C28 C27 C26 O6 165.6(3) . . . . ?
C28 C27 C26 O5 -14.1(6) . . . . ?
C27 C32 C31 C30 0.0(5) . . . . ?
C32 C27 C26 O6 -13.4(5) . . . . ?
C32 C27 C26 O5 166.9(4) . . . . ?
C31 C30 C29 C28 1.1(4) . . . . ?
C31 C30 C33 O7 161.3(2) . . . . ?
C31 C30 C33 C34 -74.1(3) . . . . ?
C33 C30 C29 C28 -178.1(3) . . . . ?
C33 C30 C31 C32 178.8(3) . . . . ?
C33 C34 C38 C39 -170.9(3) . . . . ?
C33 C34 C38 C42 5.5(5) . . . . ?
C33 C34 C35 C36 97.0(3) . . . . ?
C34 C38 C39 C40 -115.3(4) . . . . ?
C34 C38 C42 C47 -108.7(4) . . . . ?
C34 C38 C42 C43 70.4(4) . . . . ?
C34 C35 C36 C37 178.9(4) . . . . ?
C38 C34 C35 C36 -80.8(4) . . . . ?
C38 C39 C40 C41 -178.4(4) . . . . ?
C38 C42 C47 C46 -179.7(3) . . . . ?
C38 C42 C43 C44 179.8(3) . . . . ?
C39 C38 C42 C47 68.0(4) . . . . ?
C39 C38 C42 C43 -113.0(4) . . . . ?
C35 C34 C38 C39 6.7(5) . . . . ?
C35 C34 C38 C42 -176.9(3) . . . . ?
C26 C27 C32 C31 178.9(3) . . . . ?
C25 O6 C26 O5 1.4(7) . . . . ?
C25 O6 C26 C27 -178.3(5) . . . . ?
C42 C38 C39 C40 68.0(5) . . . . ?
C42 C47 C46 C45 -0.1(6) . . . . ?
C47 C42 C43 C44 -1.1(5) . . . . ?
C47 C46 C45 O8 179.6(3) . . . . ?
C47 C46 C45 C44 -1.1(6) . . . . ?
C46 C45 C44 C43 1.2(5) . . . . ?
C45 C44 C43 C42 -0.1(5) . . . . ?
C43 C42 C47 C46 1.2(5) . . . . ?
C48 O8 C45 C46 -179.8(5) . . . . ?
C48 O8 C45 C44 1.0(6) . . . . ?
O3 C12 C13 C14 116.3(3) . . . . ?
O3 C12 C13 C11 -61.4(3) . . . . ?
C6 C7 C8 C3 1.5(5) . . . . ?
C6 C12 C13 C14 -122.1(3) . . . . ?
C6 C12 C13 C11 60.2(3) . . . . ?
C7 C6 C5 C4 1.7(4) . . . . ?
C7 C6 C12 O3 -158.9(2) . . . . ?
C7 C6 C12 C13 78.3(3) . . . . ?
C7 C8 C3 C4 0.2(5) . . . . ?
C7 C8 C3 C2 -177.1(3) . . . . ?
C8 C3 C4 C5 -1.0(5) . . . . ?
C8 C3 C2 O2 14.4(5) . . . . ?
C8 C3 C2 O1 -164.8(4) . . . . ?
C3 C4 C5 C6 0.0(4) . . . . ?
C4 C3 C2 O2 -162.9(3) . . . . ?
C4 C3 C2 O1 17.9(6) . . . . ?
C5 C6 C7 C8 -2.4(4) . . . . ?
C5 C6 C12 O3 21.5(3) . . . . ?
C5 C6 C12 C13 -101.2(3) . . . . ?
C12 C6 C7 C8 178.1(3) . . . . ?
C12 C6 C5 C4 -178.8(3) . . . . ?
C12 C13 C14 C15 -176.5(2) . . . . ?
C12 C13 C14 C18 0.7(4) . . . . ?
C12 C13 C11 C10 -99.9(3) . . . . ?
C13 C14 C15 C16 -115.2(3) . . . . ?
C13 C14 C18 C23 -84.3(3) . . . . ?
C13 C14 C18 C19 97.4(3) . . . . ?
C13 C11 C10 C9 174.2(3) . . . . ?
C14 C13 C11 C10 82.4(3) . . . . ?
C14 C15 C16 C17 -174.0(3) . . . . ?
C14 C18 C23 C22 179.8(3) . . . . ?
C14 C18 C19 C20 178.2(3) . . . . ?
C15 C14 C18 C23 93.2(3) . . . . ?
C15 C14 C18 C19 -85.2(3) . . . . ?
C11 C13 C14 C15 1.0(4) . . . . ?
C11 C13 C14 C18 178.2(2) . . . . ?
C2 C3 C4 C5 176.5(3) . . . . ?
C1 O2 C2 O1 -2.4(6) . . . . ?
C1 O2 C2 C3 178.4(4) . . . . ?
C18 C14 C15 C16 67.3(4) . . . . ?
C18 C23 C22 C21 1.6(6) . . . . ?
C23 C18 C19 C20 -0.2(5) . . . . ?
C23 C22 C21 C20 0.6(6) . . . . ?
C23 C22 C21 O4 179.3(4) . . . . ?
C22 C21 C20 C19 -2.6(6) . . . . ?
C22 C21 O4 C24 23.6(8) . . . . ?
C21 C20 C19 C18 2.4(6) . . . . ?
C20 C21 O4 C24 -157.6(6) . . . . ?
C19 C18 C23 C22 -1.8(5) . . . . ?
O4 C21 C20 C19 178.6(4) . . . . ?

_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 4.126
_oxdiff_exptl_absorpt_empirical_full_min 0.350
####################################################################### 
# 
# 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_xcalibur
_database_code_depnum_ccdc_archive 'CCDC 2209526'
loop_
_audit_author_name
_audit_author_address
'Sichen Tao'
;TJUT
China
;
_audit_update_record             
;
2022-09-24 deposited with the CCDC.	2023-01-20 downloaded from the CCDC.
;
_audit_creation_date             2022-07-19
_audit_creation_method           'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_cell_length_a                   12.3606(7)
_cell_length_b                   13.3752(10)
_cell_length_c                   14.6048(8)
_cell_angle_alpha                84.368(5)
_cell_angle_beta                 77.529(5)
_cell_angle_gamma                69.589(6)
_cell_volume                     2208.8(2)
_cell_measurement_reflns_used    7861
_cell_measurement_theta_min      3.1180
_cell_measurement_theta_max      64.8960
_cell_oxdiff_length_a            12.3606(7)
_cell_oxdiff_length_b            13.3752(10)
_cell_oxdiff_length_c            14.6048(8)
_cell_oxdiff_angle_alpha         84.368(5)
_cell_oxdiff_angle_beta          77.529(5)
_cell_oxdiff_angle_gamma         69.589(6)
_cell_oxdiff_volume              2208.8(2)
_cell_oxdiff_measurement_reflns_used 7861
_exptl_absorpt_correction_T_min  0.69576
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.568
_oxdiff_exptl_absorpt_empirical_full_max 1.997
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro II AFC12 (RINC): Kappa single'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            21527
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_sigmaI/netI    0.1123
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.0999
_diffrn_reflns_theta_max         68.8192
_diffrn_measured_fraction_theta_max 0.9521
_diffrn_reflns_theta_full        66.9682
_diffrn_measured_fraction_theta_full 0.9711
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0171743000
_diffrn_orient_matrix_UB_12      0.1092532000
_diffrn_orient_matrix_UB_13      -0.0205729000
_diffrn_orient_matrix_UB_21      -0.0634060000
_diffrn_orient_matrix_UB_22      0.0337032000
_diffrn_orient_matrix_UB_23      0.1008789000
_diffrn_orient_matrix_UB_31      0.1186067000
_diffrn_orient_matrix_UB_32      -0.0451773000
_diffrn_orient_matrix_UB_33      0.0328398000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     63.00 132.00   0.50    0.80    --   42.30  82.00-150.00  138
  2  ω    -46.00  67.00   0.50    0.80    --   42.30 -77.00-120.00  226
  3  ω    -36.00  19.00   0.50    0.80    --   42.30 -77.00 120.00  110
  4  ω    -42.00 -16.00   0.50    0.80    --   42.30 -82.00  60.00   52
  5  ω     29.00  69.00   0.50    0.80    --   42.30 -82.00 -30.00   80
  6  ω     -5.00  66.00   0.50    0.80    --   42.30 -82.00  30.00  142
  7  ω    105.00 130.00   0.50    0.80    --   42.30  11.00  90.00   50
  8  ω     23.00  49.00   0.50    0.80    --   42.30 -77.00 -60.00   52
  9  ω     -6.00  20.00   0.50    0.80    --   42.30 -77.00 -90.00   52
 10  ω     36.00  70.00   0.50    0.80    --   42.30 -82.00  60.00   68
 11  ω     25.00  56.00   0.50    0.80    --   42.30  82.00-150.00   62
 12  ω    -45.00  69.00   0.50    0.80    --   42.30 -82.00-180.00  228
 13  ω     -9.00  16.00   0.50    0.80    --   42.30 -82.00 -30.00   50
 14  ω    -38.00 -12.00   0.50    0.80    --   42.30 -82.00  30.00   52
 15  ω    -43.00  42.00   0.50    0.80    --   42.30  11.00  90.00  170
 16  ω    -38.00 -13.00   0.50    0.80    --   42.30 -82.00 -30.00   50
 17  ω    -19.00   6.00   0.50    0.80    --   42.30 -77.00 -60.00   50
 18  ω     24.00  51.00   0.50    0.80    --   42.30 -77.00 120.00   54
 19  ω      3.00  28.00   0.50    0.80    --   42.30 -65.00-180.00   50
 20  ω      5.00 112.00   0.50    1.00    --   93.70 -59.00 -30.00  214
 21  ω      7.00  89.00   0.50    1.00    --   93.70 -33.00 150.00  164
 22  ω      4.00 106.00   0.50    1.00    --   93.70 -59.00 150.00  204
 23  ω     70.00  96.00   0.50    1.00    --   93.70 -82.00-150.00   52
 24  ω     11.00 121.00   0.50    1.00    --   93.70 -82.00 150.00  220
 25  ω    109.00 135.00   0.50    1.00    --   93.70  77.00  60.00   52
 26  ω    153.00 182.00   0.50    1.00    --   93.70  77.00  60.00   58
 27  ω     70.00  98.00   0.50    1.00    --   93.70 -82.00 -41.25   56
 28  ω     65.00  91.00   0.50    1.00    --   93.70 -82.00  30.00   52
 29  ω      4.00 103.00   0.50    1.00    --   93.70 -82.00 -90.00  198
 30  ω      4.00  99.00   0.50    1.00    --   93.70 -82.00 120.00  190
 31  ω     68.00 110.00   0.50    1.00    --   93.70 -82.00-180.00   84
 32  ω     69.00 101.00   0.50    1.00    --   93.70 -82.00  60.00   64
 33  ω      4.00 183.00   0.50    1.00    --   93.70   0.00-120.00  358
 34  ω     83.00 114.00   0.50    1.00    --   93.70 -33.00   0.00   62
 35  ω     19.00  45.00   0.50    1.00    --   93.70 -33.00   0.00   52
 36  ω      8.00  89.00   0.50    1.00    --   93.70 -33.00 -30.00  162
