# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1997770'
loop_
_audit_author_name
_audit_author_address
'Yasutomo Segawa'
;Nagoya University
Japan
;
_audit_update_record             
;
2020-04-19 deposited with the CCDC.	2020-06-04 downloaded from the CCDC.
;
_audit_creation_date             2020-04-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C84 H48, 2(C H Cl3), 2(C5 H12)'
_chemical_formula_sum            'C96 H74 Cl6'
_chemical_formula_weight         1440.25
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

_symmetry_space_group_name_H-M_alt 'P 1 21/c 1'
_cell_length_a                   13.9419(3)
_cell_length_b                   18.9963(3)
_cell_length_c                   14.6207(3)
_cell_angle_alpha                90.0
_cell_angle_beta                 97.9869(19)
_cell_angle_gamma                90.0
_cell_volume                     3834.64(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    23233
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.1010
_cell_measurement_theta_min      2.5650
_cell_oxdiff_angle_alpha         90.0015(12)
_cell_oxdiff_angle_beta          97.9891(12)
_cell_oxdiff_angle_gamma         90.0035(11)
_cell_oxdiff_length_a            13.9422(2)
_cell_oxdiff_length_b            18.9958(3)
_cell_oxdiff_length_c            14.6209(2)
_cell_oxdiff_measurement_reflns_used 23233
_cell_oxdiff_volume              3834.64(9)
_shelx_estimated_absorpt_T_max   0.992
_shelx_estimated_absorpt_T_min   0.973
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            69561
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.613
_diffrn_reflns_theta_min         2.174
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -105.00  75.00   0.50   30.00    --  -15.00  45.00   0.00  360
  2  ω   -105.00  75.00   0.50   30.00    --  -15.00  45.00  90.00  360
  3  ω   -105.00  75.00   0.50   30.00    --  -15.00  45.00 180.00  360
  4  ω   -105.00  75.00   0.50   30.00    --  -15.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0001556000
_diffrn_orient_matrix_UB_12      0.0189918000
_diffrn_orient_matrix_UB_13      -0.0417476000
_diffrn_orient_matrix_UB_21      -0.0310232000
_diffrn_orient_matrix_UB_22      -0.0255920000
_diffrn_orient_matrix_UB_23      -0.0238563000
_diffrn_orient_matrix_UB_31      -0.0409478000
_diffrn_orient_matrix_UB_32      0.0194584000
_diffrn_orient_matrix_UB_33      0.0093735000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8234
_reflns_number_total             10893
_reflns_odcompleteness_completeness 92.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.54
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    ?
_refine_diff_density_max         1.364
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         10893
_refine_ls_number_restraints     200
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0732
_refine_ls_restrained_S_all      1.094
_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)+(0.1400P)²+4.4484P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2204
_refine_ls_wR_factor_ref         0.2390
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C44-C45 = C45-C46 = C46-C47 = C47-C48
 1.54 with sigma of 0.01
 C44-C46 = C46-C48 = C45-C47
 2.54 with sigma of 0.01
 C49-C50 = C50-C51 = C51-C52 = C52-C53
 1.54 with sigma of 0.01
 C49-C51 = C51-C53 = C50-C52
 2.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim
C52 \\sim C53: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq,
Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.02
4. Others
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C50)=
 Sof(H50A)=Sof(H50B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C53)=Sof(H53A)=Sof(H53B)=
 Sof(H53C)=1-FVAR(1)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=
 Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=
 Sof(H48C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C8(H8), C21(H21), C22(H22), C35(H35), C36(H36), C43(H43)
5.b Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C51(H51A,H51B), C50(H50A,
 H50B), C52(H52A,H52B)
5.c Me refined with riding coordinates:
 C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C53(H53A,H53B,
 H53C)
5.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17),
 C24(H24), C25(H25), C26(H26), C27(H27), C32(H32), C33(H33), C38(H38), C39(H39),
  C40(H40), C41(H41)
;
_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
C1 C 0.52439(15) 0.10699(11) 0.26069(14) 0.0130(4) Uani 1 1 d . . . . .
C2 C 0.44385(15) 0.14042(11) 0.28525(14) 0.0137(4) Uani 1 1 d . . . . .
C3 C 0.45476(15) 0.18736(11) 0.36052(14) 0.0133(4) Uani 1 1 d . . . . .
C4 C 0.54519(16) 0.20329(12) 0.40712(14) 0.0153(4) Uani 1 1 d . . . . .
H4 H 0.551684 0.236300 0.456406 0.018 Uiso 1 1 calc R . . . .
C5 C 0.62743(15) 0.17040(12) 0.38122(15) 0.0155(4) Uani 1 1 d . . . . .
H5 H 0.690087 0.181240 0.412391 0.019 Uiso 1 1 calc R . . . .
C6 C 0.61634(15) 0.12220(11) 0.31008(14) 0.0134(4) Uani 1 1 d . . . . .
C7 C 0.52826(15) 0.04935(11) 0.18828(14) 0.0136(4) Uani 1 1 d . . . . .
H7 H 0.463449 0.038802 0.152422 0.016 Uiso 1 1 calc R . . . .
C8 C 0.69706(15) 0.07692(11) 0.28101(14) 0.0130(4) Uani 1 1 d . . . . .
H8 H 0.762020 0.087607 0.316502 0.016 Uiso 1 1 calc R . . . .
C9 C 0.60242(16) 0.07325(11) 0.12737(14) 0.0147(4) Uani 1 1 d . . . . .
C10 C 0.58726(17) 0.08106(13) 0.03228(15) 0.0198(4) Uani 1 1 d . . . . .
H10 H 0.525210 0.072556 -0.001741 0.024 Uiso 1 1 calc R . . . .
C11 C 0.66475(19) 0.10166(15) -0.01278(17) 0.0267(5) Uani 1 1 d . . . . .
H11 H 0.655134 0.107197 -0.077987 0.032 Uiso 1 1 calc R . . . .
C12 C 0.75542(18) 0.11413(15) 0.03645(17) 0.0258(5) Uani 1 1 d . . . . .
H12 H 0.807591 0.127556 0.004756 0.031 Uiso 1 1 calc R . . . .
C13 C 0.77055(17) 0.10701(13) 0.13277(16) 0.0196(4) Uani 1 1 d . . . . .
H13 H 0.832475 0.115975 0.166795 0.024 Uiso 1 1 calc R . . . .
C14 C 0.69380(15) 0.08672(11) 0.17758(15) 0.0148(4) Uani 1 1 d . . . . .
C15 C 0.57299(15) -0.01385(11) 0.24280(14) 0.0139(4) Uani 1 1 d . . . . .
C16 C 0.53148(16) -0.07955(12) 0.24694(15) 0.0169(4) Uani 1 1 d . . . . .
H16 H 0.470710 -0.089395 0.211217 0.020 Uiso 1 1 calc R . . . .
C17 C 0.57908(16) -0.13160(12) 0.30384(15) 0.0173(4) Uani 1 1 d . . . . .
H17 H 0.551268 -0.177077 0.306501 0.021 Uiso 1 1 calc R . . . .
C18 C 0.66726(15) -0.11620(11) 0.35636(14) 0.0143(4) Uani 1 1 d . . . . .
C19 C 0.71036(15) -0.04943(11) 0.35219(14) 0.0133(4) Uani 1 1 d . . . . .
C20 C 0.66400(15) 0.00120(11) 0.29433(14) 0.0136(4) Uani 1 1 d . . . . .
C21 C 0.72504(15) -0.16536(11) 0.42608(14) 0.0137(4) Uani 1 1 d . . . . .
H21 H 0.694960 -0.213012 0.428287 0.016 Uiso 1 1 calc R . . . .