 37  ω    111.00 149.00   0.50    1.00    --   93.70  59.00-150.00   76
 38  ω     74.00 106.00   0.50    1.00    --   93.70 -82.00   0.00   64
 39  ω     99.00 126.00   0.50    1.00    --   93.70 -33.00 150.00   54
 40  ω     72.00  97.00   0.50    1.00    --   93.70 -82.00-120.00   50
 41  ω     12.00  73.00   0.50    1.00    --   93.70 -82.00  90.00  122
 42  ω     60.00  86.00   0.50    1.00    --   93.70 -82.00 -60.00   52
 43  ω      9.00  59.00   0.50    1.00    --   93.70 -82.00 -41.25  100
 44  ω     10.00  95.00   0.50    1.00    --   93.70 -82.00 -26.45  170
;
_diffrn_measurement_method       'ω scans'
_diffrn_oxdiff_digest_frames     
;
01825f2e3351879ab3b16bf098382c1bab000279fe2
;
_diffrn_oxdiff_digest_hkl        
;
01ebd5e0b28b7e0bd2481a47ab256f8b772dcb
;
_space_group_IT_number           2
_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_reflns_odcompleteness_completeness 97.11
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
####################################################################### 
# 
# 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_2j-3_auto
_database_code_depnum_ccdc_archive 'CCDC 2209525'
loop_
_audit_author_name
_audit_author_address
'Sichen Tao'
;TJUT
China
;
_audit_update_record             
;
2022-09-24 deposited with the CCDC.	2023-01-20 downloaded from the CCDC.
;
_audit_creation_date             2022-07-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        1
_chemical_formula_moiety         '2(C23 H27 F3 O3)'
_chemical_formula_sum            'C46 H54 F6 O6'
_chemical_formula_weight         816.89
_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'
F F 0.0727 0.0534 '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                   12.5957(3)
_cell_length_b                   13.0422(4)
_cell_length_c                   15.1090(5)
_cell_angle_alpha                84.924(3)
_cell_angle_beta                 76.057(2)
_cell_angle_gamma                69.976(2)
_cell_volume                     2263.24(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7139
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      59.7040
_cell_measurement_theta_min      3.0010
_shelx_estimated_absorpt_T_max   0.969
_shelx_estimated_absorpt_T_min   0.954
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
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    1.199
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_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            21866
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        66.582
_diffrn_reflns_theta_max         66.581
_diffrn_reflns_theta_min         3.014
_diffrn_ambient_temperature      293
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     14.00  79.00   0.50    1.00    --   42.30  43.00   0.00  130
  2  ω    -45.00  30.00   0.50    1.00    --   42.30 -77.00  90.00  150
  3  ω     31.00 130.00   0.50    1.00    --   42.30  77.00 120.00  198
  4  ω     85.00 122.00   0.50    1.00    --   42.30  43.00   0.00   74
  5  ω     36.00  66.00   0.50    1.00    --   42.30 -82.00-120.00   60
  6  ω     80.00 132.00   0.50    1.00    --   42.30  77.00-120.00  104
  7  ω    -11.00  69.00   0.50    1.00    --   42.30 -82.00-180.00  160
  8  ω    -43.00  17.00   0.50    1.00    --   42.30 -65.00 -90.00  120
  9  ω     -5.00  27.00   0.50    1.00    --   42.30 -82.00-120.00   64
 10  ω     34.00  63.00   0.50    1.00    --   42.30  77.00-120.00   58
 11  ω    -10.00  41.00   0.50    1.00    --   42.30 -77.00-180.00  102
 12  ω    -10.00  39.00   0.50    1.00    --   42.30 -65.00   0.00   98
 13  ω     41.00  69.00   0.50    1.00    --   42.30 -82.00  60.00   56
 14  ω    -46.00  13.00   0.50    1.00    --   42.30 -82.00  60.00  118
 15  ω    -39.00 -14.00   0.50    1.00    --   42.30 -82.00-120.00   50
 16  ω     34.00  69.00   0.50    1.00    --   42.30 -82.00 -60.00   70
 17  ω    -29.00  -4.00   0.50    1.00    --   42.30 -77.00 -60.00   50
 18  ω     41.00  66.00   0.50    1.00    --   42.30 -65.00 -90.00   50
 19  ω     28.00  62.00   0.50    1.00    --   42.30 -82.00  30.00   68
 20  ω     72.00  98.00   0.50    1.50    --   93.70 -82.00 -60.00   52
 21  ω     66.00 183.00   0.50    1.50    --   93.70  82.00 -60.00  234
 22  ω    155.00 181.00   0.50    1.50    --   93.70  59.00 150.00   52
 23  ω    129.00 163.00   0.50    1.50    --   93.70  33.00 -90.00   68
 24  ω     60.00 104.00   0.50    1.50    --   93.70  33.00 -90.00   88
 25  ω      5.00  99.00   0.50    1.50    --   93.70 -82.00-150.00  188
 26  ω      4.00 104.00   0.50    1.50    --   93.70 -82.00 120.00  200
 27  ω    134.00 160.00   0.50    1.50    --   93.70  68.00-180.00   52
 28  ω      4.00 111.00   0.50    1.50    --   93.70 -82.00   0.00  214
 29  ω     71.00  97.00   0.50    1.50    --   93.70  68.00-180.00   52
 30  ω      4.00  67.00   0.50    1.50    --   93.70 -82.00  60.00  126
 31  ω      7.00  94.00   0.50    1.50    --   93.70 -82.00 -30.00  174
 32  ω     31.00  96.00   0.50    1.50    --   93.70 -82.00-120.00  130
 33  ω     66.00 183.00   0.50    1.50    --   93.70  33.00-150.00  234
 34  ω     23.00  98.00   0.50    1.50    --   93.70 -82.00  90.00  150
 35  ω    114.00 183.00   0.50    1.50    --   93.70  33.00 150.00  138
 36  ω     79.00 105.00   0.50    1.50    --   93.70 -82.00 -90.00   52
 37  ω    117.00 182.00   0.50    1.50    --   93.70  59.00  60.00  130
 38  ω     79.00 105.00   0.50    1.50    --   93.70 -82.00-180.00   52
 39  ω     65.00  90.00   0.50    1.50    --   93.70  33.00 150.00   50
 40  ω      4.00  70.00   0.50    1.50    --   93.70 -82.00 -90.00  132
 41  ω     71.00  96.00   0.50    1.50    --   93.70 -82.00 150.00   50
 42  ω     58.00 107.00   0.50    1.50    --   93.70 -82.00  30.00   98
 43  ω     74.00  99.00   0.50    1.50    --   93.70 -82.00  60.00   50
 44  ω     66.00  91.00   0.50    1.50    --   93.70  59.00  60.00   50
 45  ω     91.00 183.00   0.50    1.50    --   93.70  77.00 -90.00  184
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro II AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0299810000
_diffrn_orient_matrix_UB_12      -0.0847192000
_diffrn_orient_matrix_UB_13      -0.0748900000
_diffrn_orient_matrix_UB_21      -0.0330545000
_diffrn_orient_matrix_UB_22      0.0928935000
_diffrn_orient_matrix_UB_23      -0.0691620000
_diffrn_orient_matrix_UB_31      0.1259335000
_diffrn_orient_matrix_UB_32      0.0002477000
_diffrn_orient_matrix_UB_33      -0.0254145000
_diffrn_oxdiff_digest_frames     
;
01b620c7b376e31582fd8e1b8be70d562900027c3dd
;
_diffrn_oxdiff_digest_hkl        
;
01d922bc0fe4111cff4d9766501d8cae16bfa5
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed 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                4776
_reflns_number_total             7780
_reflns_odcompleteness_completeness 97.26
_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 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         7780
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1139
_refine_ls_R_factor_gt           0.0881
_refine_ls_restrained_S_all      1.220
_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          0.2964
_refine_ls_wR_factor_ref         0.3349
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C8(H8), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C33(H33A,H33B), C10(H10A,H10B), C14(H14A,H14B), C34(H34A,
 H34B), C37(H37A,H37B), C38(H38A,H38B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C5(H5), C30(H30), C22(H22), C19(H19), C20(H20), C41(H41), C28(H28),
 C25(H25), C7(H7), C4(H4), C45(H45), C42(H42), C2(H2A), C44(H44), C27(H27)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C23(H23A,H23B,H23C), C16(H16A,H16B,H16C), C35(H35A,H35B,
 H35C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C)
2.e Idealised tetrahedral OH refined as rotating group:
 O5(H5A)
;
_atom_sites_solution_hydrogens   mixed
_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
O2 O 0.36274(16) 0.61220(16) 0.52778(14) 0.0851(6) Uani 1 1 d . . . . .
O5 O 0.55062(17) 0.54772(18) 0.61057(13) 0.0925(6) Uani 1 1 d . . . . .
H5A H 0.486665 0.583945 0.601454 0.139 Uiso 1 1 calc GR . . . .
O3 O -0.1770(2) 0.6345(3) 0.5111(2) 0.1287(9) Uani 1 1 d . . . . .
C8 C 0.2903(2) 0.7136(2) 0.49697(19) 0.0810(7) Uani 1 1 d . . . . .
H8 H 0.227794 0.699170 0.477810 0.097 Uiso 1 1 calc R . . . .
C12 C 0.2364(2) 0.7902(2) 0.5764(2) 0.0844(8) Uani 1 1 d . . . . .
C32 C 0.5017(3) 0.6225(3) 0.7629(2) 0.0890(8) Uani 1 1 d . . . . .
C31 C 0.5401(2) 0.5208(2) 0.70625(19) 0.0852(8) Uani 1 1 d . . . . .
H31 H 0.481418 0.484731 0.725002 0.102 Uiso 1 1 calc R . . . .
C6 C 0.3552(2) 0.7614(2) 0.41661(19) 0.0821(7) Uani 1 1 d . . . . .
C29 C 0.6548(3) 0.4416(2) 0.7194(2) 0.0871(8) Uani 1 1 d . . . . .
C11 C 0.3180(3) 0.8298(3) 0.6118(2) 0.0914(8) Uani 1 1 d . . . . .
H11A H 0.395952 0.778586 0.593100 0.110 Uiso 1 1 calc R . . . .
H11B H 0.296916 0.828912 0.677928 0.110 Uiso 1 1 calc R . . . .
C18 C 0.0441(2) 0.7735(3) 0.5807(2) 0.0890(8) Uani 1 1 d . . . . .
C17 C 0.0546(3) 0.6642(3) 0.5953(2) 0.0951(9) Uani 1 1 d . . . . .
H17 H 0.113643 0.619057 0.622032 0.114 Uiso 1 1 calc R . . . .
C13 C 0.1209(3) 0.8201(3) 0.6123(2) 0.0936(9) Uani 1 1 d . . . . .
C5 C 0.4738(3) 0.7206(3) 0.3850(2) 0.0950(9) Uani 1 1 d . . . . .
H5 H 0.517432 0.661835 0.415042 0.114 Uiso 1 1 calc R . . . .
C21 C -0.1090(3) 0.6863(3) 0.5326(2) 0.0980(9) Uani 1 1 d . . . . .
C36 C 0.4078(3) 0.6448(3) 0.8321(2) 0.0950(9) Uani 1 1 d . . . . .
C30 C 0.7581(3) 0.4346(3) 0.6593(2) 0.0942(8) Uani 1 1 d . . . . .
H30 H 0.758320 0.480547 0.608603 0.113 Uiso 1 1 calc R . . . .
C40 C 0.3314(3) 0.5772(3) 0.8553(2) 0.1019(10) Uani 1 1 d . . . . .
C22 C -0.0196(3) 0.6207(3) 0.5714(2) 0.0988(9) Uani 1 1 d . . . . .
H22 H -0.009647 0.546934 0.581267 0.119 Uiso 1 1 calc R . . . .
C33 C 0.5797(3) 0.6913(3) 0.7407(2) 0.1012(9) Uani 1 1 d . . . . .
H33A H 0.531597 0.767478 0.741327 0.121 Uiso 1 1 calc R . . . .
H33B H 0.626269 0.674481 0.679147 0.121 Uiso 1 1 calc R . . . .
C19 C -0.0472(3) 0.8372(3) 0.5421(3) 0.1051(10) Uani 1 1 d . . . . .
H19 H -0.058440 0.911248 0.532218 0.126 Uiso 1 1 calc R . . . .
O1 O 0.5235(4) 0.9022(4) 0.1916(4) 0.1925(18) Uani 1 1 d . . . . .
C20 C -0.1213(3) 0.7932(3) 0.5180(3) 0.1086(11) Uani 1 1 d . . . . .
H20 H -0.180709 0.837637 0.491371 0.130 Uiso 1 1 calc R . . . .
C10 C 0.3192(4) 0.9430(3) 0.5803(3) 0.1101(10) Uani 1 1 d . . . . .
H10A H 0.241035 0.994518 0.596590 0.132 Uiso 1 1 calc R . . . .
H10B H 0.344740 0.943641 0.514388 0.132 Uiso 1 1 calc R . . . .
C41 C 0.2637(3) 0.5683(3) 0.7987(2) 0.1079(10) Uani 1 1 d . . . . .
H41 H 0.266296 0.604888 0.742996 0.129 Uiso 1 1 calc R . . . .
O4 O 0.9623(4) 0.2041(4) 0.7549(4) 0.1942(18) Uani 1 1 d . . . . .
C14 C 0.0599(3) 0.8993(3) 0.6896(3) 0.1198(12) Uani 1 1 d . . . . .
H14A H 0.005515 0.963333 0.667988 0.144 Uiso 1 1 calc R . . . .
H14B H 0.116661 0.922520 0.708164 0.144 Uiso 1 1 calc R . . . .
O6 O 0.1050(5) 0.3988(4) 0.9247(3) 0.2053(19) Uani 1 1 d . . . . .
C28 C 0.6566(3) 0.3724(3) 0.7939(3) 0.1172(11) Uani 1 1 d . . . . .
H28 H 0.587478 0.376854 0.835451 0.141 Uiso 1 1 calc R . . . .
C25 C 0.8613(3) 0.3604(3) 0.6729(3) 0.1167(11) Uani 1 1 d . . . . .
H25 H 0.931289 0.356371 0.632690 0.140 Uiso 1 1 calc R . . . .
C7 C 0.2930(4) 0.8502(3) 0.3710(3) 0.1169(12) Uani 1 1 d . . . . .
H7 H 0.212778 0.877897 0.390549 0.140 Uiso 1 1 calc R . . . .
C4 C 0.5290(4) 0.7659(4) 0.3089(3) 0.1212(12) Uani 1 1 d . . . . .
H4 H 0.608666 0.736301 0.286514 0.145 Uiso 1 1 calc R . . . .
C34 C 0.6606(4) 0.6766(4) 0.8044(3) 0.1241(13) Uani 1 1 d . . . . .
H34A H 0.615814 0.685094 0.866876 0.149 Uiso 1 1 calc R . . . .
H34B H 0.716141 0.603163 0.798063 0.149 Uiso 1 1 calc R . . . .
C37 C 0.3697(4) 0.7437(4) 0.8932(3) 0.1222(12) Uani 1 1 d . . . . .
H37A H 0.377243 0.717964 0.954388 0.147 Uiso 1 1 calc R . . . .
H37B H 0.422516 0.784567 0.871660 0.147 Uiso 1 1 calc R . . . .
C45 C 0.3199(4) 0.5223(4) 0.9391(3) 0.1230(12) Uani 1 1 d . . . . .
H45 H 0.363112 0.527228 0.979557 0.148 Uiso 1 1 calc R . . . .
F5 F 1.1246(4) 0.1473(5) 0.7997(4) 0.286(3) Uani 1 1 d . . . . .
F6 F 1.0634(5) 0.3061(6) 0.7585(4) 0.255(2) Uani 1 1 d . . . . .