C22 C 0.80382(15) -0.04182(11) 0.42006(14) 0.0134(4) Uani 1 1 d . . . . .
H22 H 0.834250 0.005695 0.417686 0.016 Uiso 1 1 calc R . . . .
C23 C 0.82759(16) -0.16793(11) 0.40136(15) 0.0158(4) Uani 1 1 d . . . . .
C24 C 0.87821(18) -0.22784(13) 0.38283(17) 0.0218(5) Uani 1 1 d . . . . .
H24 H 0.849013 -0.272965 0.383855 0.026 Uiso 1 1 calc R . . . .
C25 C 0.9730(2) -0.22092(14) 0.3626(2) 0.0290(6) Uani 1 1 d . . . . .
H25 H 1.008094 -0.261671 0.349389 0.035 Uiso 1 1 calc R . . . .
C26 C 1.01616(19) -0.15516(15) 0.3615(2) 0.0286(6) Uani 1 1 d . . . . .
H26 H 1.080770 -0.151150 0.348359 0.034 Uiso 1 1 calc R . . . .
C27 C 0.96450(17) -0.09462(13) 0.37989(17) 0.0214(5) Uani 1 1 d . . . . .
H27 H 0.993867 -0.049526 0.379363 0.026 Uiso 1 1 calc R . . . .
C28 C 0.87022(16) -0.10118(11) 0.39883(15) 0.0156(4) Uani 1 1 d . . . . .
C29 C 0.73165(15) -0.12591(11) 0.51776(14) 0.0128(4) Uani 1 1 d . . . . .
C30 C 0.69764(14) -0.14691(11) 0.59787(14) 0.0128(4) Uani 1 1 d . . . . .
C31 C 0.70884(15) -0.10150(11) 0.67506(14) 0.0140(4) Uani 1 1 d . . . . .
C32 C 0.75316(15) -0.03689(12) 0.67199(15) 0.0164(4) Uani 1 1 d . . . . .
H32 H 0.761484 -0.007486 0.725063 0.020 Uiso 1 1 calc R . . . .
C33 C 0.78606(15) -0.01458(11) 0.58999(15) 0.0157(4) Uani 1 1 d . . . . .
H33 H 0.815524 0.030270 0.586750 0.019 Uiso 1 1 calc R . . . .
C34 C 0.77490(15) -0.05881(11) 0.51430(15) 0.0134(4) Uani 1 1 d . . . . .
C35 C 0.64113(15) -0.21403(11) 0.61410(14) 0.0128(4) Uani 1 1 d . . . . .
H35 H 0.632921 -0.246356 0.559587 0.015 Uiso 1 1 calc R . . . .
C36 C 0.66255(15) -0.12994(11) 0.75564(14) 0.0140(4) Uani 1 1 d . . . . .
H36 H 0.670883 -0.097877 0.810418 0.017 Uiso 1 1 calc R . . . .
C37 C 0.69338(15) -0.24823(11) 0.70077(14) 0.0143(4) Uani 1 1 d . . . . .
C38 C 0.72818(16) -0.31656(12) 0.70858(15) 0.0169(4) Uani 1 1 d . . . . .
H38 H 0.718447 -0.347484 0.657053 0.020 Uiso 1 1 calc R . . . .
C39 C 0.77781(17) -0.33965(13) 0.79301(17) 0.0214(5) Uani 1 1 d . . . . .
H39 H 0.803411 -0.386041 0.798648 0.026 Uiso 1 1 calc R . . . .
C40 C 0.78956(18) -0.29459(14) 0.86856(17) 0.0233(5) Uani 1 1 d . . . . .
H40 H 0.823090 -0.310566 0.925811 0.028 Uiso 1 1 calc R . . . .
C41 C 0.75279(17) -0.22618(13) 0.86155(15) 0.0203(4) Uani 1 1 d . . . . .
H41 H 0.760416 -0.195867 0.913731 0.024 Uiso 1 1 calc R . . . .
C42 C 0.70491(15) -0.20300(12) 0.77728(15) 0.0153(4) Uani 1 1 d . . . . .
C43 C 0.4943(2) 0.31287(16) 0.8916(2) 0.0335(6) Uani 1 1 d . . . . .
H43 H 0.516625 0.318738 0.959170 0.040 Uiso 1 1 calc R . . . .
Cl1 Cl 0.57938(5) 0.26230(4) 0.84397(7) 0.0452(2) Uani 1 1 d . . . . .
Cl2 Cl 0.38188(7) 0.26996(6) 0.87736(10) 0.0662(3) Uani 1 1 d . . . . .
Cl3 Cl 0.48225(6) 0.39655(4) 0.84023(8) 0.0545(3) Uani 1 1 d . . . . .
C44 C -0.0365(5) 0.0261(3) 0.8437(5) 0.0574(19) Uani 0.612(6) 1 d D U P A 1
H44A H -0.050906 -0.023902 0.832767 0.086 Uiso 0.612(6) 1 calc R . P A 1
H44B H -0.073317 0.043883 0.891248 0.086 Uiso 0.612(6) 1 calc R . P A 1
H44C H -0.054725 0.052488 0.786252 0.086 Uiso 0.612(6) 1 calc R . P A 1
C45 C 0.0689(7) 0.0352(5) 0.8751(11) 0.124(4) Uani 0.612(6) 1 d D U P A 1
H45A H 0.105877 0.016331 0.827400 0.149 Uiso 0.612(6) 1 calc R . P A 1
H45B H 0.087277 0.007722 0.932438 0.149 Uiso 0.612(6) 1 calc R . P A 1
C46 C 0.0956(5) 0.1113(4) 0.8930(8) 0.097(3) Uani 0.612(6) 1 d D U P A 1
H46A H 0.051045 0.140707 0.850337 0.116 Uiso 0.612(6) 1 calc R . P A 1
H46B H 0.084535 0.123086 0.956705 0.116 Uiso 0.612(6) 1 calc R . P A 1
C47 C 0.1964(6) 0.1307(4) 0.8825(6) 0.079(2) Uani 0.612(6) 1 d D U P A 1
H47A H 0.204067 0.181801 0.894975 0.095 Uiso 0.612(6) 1 calc R . P A 1
H47B H 0.204797 0.123205 0.817130 0.095 Uiso 0.612(6) 1 calc R . P A 1
C48 C 0.2787(6) 0.0927(6) 0.9424(7) 0.078(3) Uani 0.612(6) 1 d D U P A 1
H48A H 0.340927 0.110595 0.928465 0.117 Uiso 0.612(6) 1 calc R . P A 1
H48B H 0.273587 0.100937 1.007744 0.117 Uiso 0.612(6) 1 calc R . P A 1
H48C H 0.274320 0.042071 0.929542 0.117 Uiso 0.612(6) 1 calc R . P A 1
C49 C 0.0330(6) 0.1172(4) 0.9918(5) 0.0340(18) Uani 0.388(6) 1 d D U P A 2
H49A H -0.022689 0.137135 1.016972 0.051 Uiso 0.388(6) 1 calc R . P A 2
H49B H 0.065682 0.082875 1.035512 0.051 Uiso 0.388(6) 1 calc R . P A 2
H49C H 0.078263 0.154970 0.981812 0.051 Uiso 0.388(6) 1 calc R . P A 2
C51 C 0.0864(9) 0.0495(7) 0.8608(11) 0.111(4) Uani 0.388(6) 1 d D U P A 2
H51A H 0.111620 0.008985 0.899560 0.133 Uiso 0.388(6) 1 calc R . P A 2
H51B H 0.064418 0.031452 0.797839 0.133 Uiso 0.388(6) 1 calc R . P A 2
C50 C -0.0017(7) 0.0809(7) 0.9005(8) 0.084(3) Uani 0.388(6) 1 d D U P A 2
H50A H -0.035333 0.115295 0.856261 0.101 Uiso 0.388(6) 1 calc R . P A 2
H50B H -0.047945 0.043020 0.910094 0.101 Uiso 0.388(6) 1 calc R . P A 2
C52 C 0.1650(7) 0.0995(5) 0.8564(7) 0.044(2) Uani 0.388(6) 1 d D U P A 2
H52A H 0.140968 0.145582 0.875154 0.053 Uiso 0.388(6) 1 calc R . P A 2
H52B H 0.172485 0.103833 0.790311 0.053 Uiso 0.388(6) 1 calc R . P A 2
C53 C 0.2647(9) 0.0917(12) 0.9073(14) 0.095(5) Uani 0.388(6) 1 d D U P A 2
H53A H 0.304369 0.131818 0.893278 0.143 Uiso 0.388(6) 1 calc R . P A 2
H53B H 0.261715 0.090143 0.973803 0.143 Uiso 0.388(6) 1 calc R . P A 2
H53C H 0.293536 0.047991 0.888140 0.143 Uiso 0.388(6) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.380(3) . ?
C1 C6 1.411(3) . ?
C1 C7 1.529(3) . ?
C2 C3 1.408(3) . ?
C2 C36 1.533(3) 3_656 ?
C3 C4 1.381(3) . ?
C3 C35 1.523(3) 3_656 ?
C4 C5 1.403(3) . ?
C5 C6 1.378(3) . ?
C6 C8 1.523(3) . ?
C7 C9 1.524(3) . ?
C7 C15 1.526(3) . ?
C8 C14 1.518(3) . ?
C8 C20 1.531(3) . ?
C9 C10 1.385(3) . ?
C9 C14 1.403(3) . ?
C10 C11 1.397(3) . ?
C11 C12 1.385(4) . ?
C12 C13 1.401(3) . ?
C13 C14 1.385(3) . ?
C15 C16 1.381(3) . ?
C15 C20 1.412(3) . ?
C16 C17 1.399(3) . ?
C17 C18 1.387(3) . ?
C18 C19 1.408(3) . ?
C18 C21 1.527(3) . ?
C19 C20 1.381(3) . ?
C19 C22 1.531(3) . ?
C21 C23 1.523(3) . ?
C21 C29 1.527(3) . ?
C22 C28 1.518(3) . ?
C22 C34 1.523(3) . ?
C23 C24 1.386(3) . ?
C23 C28 1.403(3) . ?
C24 C25 1.400(3) . ?
C25 C26 1.388(4) . ?
C26 C27 1.403(3) . ?
C27 C28 1.386(3) . ?
C29 C30 1.382(3) . ?
C29 C34 1.414(3) . ?
C30 C31 1.412(3) . ?
C30 C35 1.535(3) . ?
C31 C32 1.378(3) . ?
C31 C36 1.519(3) . ?
C32 C33 1.407(3) . ?
C33 C34 1.381(3) . ?
C35 C37 1.517(3) . ?
C36 C42 1.524(3) . ?
C37 C38 1.385(3) . ?
C37 C42 1.402(3) . ?
C38 C39 1.399(3) . ?
C39 C40 1.389(4) . ?
C40 C41 1.395(4) . ?
C41 C42 1.389(3) . ?
C43 Cl1 1.745(3) . ?
C43 Cl2 1.753(3) . ?
C43 Cl3 1.756(3) . ?
C44 C45 1.488(9) . ?
C45 C46 1.507(8) . ?
C46 C47 1.482(8) . ?
C47 C48 1.525(8) . ?
C49 C50 1.520(9) . ?
C51 C50 1.549(8) . ?
C51 C52 1.459(9) . ?
C52 C53 1.489(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 119.12(19) . . ?
C2 C1 C7 128.16(19) . . ?
C6 C1 C7 112.57(18) . . ?
C1 C2 C3 119.43(19) . . ?
C1 C2 C36 128.08(19) . 3_656 ?
C3 C2 C36 112.36(18) . 3_656 ?
C2 C3 C35 113.45(18) . 3_656 ?
C4 C3 C2 121.10(19) . . ?
C4 C3 C35 125.38(19) . 3_656 ?
C3 C4 C5 119.57(19) . . ?
C6 C5 C4 119.29(19) . . ?
C1 C6 C8 113.30(18) . . ?
C5 C6 C1 121.40(19) . . ?
C5 C6 C8 125.16(19) . . ?
C9 C7 C1 106.46(17) . . ?
C9 C7 C15 106.16(17) . . ?
C15 C7 C1 104.65(16) . . ?
C6 C8 C20 104.35(16) . . ?
C14 C8 C6 106.72(17) . . ?
C14 C8 C20 105.90(17) . . ?
C10 C9 C7 126.7(2) . . ?
C10 C9 C14 120.4(2) . . ?
C14 C9 C7 112.89(18) . . ?
C9 C10 C11 118.9(2) . . ?
C12 C11 C10 120.8(2) . . ?
C11 C12 C13 120.3(2) . . ?
C14 C13 C12 119.0(2) . . ?
C9 C14 C8 113.47(18) . . ?
C13 C14 C8 126.0(2) . . ?
C13 C14 C9 120.6(2) . . ?
C16 C15 C7 126.22(19) . . ?
C16 C15 C20 120.72(19) . . ?
C20 C15 C7 113.02(18) . . ?
C15 C16 C17 119.9(2) . . ?
C18 C17 C16 119.4(2) . . ?
C17 C18 C19 121.1(2) . . ?
C17 C18 C21 125.82(19) . . ?
C19 C18 C21 113.02(18) . . ?
C18 C19 C22 112.75(18) . . ?
C20 C19 C18 119.19(19) . . ?
C20 C19 C22 127.95(19) . . ?
C15 C20 C8 112.74(18) . . ?
C19 C20 C8 127.50(19) . . ?
C19 C20 C15 119.68(19) . . ?
C18 C21 C29 104.33(16) . . ?
C23 C21 C18 106.65(17) . . ?
C23 C21 C29 106.25(17) . . ?
C28 C22 C19 106.59(17) . . ?
C28 C22 C34 105.86(16) . . ?
C34 C22 C19 104.95(16) . . ?
C24 C23 C21 126.4(2) . . ?
C24 C23 C28 120.5(2) . . ?
C28 C23 C21 113.10(18) . . ?
C23 C24 C25 119.1(2) . . ?
C26 C25 C24 120.7(2) . . ?
C25 C26 C27 120.1(2) . . ?
C28 C27 C26 119.4(2) . . ?
C23 C28 C22 113.16(18) . . ?
C27 C28 C22 126.6(2) . . ?
C27 C28 C23 120.2(2) . . ?
C30 C29 C21 128.03(19) . . ?
C30 C29 C34 119.27(19) . . ?
C34 C29 C21 112.64(17) . . ?
C29 C30 C31 119.22(19) . . ?
C29 C30 C35 127.95(18) . . ?
C31 C30 C35 112.72(17) . . ?
C30 C31 C36 113.01(18) . . ?
C32 C31 C30 121.24(19) . . ?
C32 C31 C36 125.66(19) . . ?
C31 C32 C33 119.8(2) . . ?
C34 C33 C32 119.07(19) . . ?
C29 C34 C22 113.03(18) . . ?
C33 C34 C22 125.56(19) . . ?
C33 C34 C29 121.39(19) . . ?
C3 C35 C30 104.37(16) 3_656 . ?
C37 C35 C3 105.94(16) . 3_656 ?
C37 C35 C30 106.72(16) . . ?
C31 C36 C2 103.65(16) . 3_656 ?
C31 C36 C42 106.90(17) . . ?
C42 C36 C2 106.79(17) . 3_656 ?