C3 C 0.4648(5) 0.8542(4) 0.2676(3) 0.1318(15) Uani 1 1 d . . . . .
C42 C 0.1922(4) 0.5055(4) 0.8240(3) 0.1317(14) Uani 1 1 d . . . . .
H42 H 0.149458 0.498591 0.783923 0.158 Uiso 1 1 calc R . . . .
C2 C 0.3470(5) 0.8979(4) 0.2977(3) 0.1387(15) Uani 1 1 d . . . . .
H2A H 0.304512 0.958823 0.269001 0.166 Uiso 1 1 calc R . . . .
C44 C 0.2483(5) 0.4622(5) 0.9638(3) 0.1463(16) Uani 1 1 d . . . . .
H44 H 0.243400 0.426497 1.019970 0.176 Uiso 1 1 calc R . . . .
C43 C 0.1830(4) 0.4541(5) 0.9057(3) 0.1383(15) Uani 1 1 d . . . . .
C38 C 0.2482(4) 0.8199(4) 0.8984(3) 0.1468(17) Uani 1 1 d . . . . .
H38A H 0.239024 0.843143 0.837095 0.176 Uiso 1 1 calc R . . . .
H38B H 0.194687 0.780515 0.923391 0.176 Uiso 1 1 calc R . . . .
C24 C 1.0230(10) 0.2258(8) 0.7913(6) 0.204(4) Uani 1 1 d . . . . .
C9 C 0.3997(5) 0.9797(4) 0.6229(4) 0.1462(16) Uani 1 1 d . . . . .
H9A H 0.394643 1.053124 0.603820 0.219 Uiso 1 1 calc GR . . . .
H9B H 0.478163 0.932139 0.603178 0.219 Uiso 1 1 calc GR . . . .
H9C H 0.376418 0.976798 0.688133 0.219 Uiso 1 1 calc GR . . . .
C27 C 0.7562(5) 0.2985(4) 0.8077(3) 0.1475(17) Uani 1 1 d . . . . .
H27 H 0.755741 0.251687 0.857856 0.177 Uiso 1 1 calc R . . . .
C15 C -0.0061(4) 0.8520(4) 0.7733(3) 0.1428(16) Uani 1 1 d . . . . .
H15A H -0.060171 0.825444 0.754163 0.171 Uiso 1 1 calc R . . . .
H15B H 0.048876 0.790185 0.796812 0.171 Uiso 1 1 calc R . . . .
C26 C 0.8578(4) 0.2929(4) 0.7474(4) 0.1352(15) Uani 1 1 d . . . . .
F4 F 0.9819(5) 0.2482(8) 0.8775(4) 0.307(4) Uani 1 1 d . . . . .
C23 C -0.2681(4) 0.6958(6) 0.4669(4) 0.173(2) Uani 1 1 d . . . . .
H23A H -0.236769 0.730843 0.413420 0.260 Uiso 1 1 calc GR . . . .
H23B H -0.325762 0.750136 0.507921 0.260 Uiso 1 1 calc GR . . . .
H23C H -0.302710 0.647746 0.449808 0.260 Uiso 1 1 calc GR . . . .
C16 C -0.0705(5) 0.9317(5) 0.8471(4) 0.174(2) Uani 1 1 d . . . . .
H16A H -0.104100 1.001934 0.821184 0.261 Uiso 1 1 calc GR . . . .
H16B H -0.018415 0.936572 0.882374 0.261 Uiso 1 1 calc GR . . . .
H16C H -0.130847 0.908600 0.885679 0.261 Uiso 1 1 calc GR . . . .
C35 C 0.7246(5) 0.7565(6) 0.7855(4) 0.174(2) Uani 1 1 d . . . . .
H35A H 0.784210 0.736095 0.730786 0.260 Uiso 1 1 calc GR . . . .
H35B H 0.759039 0.756579 0.835663 0.260 Uiso 1 1 calc GR . . . .
H35C H 0.671612 0.828072 0.777967 0.260 Uiso 1 1 calc GR . . . .
C39 C 0.2169(5) 0.9166(5) 0.9539(4) 0.171(2) Uani 1 1 d . . . . .
H39A H 0.240079 0.972449 0.916971 0.256 Uiso 1 1 calc GR . . . .
H39B H 0.255491 0.898095 1.003533 0.256 Uiso 1 1 calc GR . . . .
H39C H 0.134476 0.942860 0.977511 0.256 Uiso 1 1 calc GR . . . .
C46 C 0.0915(7) 0.3442(8) 1.0116(6) 0.241(4) Uani 1 1 d . . . . .
H46A H 0.140497 0.269222 1.005067 0.361 Uiso 1 1 calc GR . . . .
H46B H 0.012146 0.347927 1.033216 0.361 Uiso 1 1 calc GR . . . .
H46C H 0.113016 0.379122 1.054518 0.361 Uiso 1 1 calc GR . . . .
F3 F 0.5926(5) 0.9207(5) 0.0512(3) 0.275(3) Uani 1 1 d . . . . .
C1 C 0.5337(10) 0.8796(12) 0.1114(7) 0.227(5) Uani 1 1 d . . . . .
F1 F 0.4334(9) 0.9051(10) 0.0938(4) 0.355(5) Uani 1 1 d . . . . .
F2 F 0.5671(11) 0.7764(8) 0.1008(5) 0.388(7) Uani 1 1 d . . . . .
H2 H 0.393(3) 0.560(3) 0.478(2) 0.100(9) Uiso 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
O2 C8 1.438(3) . ?
O5 C31 1.442(4) . ?
O3 C21 1.367(4) . ?
O3 C23 1.430(5) . ?
C8 C12 1.501(4) . ?
C8 C6 1.506(4) . ?
C12 C11 1.512(4) . ?
C12 C13 1.353(4) . ?
C32 C31 1.513(4) . ?
C32 C36 1.341(4) . ?
C32 C33 1.508(5) . ?
C31 C29 1.508(4) . ?
C6 C5 1.377(4) . ?
C6 C7 1.388(4) . ?
C29 C30 1.374(4) . ?
C29 C28 1.379(5) . ?
C11 C10 1.516(5) . ?
C18 C17 1.389(5) . ?
C18 C13 1.487(5) . ?
C18 C19 1.392(5) . ?
C17 C22 1.374(5) . ?
C13 C14 1.502(5) . ?
C5 C4 1.390(5) . ?
C21 C22 1.382(4) . ?
C21 C20 1.353(5) . ?
C36 C40 1.480(5) . ?
C36 C37 1.523(5) . ?
C30 C25 1.379(5) . ?
C40 C41 1.381(5) . ?
C40 C45 1.401(5) . ?
C33 C34 1.520(5) . ?
C19 C20 1.379(5) . ?
O1 C3 1.428(6) . ?
O1 C1 1.239(12) . ?
C10 C9 1.540(6) . ?
C41 C42 1.382(6) . ?
O4 C24 1.161(8) . ?
O4 C26 1.447(6) . ?
C14 C15 1.543(6) . ?
O6 C43 1.371(6) . ?
O6 C46 1.438(7) . ?
C28 C27 1.344(6) . ?
C25 C26 1.367(6) . ?
C7 C2 1.372(6) . ?
C4 C3 1.359(6) . ?
C34 C35 1.492(7) . ?
C37 C38 1.501(6) . ?
C45 C44 1.356(7) . ?
F5 C24 1.364(10) . ?
F6 C24 1.325(8) . ?
C3 C2 1.368(7) . ?
C42 C43 1.351(6) . ?
C44 C43 1.371(7) . ?
C38 C39 1.461(7) . ?
C24 F4 1.300(9) . ?
C27 C26 1.364(6) . ?
C15 C16 1.475(6) . ?
F3 C1 1.235(9) . ?
C1 F1 1.279(11) . ?
C1 F2 1.278(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
C21 O3 C23 118.5(4) . . ?
O2 C8 C12 108.2(2) . . ?
O2 C8 C6 112.5(2) . . ?
C12 C8 C6 112.3(2) . . ?
C8 C12 C11 116.2(2) . . ?
C13 C12 C8 120.2(3) . . ?
C13 C12 C11 123.6(3) . . ?
C36 C32 C31 121.0(3) . . ?
C36 C32 C33 123.0(3) . . ?
C33 C32 C31 115.9(2) . . ?
O5 C31 C32 111.0(2) . . ?
O5 C31 C29 108.5(2) . . ?
C29 C31 C32 111.9(2) . . ?
C5 C6 C8 123.2(3) . . ?
C5 C6 C7 118.0(3) . . ?
C7 C6 C8 118.8(3) . . ?
C30 C29 C31 122.6(3) . . ?
C30 C29 C28 118.4(3) . . ?
C28 C29 C31 119.0(3) . . ?
C12 C11 C10 115.3(3) . . ?
C17 C18 C13 120.9(3) . . ?
C17 C18 C19 116.3(3) . . ?
C19 C18 C13 122.6(3) . . ?
C22 C17 C18 121.9(3) . . ?
C12 C13 C18 122.4(3) . . ?
C12 C13 C14 123.4(3) . . ?
C18 C13 C14 114.2(3) . . ?