C38 C37 C35 126.31(19) . . ?
C38 C37 C42 120.6(2) . . ?
C42 C37 C35 113.11(18) . . ?
C37 C38 C39 119.4(2) . . ?
C40 C39 C38 119.8(2) . . ?
C39 C40 C41 120.9(2) . . ?
C42 C41 C40 119.1(2) . . ?
C37 C42 C36 113.22(18) . . ?
C41 C42 C36 126.7(2) . . ?
C41 C42 C37 120.1(2) . . ?
Cl1 C43 Cl2 110.05(16) . . ?
Cl1 C43 Cl3 110.94(18) . . ?
Cl2 C43 Cl3 109.85(16) . . ?
C44 C45 C46 111.9(8) . . ?
C47 C46 C45 115.8(7) . . ?
C46 C47 C48 118.1(7) . . ?
C52 C51 C50 113.9(8) . . ?
C49 C50 C51 109.4(7) . . ?
C51 C52 C53 124.6(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 3.4(3) . . . . ?
C1 C2 C3 C35 -173.75(18) . . . 3_656 ?
C1 C6 C8 C14 55.5(2) . . . . ?
C1 C6 C8 C20 -56.3(2) . . . . ?
C1 C7 C9 C10 -124.3(2) . . . . ?
C1 C7 C9 C14 56.6(2) . . . . ?
C1 C7 C15 C16 121.9(2) . . . . ?
C1 C7 C15 C20 -56.0(2) . . . . ?
C2 C1 C6 C5 -1.0(3) . . . . ?
C2 C1 C6 C8 174.99(18) . . . . ?
C2 C1 C7 C9 129.8(2) . . . . ?
C2 C1 C7 C15 -118.1(2) . . . . ?
C2 C3 C4 C5 -2.2(3) . . . . ?
C2 C36 C42 C37 55.2(2) 3_656 . . . ?
C2 C36 C42 C41 -126.1(2) 3_656 . . . ?
C3 C4 C5 C6 -0.6(3) . . . . ?
C3 C35 C37 C38 124.5(2) 3_656 . . . ?
C3 C35 C37 C42 -55.7(2) 3_656 . . . ?
C4 C5 C6 C1 2.2(3) . . . . ?
C4 C5 C6 C8 -173.30(19) . . . . ?
C5 C6 C8 C14 -128.7(2) . . . . ?
C5 C6 C8 C20 119.5(2) . . . . ?
C6 C1 C2 C3 -1.8(3) . . . . ?
C6 C1 C2 C36 -177.3(2) . . . 3_656 ?
C6 C1 C7 C9 -54.6(2) . . . . ?
C6 C1 C7 C15 57.5(2) . . . . ?
C6 C8 C14 C9 -53.9(2) . . . . ?
C6 C8 C14 C13 126.0(2) . . . . ?
C6 C8 C20 C15 57.8(2) . . . . ?
C6 C8 C20 C19 -119.0(2) . . . . ?
C7 C1 C2 C3 173.6(2) . . . . ?
C7 C1 C2 C36 -1.9(4) . . . 3_656 ?
C7 C1 C6 C5 -177.03(19) . . . . ?
C7 C1 C6 C8 -1.1(2) . . . . ?
C7 C9 C10 C11 -178.2(2) . . . . ?
C7 C9 C14 C8 -2.0(3) . . . . ?
C7 C9 C14 C13 178.2(2) . . . . ?
C7 C15 C16 C17 -176.7(2) . . . . ?
C7 C15 C20 C8 -1.5(2) . . . . ?
C7 C15 C20 C19 175.54(18) . . . . ?
C9 C7 C15 C16 -125.8(2) . . . . ?
C9 C7 C15 C20 56.4(2) . . . . ?
C9 C10 C11 C12 0.0(4) . . . . ?
C10 C9 C14 C8 178.9(2) . . . . ?
C10 C9 C14 C13 -1.0(3) . . . . ?
C10 C11 C12 C13 -0.8(4) . . . . ?
C11 C12 C13 C14 0.6(4) . . . . ?
C12 C13 C14 C8 -179.6(2) . . . . ?
C12 C13 C14 C9 0.2(3) . . . . ?
C14 C8 C20 C15 -54.7(2) . . . . ?
C14 C8 C20 C19 128.6(2) . . . . ?
C14 C9 C10 C11 0.8(4) . . . . ?
C15 C7 C9 C10 124.5(2) . . . . ?
C15 C7 C9 C14 -54.5(2) . . . . ?
C15 C16 C17 C18 0.7(3) . . . . ?
C16 C15 C20 C8 -179.52(19) . . . . ?
C16 C15 C20 C19 -2.5(3) . . . . ?
C16 C17 C18 C19 -1.0(3) . . . . ?
C16 C17 C18 C21 175.9(2) . . . . ?
C17 C18 C19 C20 -0.4(3) . . . . ?
C17 C18 C19 C22 176.19(19) . . . . ?
C17 C18 C21 C23 128.4(2) . . . . ?
C17 C18 C21 C29 -119.4(2) . . . . ?
C18 C19 C20 C8 178.67(19) . . . . ?
C18 C19 C20 C15 2.1(3) . . . . ?
C18 C19 C22 C28 56.0(2) . . . . ?
C18 C19 C22 C34 -56.0(2) . . . . ?
C18 C21 C23 C24 -124.6(2) . . . . ?
C18 C21 C23 C28 55.7(2) . . . . ?
C18 C21 C29 C30 119.7(2) . . . . ?
C18 C21 C29 C34 -57.3(2) . . . . ?
C19 C18 C21 C23 -54.4(2) . . . . ?
C19 C18 C21 C29 57.8(2) . . . . ?
C19 C22 C28 C23 -55.0(2) . . . . ?
C19 C22 C28 C27 126.2(2) . . . . ?
C19 C22 C34 C29 56.4(2) . . . . ?
C19 C22 C34 C33 -122.1(2) . . . . ?
C20 C8 C14 C9 56.9(2) . . . . ?
C20 C8 C14 C13 -123.3(2) . . . . ?
C20 C15 C16 C17 1.0(3) . . . . ?
C20 C19 C22 C28 -127.8(2) . . . . ?
C20 C19 C22 C34 120.2(2) . . . . ?
C21 C18 C19 C20 -177.71(18) . . . . ?
C21 C18 C19 C22 -1.1(2) . . . . ?
C21 C23 C24 C25 -179.0(2) . . . . ?
C21 C23 C28 C22 -0.8(3) . . . . ?
C21 C23 C28 C27 178.2(2) . . . . ?
C21 C29 C30 C31 -178.30(19) . . . . ?
C21 C29 C30 C35 -2.5(3) . . . . ?
C21 C29 C34 C22 0.4(2) . . . . ?
C21 C29 C34 C33 179.00(19) . . . . ?
C22 C19 C20 C8 2.7(4) . . . . ?
C22 C19 C20 C15 -173.89(19) . . . . ?
C23 C21 C29 C30 -127.8(2) . . . . ?
C23 C21 C29 C34 55.1(2) . . . . ?
C23 C24 C25 C26 0.4(4) . . . . ?
C24 C23 C28 C22 179.5(2) . . . . ?
C24 C23 C28 C27 -1.6(3) . . . . ?
C24 C25 C26 C27 -0.7(4) . . . . ?
C25 C26 C27 C28 -0.1(4) . . . . ?
C26 C27 C28 C22 -180.0(2) . . . . ?
C26 C27 C28 C23 1.2(4) . . . . ?
C28 C22 C34 C29 -56.1(2) . . . . ?
C28 C22 C34 C33 125.4(2) . . . . ?
C28 C23 C24 C25 0.7(4) . . . . ?