C6 C5 C4 120.9(3) . . ?
O3 C21 C22 115.3(3) . . ?
C20 C21 O3 125.7(3) . . ?
C20 C21 C22 119.0(3) . . ?
C32 C36 C40 123.5(3) . . ?
C32 C36 C37 122.5(3) . . ?
C40 C36 C37 114.0(3) . . ?
C29 C30 C25 121.0(3) . . ?
C41 C40 C36 122.8(3) . . ?
C41 C40 C45 116.0(3) . . ?
C45 C40 C36 121.0(3) . . ?
C17 C22 C21 120.2(3) . . ?
C32 C33 C34 115.4(3) . . ?
C20 C19 C18 121.5(3) . . ?
C1 O1 C3 123.1(7) . . ?
C21 C20 C19 121.0(3) . . ?
C11 C10 C9 112.2(3) . . ?
C40 C41 C42 120.8(4) . . ?
C24 O4 C26 114.9(7) . . ?
C13 C14 C15 113.6(3) . . ?
C43 O6 C46 117.6(5) . . ?
C27 C28 C29 121.5(4) . . ?
C26 C25 C30 118.0(4) . . ?
C2 C7 C6 121.6(4) . . ?
C3 C4 C5 119.0(4) . . ?
C35 C34 C33 112.5(4) . . ?
C38 C37 C36 115.7(4) . . ?
C44 C45 C40 122.7(4) . . ?
C4 C3 O1 118.2(5) . . ?
C4 C3 C2 121.8(4) . . ?
C2 C3 O1 120.0(5) . . ?
C43 C42 C41 121.4(4) . . ?
C3 C2 C7 118.6(4) . . ?
C45 C44 C43 119.8(4) . . ?
C42 C43 O6 115.9(5) . . ?
C42 C43 C44 119.2(4) . . ?
C44 C43 O6 124.9(5) . . ?
C39 C38 C37 114.1(5) . . ?
O4 C24 F5 118.7(9) . . ?
O4 C24 F6 119.3(7) . . ?
O4 C24 F4 115.5(9) . . ?
F6 C24 F5 99.1(8) . . ?
F4 C24 F5 97.0(6) . . ?
F4 C24 F6 103.7(8) . . ?
C28 C27 C26 119.2(4) . . ?
C16 C15 C14 113.4(4) . . ?
C25 C26 O4 118.4(4) . . ?
C27 C26 O4 119.2(4) . . ?
C27 C26 C25 121.8(4) . . ?
O1 C1 F1 109.8(10) . . ?
O1 C1 F2 110.9(8) . . ?
F3 C1 O1 117.7(13) . . ?
F3 C1 F1 107.5(8) . . ?
F3 C1 F2 110.3(12) . . ?
F2 C1 F1 99.0(14) . . ?

_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 2.120
_oxdiff_exptl_absorpt_empirical_full_min 0.708
####################################################################### 
# 
# 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_2j-danjing4_auto
_database_code_depnum_ccdc_archive 'CCDC 2209527'
loop_
_audit_author_name
_audit_author_address
'Sichen Tao'
;TJUT
China
;
_audit_update_record             
;
2022-09-27 deposited with the CCDC.	2023-01-20 downloaded from the CCDC.
;
_audit_creation_date             2022-07-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        1
_chemical_formula_moiety         '2(C28 H32 O2)'
_chemical_formula_sum            'C56 H64 O4'
_chemical_formula_weight         801.07
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   17.9673(7)
_cell_length_b                   15.1856(5)
_cell_length_c                   18.5806(8)
_cell_angle_alpha                90
_cell_angle_beta                 103.304(4)
_cell_angle_gamma                90
_cell_volume                     4933.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11817
_cell_measurement_temperature    293
_cell_measurement_theta_max      67.8060
_cell_measurement_theta_min      2.4550
_shelx_estimated_absorpt_T_max   0.980
_shelx_estimated_absorpt_T_min   0.970
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
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    1.078
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1064
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49159
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        63.687
_diffrn_reflns_theta_max         63.687
_diffrn_reflns_theta_min         3.085
_diffrn_ambient_temperature      293
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_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    -42.00  69.00   0.50    1.00    --   42.30 -82.00-150.00  222
  2  ω    -28.00  -2.00   0.50    1.00    --   42.30 -82.00  60.00   52
  3  ω     16.00  70.00   0.50    1.00    --   42.30 -82.00 -90.00  108
  4  ω     24.00  93.00   0.50    1.00    --   42.30  65.00  30.00  138
  5  ω     13.00  72.00   0.50    1.00    --   42.30 -43.00-120.00  118
  6  ω      6.00  70.00   0.50    1.00    --   42.30 -82.00  60.00  128
  7  ω     21.00  64.00   0.50    1.00    --   42.30  65.00 120.00   86
  8  ω     19.00  49.00   0.50    1.00    --   42.30  65.00 -30.00   60
  9  ω     43.00  68.00   0.50    1.00    --   42.30 -77.00-150.00   50
 10  ω     -9.00  65.00   0.50    1.00    --   42.30 -82.00-180.00  148
 11  ω    -46.00   7.00   0.50    1.00    --   42.30 -54.00 120.00  106
 12  ω     10.00  70.00   0.50    1.00    --   42.30 -82.00   0.00  120
 13  ω    -47.00   2.00   0.50    1.00    --   42.30 -82.00   0.00   98
 14  ω    -30.00  -4.00   0.50    1.00    --   42.30 -43.00-120.00   52
 15  ω     44.00  69.00   0.50    1.00    --   42.30 -82.00  90.00   50
 16  ω     42.00  67.00   0.50    1.00    --   42.30 -77.00 -90.00   50
 17  ω     42.00  67.00   0.50    1.00    --   42.30 -77.00 120.00   50
 18  ω      9.00  34.00   0.50    1.00    --   42.30 -77.00-150.00   50
 19  ω     31.00  86.00   0.50    1.00    --   42.30  43.00 120.00  110
 20  ω    -24.00   1.00   0.50    1.00    --   42.30 -77.00  90.00   50
 21  ω    100.00 125.00   0.50    1.00    --   42.30  43.00 120.00   50
 22  ω    -42.00   5.00   0.50    1.00    --   42.30 -82.00 -90.00   94
 23  ω     22.00 120.00   0.50    1.00    --   42.30  65.00-180.00  196
 24  ω     -9.00  16.00   0.50    1.00    --   42.30 -77.00 120.00   50
 25  ω     10.00  70.00   0.50    1.00    --   42.30 -43.00-180.00  120
 26  ω      5.00  34.00   0.50    1.50    --   93.70 -82.00 -90.00   58
 27  ω     59.00  96.00   0.50    1.50    --   93.70 -82.00 -30.00   74
 28  ω     29.00  98.00   0.50    1.50    --   93.70 -82.00-150.00  138
 29  ω     78.00 110.00   0.50    1.50    --   93.70 -33.00 120.00   64
 30  ω     26.00 114.00   0.50    1.50    --   93.70 -82.00  30.00  176
 31  ω      6.00  35.00   0.50    1.50    --   93.70 -33.00 120.00   58
 32  ω      8.00 111.00   0.50    1.50    --   93.70 -59.00 -90.00  206
 33  ω      4.00 180.00   0.50    1.50    --   93.70  -8.00 -90.00  352
 34  ω     12.00  99.00   0.50    1.50    --   93.70 -82.00 120.00  174
 35  ω    117.00 183.00   0.50    1.50    --   93.70  68.00 -90.00  132
 36  ω     73.00  98.00   0.50    1.50    --   93.70  68.00 -90.00   50
 37  ω     70.00  96.00   0.50    1.50    --   93.70 -82.00 -60.00   52
 38  ω      4.00  46.00   0.50    1.50    --   93.70 -42.00  60.00   84
 39  ω    135.00 183.00   0.50    1.50    --   93.70  50.00 -30.00   96
 40  ω     75.00 100.00   0.50    1.50    --   93.70 -82.00   0.00   50
 41  ω     50.00  96.00   0.50    1.50    --   93.70 -82.00 150.00   92
 42  ω      9.00  93.00   0.50    1.50    --   93.70 -82.00-180.00  168
 43  ω    152.00 183.00   0.50    1.50    --   93.70  68.00-180.00   62
 44  ω    114.00 139.00   0.50    1.50    --   93.70  68.00-180.00   50
 45  ω     49.00 101.00   0.50    1.50    --   93.70 -82.00 -90.00  104
 46  ω     99.00 124.00   0.50    1.50    --   93.70  68.00-150.00   50
 47  ω      8.00 120.00   0.50    1.50    --   93.70 -33.00 -90.00  224
 48  ω     10.00  98.00   0.50    1.50    --   93.70 -82.00-120.00  176
 49  ω     73.00  98.00   0.50    1.50    --   93.70 -82.00  70.41   50
 50  ω     42.00  91.00   0.50    1.50    --   93.70 -82.00  90.00   98
 51  ω     16.00  65.00   0.50    1.50    --   93.70 -82.00  70.41   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro II AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0442038000
_diffrn_orient_matrix_UB_12      0.0251858000
_diffrn_orient_matrix_UB_13      -0.0784437000
_diffrn_orient_matrix_UB_21      -0.0738023000
_diffrn_orient_matrix_UB_22      0.0100499000
_diffrn_orient_matrix_UB_23      0.0282074000
_diffrn_orient_matrix_UB_31      0.0190211000
_diffrn_orient_matrix_UB_32      0.0977921000
_diffrn_orient_matrix_UB_33      0.0173211000
_diffrn_oxdiff_digest_frames     
;
014f011bcc05c801f8f6b8b718d8b2f1df00028aafc
;
_diffrn_oxdiff_digest_hkl        
;
014fc68681347458031dddd37c28cc0746b8ab
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed 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                4800
_reflns_number_total             8104
_reflns_odcompleteness_completeness 99.86
_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 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         8104
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0955
_refine_ls_restrained_S_all      1.081
_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)+(0.1891P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2689
_refine_ls_wR_factor_ref         0.3144
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C44(H44)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C13(H13A,H13B), C14(H14A,H14B), C37(H37A,H37B),
 C38(H38A,H38B), C41(H41A,H41B), C42(H42A,H42B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C6(H6), C7(H7), C18(H18), C19(H19), C21(H21), C22(H22),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33),
  C34(H34), C46(H46), C47(H47), C49(H49), C50(H50), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C29(H29A,H29B,
 H29C), C36(H36A,H36B,H36C), C43(H43A,H43B,H43C)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3)
;
_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 0.53128(13) 0.40777(13) 0.55291(13) 0.0851(6) Uani 1 1 d . . . . .
H1 H 0.544606 0.419598 0.514680 0.128 Uiso 1 1 calc GR . . . .
O2 O 0.91978(14) 0.46516(16) 0.62578(17) 0.1090(9) Uani 1 1 d . . . . .
C1 C 0.9243(3) 0.5492(3) 0.5938(4) 0.1455(19) Uani 1 1 d . . . . .
H1A H 0.929827 0.542207 0.543926 0.218 Uiso 1 1 calc GR . . . .
H1B H 0.967669 0.580528 0.622129 0.218 Uiso 1 1 calc GR . . . .
H1C H 0.878491 0.581807 0.593636 0.218 Uiso 1 1 calc GR . . . .
C2 C 0.85548(19) 0.4157(2) 0.5994(2) 0.0838(9) Uani 1 1 d . . . . .
C3 C 0.7980(2) 0.4371(2) 0.5399(2) 0.0846(9) Uani 1 1 d . . . . .
H3A H 0.801176 0.488505 0.513638 0.102 Uiso 1 1 calc R . . . .
C4 C 0.73546(18) 0.3828(2) 0.51879(19) 0.0789(9) Uani 1 1 d . . . . .
H4 H 0.696998 0.398123 0.478020 0.095 Uiso 1 1 calc R . . . .
C5 C 0.72834(17) 0.30591(19) 0.55669(18) 0.0727(8) Uani 1 1 d . . . . .
C6 C 0.78767(19) 0.2852(2) 0.61658(19) 0.0799(9) Uani 1 1 d . . . . .
H6 H 0.784845 0.233695 0.642856 0.096 Uiso 1 1 calc R . . . .
C7 C 0.85026(18) 0.3387(2) 0.6380(2) 0.0820(9) Uani 1 1 d . . . . .
H7 H 0.889192 0.323346 0.678386 0.098 Uiso 1 1 calc R . . . .
C8 C 0.65968(18) 0.2473(2) 0.53259(18) 0.0763(8) Uani 1 1 d . . . . .
C9 C 0.6712(2) 0.1714(3) 0.4837(2) 0.1047(12) Uani 1 1 d . . . . .
H9A H 0.623749 0.138385 0.471182 0.126 Uiso 1 1 calc R . . . .
H9B H 0.679527 0.195955 0.437961 0.126 Uiso 1 1 calc R . . . .
C10 C 0.7324(3) 0.1096(3) 0.5114(3) 0.1377(18) Uani 1 1 d . . . . .
H10A H 0.721123 0.079682 0.553799 0.165 Uiso 1 1 calc R . . . .
H10B H 0.779116 0.142857 0.528959 0.165 Uiso 1 1 calc R . . . .
C11 C 0.7474(3) 0.0412(3) 0.4587(3) 0.1296(16) Uani 1 1 d . . . . .
H11A H 0.765417 0.069052 0.419529 0.194 Uiso 1 1 calc GR . . . .
H11B H 0.700944 0.009782 0.438212 0.194 Uiso 1 1 calc GR . . . .
H11C H 0.785388 0.000737 0.484372 0.194 Uiso 1 1 calc GR . . . .
C12 C 0.59324(17) 0.26568(18) 0.55029(17) 0.0711(8) Uani 1 1 d . . . . .
C13 C 0.52182(17) 0.2100(2) 0.5268(2) 0.0811(9) Uani 1 1 d . . . . .
H13A H 0.517437 0.191219 0.476092 0.097 Uiso 1 1 calc R . . . .
H13B H 0.477704 0.246439 0.527737 0.097 Uiso 1 1 calc R . . . .
C14 C 0.5193(2) 0.1287(2) 0.5744(2) 0.1002(11) Uani 1 1 d . . . . .
H14A H 0.561186 0.089886 0.570739 0.120 Uiso 1 1 calc R . . . .
H14B H 0.526806 0.146713 0.625631 0.120 Uiso 1 1 calc R . . . .
C15 C 0.4455(3) 0.0790(3) 0.5522(4) 0.1437(19) Uani 1 1 d . . . . .
H15A H 0.434410 0.067591 0.499967 0.216 Uiso 1 1 calc GR . . . .
H15B H 0.404958 0.113360 0.563778 0.216 Uiso 1 1 calc GR . . . .
H15C H 0.449834 0.024181 0.578561 0.216 Uiso 1 1 calc GR . . . .
C16 C 0.58490(17) 0.34587(18) 0.59619(17) 0.0707(8) Uani 1 1 d . . . . .
H16 H 0.634882 0.374736 0.610929 0.085 Uiso 1 1 calc R . . . .
C17 C 0.55813(17) 0.32368(18) 0.66502(18) 0.0713(8) Uani 1 1 d . . . . .
C18 C 0.48361(18) 0.3352(2) 0.6716(2) 0.0812(9) Uani 1 1 d . . . . .
H18 H 0.446940 0.356942 0.631786 0.097 Uiso 1 1 calc R . . . .
C19 C 0.4634(2) 0.3145(2) 0.7373(2) 0.0907(10) Uani 1 1 d . . . . .
H19 H 0.412798 0.321957 0.740331 0.109 Uiso 1 1 calc R . . . .
C20 C 0.5157(2) 0.2833(2) 0.7982(2) 0.0841(9) Uani 1 1 d . . . . .
C21 C 0.5895(2) 0.2702(2) 0.7898(2) 0.0867(9) Uani 1 1 d . . . . .
H21 H 0.625894 0.246941 0.828997 0.104 Uiso 1 1 calc R . . . .
C22 C 0.61027(18) 0.2906(2) 0.72544(19) 0.0792(8) Uani 1 1 d . . . . .
H22 H 0.660675 0.281986 0.722320 0.095 Uiso 1 1 calc R . . . .
C23 C 0.4943(3) 0.2668(2) 0.8698(3) 0.0969(12) Uani 1 1 d . . . . .
C24 C 0.5473(3) 0.2797(3) 0.9363(3) 0.1164(14) Uani 1 1 d . . . . .
H24 H 0.596343 0.298425 0.935449 0.140 Uiso 1 1 calc R . . . .
C25 C 0.5288(4) 0.2652(4) 1.0038(3) 0.153(2) Uani 1 1 d . . . . .
H25 H 0.565435 0.274324 1.047495 0.184 Uiso 1 1 calc R . . . .
C26 C 0.4590(6) 0.2384(4) 1.0063(5) 0.172(3) Uani 1 1 d . . . . .
H26 H 0.447020 0.229010 1.051747 0.206 Uiso 1 1 calc R . . . .
C27 C 0.4053(5) 0.2248(4) 0.9430(5) 0.157(3) Uani 1 1 d . . . . .
H27 H 0.356715 0.205977 0.945493 0.189 Uiso 1 1 calc R . . . .
C28 C 0.4220(3) 0.2388(3) 0.8732(3) 0.1239(16) Uani 1 1 d . . . . .
H28 H 0.384829 0.229184 0.830049 0.149 Uiso 1 1 calc R . . . .
O3 O 0.46276(12) 0.55884(13) 0.59486(13) 0.0816(6) Uani 1 1 d . . . . .
H3 H 0.488686 0.516288 0.588666 0.122 Uiso 1 1 calc GR . . . .
O4 O 0.74721(19) 0.7953(2) 0.4710(2) 0.1275(10) Uani 1 1 d . . . . .
C29 C 0.7449(4) 0.7601(4) 0.4001(3) 0.160(2) Uani 1 1 d . . . . .
H29A H 0.768679 0.800535 0.372631 0.239 Uiso 1 1 calc GR . . . .
H29B H 0.692622 0.750951 0.374511 0.239 Uiso 1 1 calc GR . . . .