C29 C21 C23 C24 124.6(2) . . . . ?
C29 C21 C23 C28 -55.2(2) . . . . ?
C29 C30 C31 C32 -0.2(3) . . . . ?
C29 C30 C31 C36 176.51(18) . . . . ?
C29 C30 C35 C3 -119.3(2) . . . 3_656 ?
C29 C30 C35 C37 128.8(2) . . . . ?
C30 C29 C34 C22 -176.97(18) . . . . ?
C30 C29 C34 C33 1.6(3) . . . . ?
C30 C31 C32 C33 1.5(3) . . . . ?
C30 C31 C36 C2 -57.8(2) . . . 3_656 ?
C30 C31 C36 C42 54.8(2) . . . . ?
C30 C35 C37 C38 -124.7(2) . . . . ?
C30 C35 C37 C42 55.2(2) . . . . ?
C31 C30 C35 C3 56.7(2) . . . 3_656 ?
C31 C30 C35 C37 -55.2(2) . . . . ?
C31 C32 C33 C34 -1.3(3) . . . . ?
C31 C36 C42 C37 -55.2(2) . . . . ?
C31 C36 C42 C41 123.5(2) . . . . ?
C32 C31 C36 C2 118.7(2) . . . 3_656 ?
C32 C31 C36 C42 -128.7(2) . . . . ?
C32 C33 C34 C22 178.1(2) . . . . ?
C32 C33 C34 C29 -0.3(3) . . . . ?
C34 C22 C28 C23 56.4(2) . . . . ?
C34 C22 C28 C27 -122.5(2) . . . . ?
C34 C29 C30 C31 -1.4(3) . . . . ?
C34 C29 C30 C35 174.38(19) . . . . ?
C35 C3 C4 C5 174.6(2) 3_656 . . . ?
C35 C30 C31 C32 -176.56(19) . . . . ?
C35 C30 C31 C36 0.1(2) . . . . ?
C35 C37 C38 C39 177.9(2) . . . . ?
C35 C37 C42 C36 -0.1(3) . . . . ?
C35 C37 C42 C41 -178.96(19) . . . . ?
C36 C2 C3 C4 179.56(19) 3_656 . . . ?
C36 C2 C3 C35 2.4(2) 3_656 . . 3_656 ?
C36 C31 C32 C33 -174.7(2) . . . . ?
C37 C38 C39 C40 1.6(3) . . . . ?
C38 C37 C42 C36 179.75(19) . . . . ?
C38 C37 C42 C41 0.9(3) . . . . ?
C38 C39 C40 C41 -0.2(4) . . . . ?
C39 C40 C41 C42 -0.8(4) . . . . ?
C40 C41 C42 C36 -178.2(2) . . . . ?
C40 C41 C42 C37 0.4(3) . . . . ?
C42 C37 C38 C39 -2.0(3) . . . . ?
C44 C45 C46 C47 -153.1(10) . . . . ?
C45 C46 C47 C48 -58.7(13) . . . . ?
C50 C51 C52 C53 118.1(15) . . . . ?
C52 C51 C50 C49 -51.2(15) . . . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.148
_oxdiff_exptl_absorpt_empirical_full_min 0.888
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1997771'
loop_
_audit_author_name
_audit_author_address
'Yasutomo Segawa'
;Nagoya University
Japan
;
_audit_update_record             
;
2020-04-19 deposited with the CCDC.	2020-06-04 downloaded from the CCDC.
;
_audit_creation_date             2020-04-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C96 H72 O12), 6(C4 H8 O2), 0.5(C4 O2)'
_chemical_formula_sum            'C74 H84 O19'
_chemical_formula_weight         1277.41
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_symmetry_space_group_name_H-M_alt 'R -3'
_cell_length_a                   31.0383(8)
_cell_length_b                   31.0383(8)
_cell_length_c                   11.8708(4)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                120.0
_cell_volume                     9903.9(5)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9468
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      22.8020
_cell_measurement_theta_min      2.2600
_cell_oxdiff_angle_alpha         90.015(2)
_cell_oxdiff_angle_beta          89.998(3)
_cell_oxdiff_angle_gamma         119.907(3)
_cell_oxdiff_length_a            31.0312(10)
_cell_oxdiff_length_b            31.0228(9)
_cell_oxdiff_length_c            11.8682(4)
_cell_oxdiff_measurement_reflns_used 9486
_cell_oxdiff_volume              9903.9(5)
_shelx_estimated_absorpt_T_max   0.995
_shelx_estimated_absorpt_T_min   0.991
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4080
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            45408
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.062
_diffrn_reflns_theta_min         1.875
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -105.00  75.00   0.50   25.00    --  -15.00  45.00   0.00  360
  2  ω   -105.00  75.00   0.50   25.00    --  -15.00  45.00  90.00  360
  3  ω   -105.00  75.00   0.50   25.00    --  -15.00  45.00 180.00  360
  4  ω   -105.00  75.00   0.50   25.00    --  -15.00  45.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0081980333
_diffrn_orient_matrix_UB_12      0.0058746667
_diffrn_orient_matrix_UB_13      0.0566138667
_diffrn_orient_matrix_UB_21      -0.0197739667
_diffrn_orient_matrix_UB_22      0.0045990667
_diffrn_orient_matrix_UB_23      0.0115965667
_diffrn_orient_matrix_UB_31      -0.0153981333
_diffrn_orient_matrix_UB_32      -0.0252986667
_diffrn_orient_matrix_UB_33      0.0152376333
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2467
_reflns_number_total             5068
_reflns_odcompleteness_completeness 94.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.00
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    ?
_refine_diff_density_max         1.212
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.510
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5068
_refine_ls_number_restraints     119
_refine_ls_R_factor_all          0.2302
_refine_ls_R_factor_gt           0.1465
_refine_ls_restrained_S_all      1.568
_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          0.4100
_refine_ls_wR_factor_ref         0.4520
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17-C18 = C19-C20 = C21-C22 = C23-C24
 1.53 with sigma of 0.01
 O3-C17 = O3-C20 = O4-C18 = O4-C19 = O7-C25
 1.43 with sigma of 0.01
 O5-C21 = O5-C24 = O6-C22 = O6-C23
 1.43 with sigma of 0.01
 C17-C20 = C18-C19 = C21-C24 = C22-C23
 2.34 with sigma of 0.02
 O3-C18 = O3-C19 = O4-C17 = O4-C20
 2.43 with sigma of 0.02
 O5-C22 = O5-C23 = O6-C21 = O6-C24
 2.43 with sigma of 0.02
 C17-C19 = C18-C20 = C21-C23 = C22-C24
 2.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim O5 \\sim O6 \\sim O7: within
2A with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq,
Uanis(O7) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C25(0.66667)
5.a Ternary CH refined with riding coordinates:
 C7(H), C8(H8)
5.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C10(H10), C13(H13)
5.d Idealised Me refined as rotating group:
 C15(H15A,H15B,HA), C16(H16A,H16B,H16C)
;
_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
C1 C 0.02078(15) 0.88237(15) 0.5096(4) 0.0482(11) Uani 1 1 d . . . . .
C2 C 0.06901(15) 0.92040(15) 0.5081(4) 0.0498(11) Uani 1 1 d . . . . .
C3 C 0.09011(15) 0.94918(15) 0.6042(4) 0.0482(11) Uani 1 1 d . . . . .
C4 C 0.06250(16) 0.94037(15) 0.6998(4) 0.0518(11) Uani 1 1 d . . . . .
H4 H 0.077129 0.959795 0.765447 0.062 Uiso 1 1 calc R . . . .
C5 C 0.01289(17) 0.90287(16) 0.7010(4) 0.0537(12) Uani 1 1 d . . . . .