H29C H 0.771702 0.704990 0.405129 0.239 Uiso 1 1 calc GR . . . .
C30 C 0.7217(2) 0.7437(3) 0.5206(3) 0.0977(11) Uani 1 1 d . . . . .
C31 C 0.7209(2) 0.7831(3) 0.5876(3) 0.1050(12) Uani 1 1 d . . . . .
H31 H 0.736332 0.841385 0.595922 0.126 Uiso 1 1 calc R . . . .
C32 C 0.6977(2) 0.7372(3) 0.6411(2) 0.0992(11) Uani 1 1 d . . . . .
H32 H 0.699051 0.764613 0.686113 0.119 Uiso 1 1 calc R . . . .
C33 C 0.6953(2) 0.6589(3) 0.5080(2) 0.0962(11) Uani 1 1 d . . . . .
H33 H 0.693607 0.632148 0.462621 0.115 Uiso 1 1 calc R . . . .
C34 C 0.6711(2) 0.6135(2) 0.5633(2) 0.0911(10) Uani 1 1 d . . . . .
H34 H 0.653882 0.555870 0.554403 0.109 Uiso 1 1 calc R . . . .
C35 C 0.67192(18) 0.6510(2) 0.6313(2) 0.0837(9) Uani 1 1 d . . . . .
C36 C 0.8350(3) 0.4833(3) 0.7913(3) 0.1205(14) Uani 1 1 d . . . . .
H36A H 0.859760 0.432540 0.776671 0.181 Uiso 1 1 calc GR . . . .
H36B H 0.821047 0.471487 0.837180 0.181 Uiso 1 1 calc GR . . . .
H36C H 0.869332 0.532639 0.797366 0.181 Uiso 1 1 calc GR . . . .
C37 C 0.7627(3) 0.5047(3) 0.7313(3) 0.1296(16) Uani 1 1 d . . . . .
H37A H 0.777724 0.523847 0.686875 0.156 Uiso 1 1 calc R . . . .
H37B H 0.732453 0.451535 0.719337 0.156 Uiso 1 1 calc R . . . .
C38 C 0.7159(2) 0.5727(3) 0.7540(2) 0.1055(12) Uani 1 1 d . . . . .
H38A H 0.747816 0.623398 0.771403 0.127 Uiso 1 1 calc R . . . .
H38B H 0.696257 0.550769 0.795025 0.127 Uiso 1 1 calc R . . . .
C39 C 0.6487(2) 0.6020(2) 0.6921(2) 0.0872(9) Uani 1 1 d . . . . .
C40 C 0.57577(19) 0.5885(2) 0.69440(18) 0.0763(8) Uani 1 1 d . . . . .
C41 C 0.5514(2) 0.5393(2) 0.75477(18) 0.0834(9) Uani 1 1 d . . . . .
H41A H 0.584328 0.488331 0.767266 0.100 Uiso 1 1 calc R . . . .
H41B H 0.499837 0.517757 0.735412 0.100 Uiso 1 1 calc R . . . .
C42 C 0.5523(3) 0.5902(2) 0.8263(2) 0.0977(11) Uani 1 1 d . . . . .
H42A H 0.603400 0.612775 0.846133 0.117 Uiso 1 1 calc R . . . .
H42B H 0.517852 0.640070 0.815071 0.117 Uiso 1 1 calc R . . . .
C43 C 0.5289(4) 0.5340(3) 0.8835(3) 0.158(2) Uani 1 1 d . . . . .
H43A H 0.475833 0.518624 0.867031 0.237 Uiso 1 1 calc GR . . . .
H43B H 0.536489 0.565932 0.929165 0.237 Uiso 1 1 calc GR . . . .
H43C H 0.559244 0.481324 0.890887 0.237 Uiso 1 1 calc GR . . . .
C44 C 0.51201(17) 0.62687(19) 0.63443(18) 0.0735(8) Uani 1 1 d . . . . .
H44 H 0.535166 0.658554 0.599124 0.088 Uiso 1 1 calc R . . . .
C45 C 0.46477(17) 0.69077(19) 0.66654(17) 0.0727(8) Uani 1 1 d . . . . .
C46 C 0.49257(18) 0.77552(19) 0.68418(18) 0.0758(8) Uani 1 1 d . . . . .
H46 H 0.538376 0.792365 0.672971 0.091 Uiso 1 1 calc R . . . .
C47 C 0.45397(18) 0.8345(2) 0.71761(19) 0.0803(9) Uani 1 1 d . . . . .
H47 H 0.474795 0.890089 0.729593 0.096 Uiso 1 1 calc R . . . .
C48 C 0.38378(18) 0.8135(2) 0.73438(19) 0.0789(8) Uani 1 1 d . . . . .
C49 C 0.35588(19) 0.7294(2) 0.7151(2) 0.0851(9) Uani 1 1 d . . . . .
H49 H 0.309388 0.712824 0.724965 0.102 Uiso 1 1 calc R . . . .
C50 C 0.39504(19) 0.6701(2) 0.68195(19) 0.0817(9) Uani 1 1 d . . . . .
H50 H 0.374157 0.614543 0.669521 0.098 Uiso 1 1 calc R . . . .
C51 C 0.34330(19) 0.8784(2) 0.7704(2) 0.0835(9) Uani 1 1 d . . . . .
C52 C 0.2653(2) 0.8912(3) 0.7485(2) 0.1022(11) Uani 1 1 d . . . . .
H52 H 0.236427 0.856762 0.710826 0.123 Uiso 1 1 calc R . . . .
C53 C 0.2299(2) 0.9546(3) 0.7820(3) 0.1223(15) Uani 1 1 d . . . . .
H53 H 0.177402 0.963430 0.766248 0.147 Uiso 1 1 calc R . . . .
C54 C 0.2716(3) 1.0044(3) 0.8383(3) 0.1277(16) Uani 1 1 d . . . . .
H54 H 0.247298 1.046607 0.861014 0.153 Uiso 1 1 calc R . . . .
C55 C 0.3477(2) 0.9927(3) 0.8611(3) 0.1209(15) Uani 1 1 d . . . . .
H55 H 0.375664 1.026843 0.899498 0.145 Uiso 1 1 calc R . . . .
C56 C 0.3842(2) 0.9304(3) 0.8277(2) 0.1028(12) Uani 1 1 d . . . . .
H56 H 0.436760 0.922891 0.843739 0.123 Uiso 1 1 calc R . . . .


_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 H1 0.8200 . ?
O1 C16 1.450(4) . ?
O2 C1 1.418(5) . ?
O2 C2 1.371(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.366(5) . ?
C2 C7 1.386(5) . ?
C3 H3A 0.9300 . ?
C3 C4 1.376(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.384(4) . ?
C5 C6 1.388(5) . ?
C5 C8 1.503(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.370(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.511(5) . ?
C8 C12 1.339(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.447(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.495(6) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.515(4) . ?
C12 C16 1.514(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.525(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.500(6) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16 0.9800 . ?
C16 C17 1.505(4) . ?
C17 C18 1.383(4) . ?
C17 C22 1.381(4) . ?
C18 H18 0.9300 . ?
C18 C19 1.388(5) . ?
C19 H19 0.9300 . ?
C19 C20 1.378(5) . ?
C20 C21 1.384(5) . ?
C20 C23 1.490(5) . ?
C21 H21 0.9300 . ?
C21 C22 1.368(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.389(6) . ?
C23 C28 1.381(6) . ?
C24 H24 0.9300 . ?
C24 C25 1.387(6) . ?
C25 H25 0.9300 . ?
C25 C26 1.329(10) . ?
C26 H26 0.9300 . ?
C26 C27 1.355(10) . ?
C27 H27 0.9300 . ?
C27 C28 1.412(8) . ?
C28 H28 0.9300 . ?
O3 H3 0.8200 . ?
O3 C44 1.446(4) . ?
O4 C29 1.412(6) . ?
O4 C30 1.367(5) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.383(6) . ?
C30 C33 1.373(5) . ?
C31 H31 0.9300 . ?
C31 C32 1.356(5) . ?
C32 H32 0.9300 . ?
C32 C35 1.386(5) . ?
C33 H33 0.9300 . ?
C33 C34 1.389(5) . ?
C34 H34 0.9300 . ?
C34 C35 1.382(5) . ?
C35 C39 1.491(5) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C36 C37 1.539(6) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 C38 1.455(6) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C39 1.530(5) . ?
C39 C40 1.336(5) . ?
C40 C41 1.495(4) . ?
C40 C44 1.519(5) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C42 1.534(5) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C42 C43 1.497(6) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44 0.9800 . ?
C44 C45 1.500(4) . ?
C45 C46 1.392(4) . ?
C45 C50 1.384(4) . ?
C46 H46 0.9300 . ?
C46 C47 1.366(4) . ?
C47 H47 0.9300 . ?
C47 C48 1.404(4) . ?
C48 C49 1.388(4) . ?
C48 C51 1.474(4) . ?
C49 H49 0.9300 . ?
C49 C50 1.374(4) . ?
C50 H50 0.9300 . ?
C51 C52 1.380(5) . ?
C51 C56 1.392(5) . ?