H5 H -0.006653 0.896998 0.766849 0.064 Uiso 1 1 calc R . . . .
C6 C -0.00763(16) 0.87452(15) 0.6069(4) 0.0501(11) Uani 1 1 d . . . . .
C7 C -0.00895(15) 0.84787(15) 0.4137(4) 0.0499(11) Uani 1 1 d . . . . .
H H 0.011285 0.852639 0.344385 0.060 Uiso 1 1 calc R . . . .
C8 C -0.06124(15) 0.83413(15) 0.5934(4) 0.0501(11) Uani 1 1 d . . . . .
H8 H -0.081559 0.828670 0.662866 0.060 Uiso 1 1 calc R . . . .
C9 C -0.03290(15) 0.79536(15) 0.4611(4) 0.0527(12) Uani 1 1 d . . . . .
C10 C -0.02903(16) 0.75663(16) 0.4143(4) 0.0562(12) Uani 1 1 d . . . . .
H10 H -0.010170 0.761425 0.347664 0.067 Uiso 1 1 calc R . . . .
C11 C -0.05362(17) 0.71019(16) 0.4675(5) 0.0631(14) Uani 1 1 d . . . . .
C12 C -0.07975(17) 0.70379(17) 0.5647(5) 0.0628(13) Uani 1 1 d . . . . .
C13 C -0.08322(17) 0.74354(16) 0.6099(4) 0.0591(13) Uani 1 1 d . . . . .
H13 H -0.101417 0.739355 0.677309 0.071 Uiso 1 1 calc R . . . .
C14 C -0.06017(16) 0.78846(16) 0.5562(4) 0.0518(11) Uani 1 1 d . . . . .
O1 O -0.05205(14) 0.66919(12) 0.4276(3) 0.0782(11) Uani 1 1 d . . . . .
C15 C -0.0281(3) 0.6740(2) 0.3286(6) 0.099(2) Uani 1 1 d . . . . .
H15A H -0.042562 0.685141 0.269873 0.148 Uiso 1 1 calc GR . . . .
H15B H -0.031773 0.641879 0.307191 0.148 Uiso 1 1 calc GR . . . .
HA H 0.007266 0.698585 0.337291 0.148 Uiso 1 1 calc GR . . . .
O2 O -0.10250(15) 0.65711(12) 0.6114(4) 0.0837(13) Uani 1 1 d . . . . .
C16 C -0.1143(3) 0.6547(2) 0.7277(6) 0.096(2) Uani 1 1 d . . . . .
H16A H -0.083541 0.671064 0.771827 0.144 Uiso 1 1 calc GR . . . .
H16B H -0.134131 0.619804 0.750785 0.144 Uiso 1 1 calc GR . . . .
H16C H -0.133449 0.671553 0.740560 0.144 Uiso 1 1 calc GR . . . .
O3 O 0.1262(3) 0.8518(2) 0.7475(6) 0.152(3) Uani 1 1 d D . . . .
C17 C 0.1561(3) 0.8363(3) 0.6878(9) 0.161(5) Uani 1 1 d D . . . .
H17A H 0.189470 0.851522 0.722669 0.193 Uiso 1 1 calc R . . . .
H17B H 0.160116 0.847924 0.608798 0.193 Uiso 1 1 calc R . . . .
C18 C 0.1324(3) 0.7805(3) 0.6898(8) 0.132(3) Uani 1 1 d D . . . .
H18A H 0.152503 0.770317 0.644067 0.158 Uiso 1 1 calc R . . . .
H18B H 0.131444 0.769087 0.768098 0.158 Uiso 1 1 calc R . . . .
O4 O 0.08399(19) 0.75853(17) 0.6465(5) 0.1240(18) Uani 1 1 d D . . . .
C19 C 0.0544(2) 0.7756(3) 0.6985(7) 0.118(3) Uani 1 1 d D . . . .
H19A H 0.049075 0.765427 0.778713 0.141 Uiso 1 1 calc R . . . .
H19B H 0.021514 0.760557 0.661143 0.141 Uiso 1 1 calc R . . . .
C20 C 0.0799(3) 0.8312(3) 0.6901(8) 0.137(3) Uani 1 1 d D . . . .
H20A H 0.085409 0.841469 0.610066 0.164 Uiso 1 1 calc R . . . .
H20B H 0.058835 0.843306 0.724544 0.164 Uiso 1 1 calc R . . . .
O5 O 0.0704(5) 0.8887(5) 0.1067(9) 0.296(6) Uani 1 1 d D U . . .
C21 C 0.0678(6) 0.8871(5) -0.0162(10) 0.248(6) Uani 1 1 d D U . . .
H21A H 0.092877 0.879486 -0.047432 0.298 Uiso 1 1 calc R . . . .
H21B H 0.074554 0.919606 -0.046311 0.298 Uiso 1 1 calc R . . . .
C22 C 0.0162(6) 0.8470(5) -0.0485(11) 0.241(6) Uani 1 1 d D U . . .
H22A H -0.007918 0.856435 -0.020112 0.289 Uiso 1 1 calc R . . . .
H22B H 0.013724 0.845480 -0.131714 0.289 Uiso 1 1 calc R . . . .
O6 O 0.0022(6) 0.7989(4) -0.0076(10) 0.288(5) Uani 1 1 d D U . . .
C23 C 0.0050(7) 0.8030(5) 0.1129(10) 0.263(6) Uani 1 1 d D U . . .
H23A H -0.004865 0.770313 0.147296 0.316 Uiso 1 1 calc R . . . .
H23B H -0.017654 0.814436 0.140981 0.316 Uiso 1 1 calc R . . . .
C24 C 0.0592(6) 0.8410(6) 0.1438(11) 0.234(5) Uani 1 1 d D U . . .
H24A H 0.063766 0.841343 0.226451 0.281 Uiso 1 1 calc R . . . .
H24B H 0.082039 0.831512 0.107710 0.281 Uiso 1 1 calc R . . . .
O7 O 0.000000 1.000000 0.1168(9) 0.154(4) Uani 1 3 d DS TU P . .
C25 C 0.0442(5) 1.0243(7) 0.0546(9) 0.168(6) Uani 0.6667 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.367(6) . ?
C1 C6 1.398(6) . ?
C1 C7 1.519(6) . ?
C2 C3 1.394(6) . ?
C2 C8 1.539(6) 12_666 ?
C3 C4 1.365(6) . ?
C3 C7 1.519(6) 12_666 ?
C4 C5 1.390(6) . ?
C5 C6 1.366(6) . ?
C6 C8 1.510(6) . ?
C7 C9 1.522(6) . ?
C8 C14 1.501(6) . ?
C9 C10 1.383(6) . ?
C9 C14 1.362(6) . ?
C10 C11 1.400(7) . ?
C11 C12 1.367(7) . ?
C11 O1 1.381(6) . ?
C12 C13 1.398(6) . ?
C12 O2 1.372(6) . ?
C13 C14 1.366(6) . ?
O1 C15 1.358(7) . ?
O2 C16 1.420(7) . ?
O3 C17 1.428(8) . ?
O3 C20 1.421(7) . ?
C17 C18 1.506(8) . ?
C18 O4 1.402(7) . ?
O4 C19 1.411(7) . ?
C19 C20 1.500(7) . ?
O5 C21 1.461(9) . ?
O5 C24 1.411(9) . ?
C21 C22 1.507(9) . ?
C22 O6 1.415(9) . ?
O6 C23 1.435(9) . ?
C23 C24 1.541(9) . ?
O7 C25 1.402(9) 2_675 ?
O7 C25 1.402(9) 3_465 ?
O7 C25 1.402(9) . ?
C25 C25 1.760(19) 12_665 ?
C25 C25 1.760(19) 11_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 119.0(4) . . ?