C52 H52 0.9300 . ?
C52 C53 1.380(5) . ?
C53 H53 0.9300 . ?
C53 C54 1.367(6) . ?
C54 H54 0.9300 . ?
C54 C55 1.346(6) . ?
C55 H55 0.9300 . ?
C55 C56 1.378(5) . ?
C56 H56 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C16 O1 H1 109.5 . . ?
C2 O2 C1 117.9(3) . . ?
O2 C1 H1A 109.5 . . ?
O2 C1 H1B 109.5 . . ?
O2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 C7 115.4(3) . . ?
C3 C2 O2 125.2(3) . . ?
C3 C2 C7 119.4(3) . . ?
C2 C3 H3A 119.9 . . ?
C2 C3 C4 120.3(3) . . ?
C4 C3 H3A 119.9 . . ?
C3 C4 H4 119.2 . . ?
C3 C4 C5 121.7(3) . . ?
C5 C4 H4 119.2 . . ?
C4 C5 C6 117.0(3) . . ?
C4 C5 C8 120.9(3) . . ?
C6 C5 C8 122.1(3) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 C5 121.8(3) . . ?
C7 C6 H6 119.1 . . ?
C2 C7 H7 120.1 . . ?
C6 C7 C2 119.9(3) . . ?
C6 C7 H7 120.1 . . ?
C5 C8 C9 114.5(3) . . ?
C12 C8 C5 121.4(3) . . ?
C12 C8 C9 124.1(3) . . ?
C8 C9 H9A 107.7 . . ?
C8 C9 H9B 107.7 . . ?
H9A C9 H9B 107.1 . . ?
C10 C9 C8 118.6(4) . . ?
C10 C9 H9A 107.7 . . ?
C10 C9 H9B 107.7 . . ?
C9 C10 H10A 108.0 . . ?
C9 C10 H10B 108.0 . . ?
C9 C10 C11 117.0(4) . . ?
H10A C10 H10B 107.3 . . ?
C11 C10 H10A 108.0 . . ?
C11 C10 H10B 108.0 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 C13 123.9(3) . . ?
C8 C12 C16 121.0(3) . . ?
C16 C12 C13 115.1(2) . . ?
C12 C13 H13A 108.6 . . ?
C12 C13 H13B 108.6 . . ?
C12 C13 C14 114.9(3) . . ?
H13A C13 H13B 107.5 . . ?
C14 C13 H13A 108.6 . . ?
C14 C13 H13B 108.6 . . ?
C13 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C15 C14 C13 113.0(4) . . ?
C15 C14 H14A 109.0 . . ?
C15 C14 H14B 109.0 . . ?
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 . . ?
O1 C16 C12 110.4(2) . . ?
O1 C16 H16 108.3 . . ?
O1 C16 C17 108.4(2) . . ?
C12 C16 H16 108.3 . . ?
C17 C16 C12 113.0(2) . . ?
C17 C16 H16 108.3 . . ?
C18 C17 C16 123.5(3) . . ?
C22 C17 C16 118.9(3) . . ?
C22 C17 C18 117.7(3) . . ?
C17 C18 H18 119.9 . . ?
C17 C18 C19 120.2(3) . . ?
C19 C18 H18 119.9 . . ?
C18 C19 H19 118.9 . . ?
C20 C19 C18 122.2(3) . . ?
C20 C19 H19 118.9 . . ?
C19 C20 C21 116.6(3) . . ?
C19 C20 C23 121.6(3) . . ?
C21 C20 C23 121.8(4) . . ?
C20 C21 H21 119.1 . . ?
C22 C21 C20 121.8(3) . . ?
C22 C21 H21 119.1 . . ?
C17 C22 H22 119.3 . . ?
C21 C22 C17 121.5(3) . . ?
C21 C22 H22 119.3 . . ?
C24 C23 C20 120.4(4) . . ?
C28 C23 C20 122.1(5) . . ?
C28 C23 C24 117.5(4) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 C23 121.6(5) . . ?
C25 C24 H24 119.2 . . ?
C24 C25 H25 119.9 . . ?
C26 C25 C24 120.2(7) . . ?
C26 C25 H25 119.9 . . ?
C25 C26 H26 119.8 . . ?
C25 C26 C27 120.4(7) . . ?
C27 C26 H26 119.8 . . ?
C26 C27 H27 119.5 . . ?
C26 C27 C28 120.9(6) . . ?
C28 C27 H27 119.5 . . ?
C23 C28 C27 119.3(6) . . ?
C23 C28 H28 120.4 . . ?
C27 C28 H28 120.4 . . ?
C44 O3 H3 109.5 . . ?
C30 O4 C29 118.0(4) . . ?
O4 C29 H29A 109.5 . . ?
O4 C29 H29B 109.5 . . ?
O4 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O4 C30 C31 115.7(4) . . ?
O4 C30 C33 125.3(4) . . ?
C33 C30 C31 119.0(4) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 C30 120.4(4) . . ?
C32 C31 H31 119.8 . . ?
C31 C32 H32 118.7 . . ?
C31 C32 C35 122.6(4) . . ?
C35 C32 H32 118.7 . . ?
C30 C33 H33 120.2 . . ?
C30 C33 C34 119.6(4) . . ?
C34 C33 H33 120.2 . . ?
C33 C34 H34 118.9 . . ?
C35 C34 C33 122.1(4) . . ?
C35 C34 H34 118.9 . . ?
C32 C35 C39 121.0(3) . . ?
C34 C35 C32 116.3(3) . . ?
C34 C35 C39 122.7(3) . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C37 C36 H36A 109.5 . . ?
C37 C36 H36B 109.5 . . ?
C37 C36 H36C 109.5 . . ?
C36 C37 H37A 109.0 . . ?
C36 C37 H37B 109.0 . . ?
H37A C37 H37B 107.8 . . ?
C38 C37 C36 112.8(4) . . ?
C38 C37 H37A 109.0 . . ?
C38 C37 H37B 109.0 . . ?
C37 C38 H38A 108.9 . . ?
C37 C38 H38B 108.9 . . ?
C37 C38 C39 113.5(3) . . ?
H38A C38 H38B 107.7 . . ?
C39 C38 H38A 108.9 . . ?
C39 C38 H38B 108.9 . . ?
C35 C39 C38 113.9(3) . . ?
C40 C39 C35 123.3(3) . . ?
C40 C39 C38 122.8(3) . . ?
C39 C40 C41 124.0(3) . . ?
C39 C40 C44 119.8(3) . . ?
C41 C40 C44 116.1(3) . . ?
C40 C41 H41A 108.1 . . ?
C40 C41 H41B 108.1 . . ?
C40 C41 C42 116.9(3) . . ?
H41A C41 H41B 107.3 . . ?
C42 C41 H41A 108.1 . . ?
C42 C41 H41B 108.1 . . ?
C41 C42 H42A 109.1 . . ?
C41 C42 H42B 109.1 . . ?
H42A C42 H42B 107.9 . . ?
C43 C42 C41 112.3(3) . . ?
C43 C42 H42A 109.1 . . ?
C43 C42 H42B 109.1 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O3 C44 C40 111.7(2) . . ?
O3 C44 H44 108.3 . . ?
O3 C44 C45 109.2(2) . . ?
C40 C44 H44 108.3 . . ?
C45 C44 C40 110.9(3) . . ?
C45 C44 H44 108.3 . . ?
C46 C45 C44 119.1(3) . . ?
C50 C45 C44 123.9(3) . . ?
C50 C45 C46 117.0(3) . . ?
C45 C46 H46 119.3 . . ?
C47 C46 C45 121.4(3) . . ?
C47 C46 H46 119.3 . . ?
C46 C47 H47 119.1 . . ?
C46 C47 C48 121.9(3) . . ?
C48 C47 H47 119.1 . . ?
C47 C48 C51 120.8(3) . . ?
C49 C48 C47 116.2(3) . . ?
C49 C48 C51 123.0(3) . . ?
C48 C49 H49 119.1 . . ?
C50 C49 C48 121.8(3) . . ?
C50 C49 H49 119.1 . . ?
C45 C50 H50 119.2 . . ?
C49 C50 C45 121.7(3) . . ?
C49 C50 H50 119.2 . . ?
C52 C51 C48 122.3(3) . . ?
C52 C51 C56 117.8(3) . . ?
C56 C51 C48 119.9(3) . . ?
C51 C52 H52 119.7 . . ?
C53 C52 C51 120.5(4) . . ?
C53 C52 H52 119.7 . . ?
C52 C53 H53 119.9 . . ?
C54 C53 C52 120.2(4) . . ?
C54 C53 H53 119.9 . . ?
C53 C54 H54 119.8 . . ?
C55 C54 C53 120.5(4) . . ?
C55 C54 H54 119.8 . . ?
C54 C55 H55 119.9 . . ?
C54 C55 C56 120.2(4) . . ?
C56 C55 H55 119.9 . . ?
C51 C56 H56 119.6 . . ?
C55 C56 C51 120.8(4) . . ?
C55 C56 H56 119.6 . . ?

_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 22.635
_oxdiff_exptl_absorpt_empirical_full_min 0.404