C2 C1 C7 128.0(4) . . ?
C6 C1 C7 112.9(4) . . ?
C1 C2 C3 120.2(4) . . ?
C1 C2 C8 127.2(4) . 12_666 ?
C3 C2 C8 112.5(4) . 12_666 ?
C2 C3 C7 113.3(4) . 12_666 ?
C4 C3 C2 120.3(4) . . ?
C4 C3 C7 126.3(4) . 12_666 ?
C3 C4 C5 119.8(4) . . ?
C6 C5 C4 119.7(4) . . ?
C1 C6 C8 113.2(4) . . ?
C5 C6 C1 120.8(4) . . ?
C5 C6 C8 125.9(4) . . ?
C1 C7 C9 106.1(3) . . ?
C3 C7 C1 103.4(3) 11_456 . ?
C3 C7 C9 106.3(3) 11_456 . ?
C6 C8 C2 103.9(3) . 11_456 ?
C14 C8 C2 106.6(4) . 11_456 ?
C14 C8 C6 106.2(3) . . ?
C10 C9 C7 125.0(4) . . ?
C14 C9 C7 114.0(4) . . ?
C14 C9 C10 120.9(4) . . ?
C9 C10 C11 118.3(5) . . ?
C12 C11 C10 120.6(4) . . ?
C12 C11 O1 116.6(4) . . ?
O1 C11 C10 122.8(5) . . ?
C11 C12 C13 119.9(4) . . ?
C11 C12 O2 116.7(4) . . ?
O2 C12 C13 123.4(5) . . ?
C14 C13 C12 119.3(5) . . ?
C9 C14 C8 113.6(4) . . ?
C9 C14 C13 121.0(4) . . ?
C13 C14 C8 125.4(4) . . ?
C15 O1 C11 117.6(4) . . ?
C12 O2 C16 115.6(4) . . ?
C20 O3 C17 106.9(6) . . ?
O3 C17 C18 110.8(6) . . ?
O4 C18 C17 110.0(6) . . ?
C18 O4 C19 113.4(6) . . ?
O4 C19 C20 109.6(6) . . ?
O3 C20 C19 108.6(5) . . ?
C24 O5 C21 107.2(9) . . ?
O5 C21 C22 107.4(9) . . ?
O6 C22 C21 115.0(10) . . ?
C22 O6 C23 106.0(10) . . ?
O6 C23 C24 107.4(10) . . ?
O5 C24 C23 109.2(10) . . ?
C25 O7 C25 94.8(9) . 3_465 ?
C25 O7 C25 94.8(9) . 2_675 ?
C25 O7 C25 94.8(9) 3_465 2_675 ?
O7 C25 C25 95.8(6) . 12_665 ?
O7 C25 C25 95.8(6) . 11_455 ?
C25 C25 C25 71.8(7) 12_665 11_455 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -1.5(6) . . . . ?
C1 C2 C3 C7 -177.6(4) . . . 12_666 ?
C1 C6 C8 C2 -56.6(4) . . . 11_456 ?
C1 C6 C8 C14 55.6(5) . . . . ?
C1 C7 C9 C10 -126.6(4) . . . . ?
C1 C7 C9 C14 54.3(5) . . . . ?
C2 C1 C6 C5 -2.8(6) . . . . ?
C2 C1 C6 C8 175.3(4) . . . . ?
C2 C1 C7 C3 -117.3(4) . . . 11_456 ?
C2 C1 C7 C9 131.0(4) . . . . ?
C2 C3 C4 C5 -0.8(6) . . . . ?
C2 C8 C14 C9 54.6(5) 11_456 . . . ?
C2 C8 C14 C13 -126.0(5) 11_456 . . . ?
C3 C4 C5 C6 1.2(6) . . . . ?
C3 C7 C9 C10 123.8(4) 11_456 . . . ?
C3 C7 C9 C14 -55.3(5) 11_456 . . . ?
C4 C5 C6 C1 0.6(6) . . . . ?
C4 C5 C6 C8 -177.2(4) . . . . ?
C5 C6 C8 C2 121.4(4) . . . 11_456 ?
C5 C6 C8 C14 -126.4(5) . . . . ?
C6 C1 C2 C3 3.2(6) . . . . ?
C6 C1 C2 C8 -173.0(4) . . . 12_666 ?
C6 C1 C7 C3 58.3(4) . . . 11_456 ?
C6 C1 C7 C9 -53.4(4) . . . . ?
C6 C8 C14 C9 -55.7(5) . . . . ?
C6 C8 C14 C13 123.6(5) . . . . ?
C7 C1 C2 C3 178.5(4) . . . . ?
C7 C1 C2 C8 2.3(7) . . . 12_666 ?
C7 C1 C6 C5 -178.8(4) . . . . ?
C7 C1 C6 C8 -0.7(5) . . . . ?
C7 C3 C4 C5 174.8(4) 12_666 . . . ?
C7 C9 C10 C11 -179.5(4) . . . . ?
C7 C9 C14 C8 0.6(5) . . . . ?
C7 C9 C14 C13 -178.8(4) . . . . ?
C8 C2 C3 C4 175.3(4) 12_666 . . . ?
C8 C2 C3 C7 -0.9(5) 12_666 . . 12_666 ?
C9 C10 C11 C12 -1.5(7) . . . . ?
C9 C10 C11 O1 -179.9(4) . . . . ?
C10 C9 C14 C8 -178.6(4) . . . . ?
C10 C9 C14 C13 2.0(7) . . . . ?
C10 C11 C12 C13 1.9(7) . . . . ?
C10 C11 C12 O2 -179.7(4) . . . . ?
C10 C11 O1 C15 -4.3(7) . . . . ?
C11 C12 C13 C14 -0.2(7) . . . . ?
C11 C12 O2 C16 159.2(5) . . . . ?
C12 C11 O1 C15 177.3(5) . . . . ?
C12 C13 C14 C8 179.0(4) . . . . ?
C12 C13 C14 C9 -1.7(7) . . . . ?
C13 C12 O2 C16 -22.4(7) . . . . ?
C14 C9 C10 C11 -0.4(7) . . . . ?
O1 C11 C12 C13 -179.7(4) . . . . ?
O1 C11 C12 O2 -1.2(7) . . . . ?
O2 C12 C13 C14 -178.6(4) . . . . ?
O3 C17 C18 O4 55.8(10) . . . . ?
C17 O3 C20 C19 64.5(9) . . . . ?
C17 C18 O4 C19 -52.4(9) . . . . ?
C18 O4 C19 C20 55.6(8) . . . . ?
O4 C19 C20 O3 -61.3(9) . . . . ?
C20 O3 C17 C18 -62.4(9) . . . . ?
O5 C21 C22 O6 -58.6(19) . . . . ?
C21 O5 C24 C23 -65.0(16) . . . . ?
C21 C22 O6 C23 60.0(18) . . . . ?
C22 O6 C23 C24 -60.7(17) . . . . ?
O6 C23 C24 O5 67.5(17) . . . . ?
C24 O5 C21 C22 58.4(17) . . . . ?
C25 O7 C25 C25 -11.5(7) 2_675 . . 12_665 ?
C25 O7 C25 C25 -83.7(6) 2_675 . . 11_455 ?
C25 O7 C25 C25 83.7(6) 3_465 . . 12_665 ?
C25 O7 C25 C25 11.5(7) 3_465 . . 11_455 ?

_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 1.264
_oxdiff_exptl_absorpt_empirical_full_min 0.822
####################################################################### 
# 
# 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_12
_database_code_depnum_ccdc_archive 'CCDC 1997773'
loop_
_audit_author_name
_audit_author_address
'Yasutomo Segawa'
;Nagoya University
Japan
;
_audit_update_record             
;
2020-04-19 deposited with the CCDC.	2020-06-04 downloaded from the CCDC.
;
_audit_creation_date             2020-04-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C168 H96, 3(C H2 Cl2), 6(C5 H12)'
_chemical_formula_sum            'C201 H174 Cl6'
_chemical_formula_weight         2802.09
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_symmetry_space_group_name_H-M_alt 'C 1 2/m 1'
_cell_length_a                   46.422(4)
_cell_length_b                   7.7267(6)
_cell_length_c                   46.356(4)
_cell_angle_alpha                90.0
_cell_angle_beta                 109.884(10)
_cell_angle_gamma                90.0
_cell_volume                     15636(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4157
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      18.8560
_cell_measurement_theta_min      2.3450
_cell_oxdiff_angle_alpha         89.982(7)
_cell_oxdiff_angle_beta          109.893(6)
_cell_oxdiff_angle_gamma         89.993(7)
_cell_oxdiff_length_a            46.431(3)
_cell_oxdiff_length_b            7.7254(8)
_cell_oxdiff_length_c            46.357(3)
_cell_oxdiff_measurement_reflns_used 4161
_cell_oxdiff_volume              15636(2)
_shelx_estimated_absorpt_T_max   0.998
_shelx_estimated_absorpt_T_min   0.992
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5928
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.4476
_diffrn_reflns_av_unetI/netI     0.4720
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            92326
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.991
_diffrn_reflns_theta_min         1.866
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50  100.00    --  -20.00  45.00   0.00  360
  2  ω   -110.00  70.00   0.50  100.00    --  -20.00  45.00  70.00  360
  3  ω   -110.00  70.00   0.50  100.00    --  -20.00  45.00 140.00  360
  4  ω   -110.00  70.00   0.50  100.00    --  -20.00  45.00 210.00  360
  5  ω   -110.00  70.00   0.50  100.00    --  -20.00  45.00 280.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0004917000
_diffrn_orient_matrix_UB_12      -0.0911997000
_diffrn_orient_matrix_UB_13      -0.0018667000
_diffrn_orient_matrix_UB_21      -0.0162382000
_diffrn_orient_matrix_UB_22      0.0027401000
_diffrn_orient_matrix_UB_23      -0.0054138000
_diffrn_orient_matrix_UB_31      -0.0000735000
_diffrn_orient_matrix_UB_32      0.0102411000
_diffrn_orient_matrix_UB_33      -0.0152301000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4075
_reflns_number_total             15814
_reflns_odcompleteness_completeness 92.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.93
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    ?
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1039
_refine_ls_number_reflns         15814
_refine_ls_number_restraints     270
_refine_ls_R_factor_all          0.4275
_refine_ls_R_factor_gt           0.1677
_refine_ls_restrained_S_all      1.031
_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)+(0.1885P)²+69.9761P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3823
_refine_ls_wR_factor_ref         0.4979
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C92-C93 = C93-C94 = C94-C95 = C95-C96
 1.54 with sigma of 0.01
 C92-C94 = C94-C96 = C93-C95
 2.54 with sigma of 0.02
 C85-Cl1 = C85-Cl2 = C86-Cl3 = C85-Cl4
 1.76 with sigma of 0.01
 Cl1-Cl2 = Cl3-Cl3_$1 = Cl2-Cl4
 2.85 with sigma of 0.02
 C1A-C98A
 2.54 with sigma of 0.02
 C99A-C97A
 2.54 with sigma of 0.02
 C97-C98 = C98-C99 = C99-C100 = C100-C101
 1.54 with sigma of 0.01
 C97-C99 = C98-C100 = C99-C101
 2.54 with sigma of 0.02
 C1B-C99A
 2.54 with sigma of 0.02
 C89A-C87A
 2.54 with sigma of 0.02
 C88A-C90A
 2.54 with sigma of 0.02
 C87-C88 = C88-C89 = C89-C90 = C90-C91
 1.54 with sigma of 0.01
 C87-C89 = C89-C91 = C88-C90
 2.54 with sigma of 0.02
 C91A-C89A
 2.54 with sigma of 0.02
 C99A-C1A = C1B-C1A = C99A-C98A = C98A-C97A = C88A-C87A = C89A-C88A = C90A-
 C89A = C91A-C90A
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C97) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C100)
\\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq:
with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C87) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C90)
\\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C93) \\sim Ueq,
Uanis(C94) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C96) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.02
Uanis(C90A) \\sim Ueq, Uanis(C98A) \\sim Ueq, Uanis(C97A) \\sim Ueq,
Uanis(C91A) \\sim Ueq, Uanis(C99A) \\sim Ueq, Uanis(C88A) \\sim Ueq,
Uanis(C87A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C100, C97, C99, C98, C101, C97A, C98A, C99A, C1A, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C89, C90, C91, C88, C87, C89A, C90A, C91A, C88A, C87A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H85C)=Sof(H85D)=Sof(Cl4)=1-FVAR(1)
 Sof(Cl1)=Sof(H85A)=Sof(H85B)=FVAR(1)
 Sof(C97A)=Sof(H97D)=Sof(H97E)=Sof(H97F)=Sof(C98A)=Sof(H98C)=Sof(H98D)=
 Sof(C99A)=Sof(H99C)=Sof(H99D)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=Sof(H1BA)=
 Sof(H1BB)=Sof(H1BC)=1-FVAR(2)
 Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(C97)=Sof(H97A)=Sof(H97B)=Sof(H97C)=Sof(C99)=
 Sof(H99A)=Sof(H99B)=Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(C101)=Sof(H10C)=Sof(H10D)=
 Sof(H10E)=FVAR(2)
 Sof(C89A)=Sof(H89C)=Sof(H89D)=Sof(C90A)=Sof(H90C)=Sof(H90D)=Sof(C91A)=
 Sof(H91D)=Sof(H91E)=Sof(H91F)=Sof(C88A)=Sof(H88C)=Sof(H88D)=Sof(C87A)=
 Sof(H87D)=Sof(H87E)=Sof(H87F)=1-FVAR(3)
 Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(C91)=Sof(H91A)=
 Sof(H91B)=Sof(H91C)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(C87)=Sof(H87A)=Sof(H87B)=
 Sof(H87C)=FVAR(3)
 Fixed Sof: C86(0.5) H86A(0.5) H86B(0.5)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C8(H8), C15(H15), C16(H16), C23(H23), C24(H24), C31(H31), C32(H32),
 C51(H51), C52(H52), C71(H71), C72(H72)
6.b Secondary CH2 refined with riding coordinates:
 C85(H85A,H85B), C85(H85C,H85D), C86(H86A,H86B), C89(H89A,H89B), C90(H90A,
 H90B), C88(H88A,H88B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B),
 C100(H10A,H10B), C99(H99A,H99B), C98(H98A,H98B), C98A(H98C,H98D), C99A(H99C,
 H99D), C1A(H1AA,H1AB), C89A(H89C,H89D), C90A(H90C,H90D), C88A(H88C,H88D)
6.c Me refined with riding coordinates:
 C91(H91A,H91B,H91C), C87(H87A,H87B,H87C), C96(H96A,H96B,H96C), C92(H92A,H92B,
 H92C), C97(H97A,H97B,H97C), C101(H10C,H10D,H10E), C97A(H97D,H97E,H97F),
 C1B(H1BA,H1BB,H1BC), C91A(H91D,H91E,H91F), C87A(H87D,H87E,H87F)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C11(H11), C12(H12), C18(H18), C19(H19), C26(H26), C29(H29),
 C34(H34), C35(H35), C36(H36), C37(H37), C40(H40), C41(H41), C42(H42), C43(H43),
  C46(H46), C49(H49), C54(H54), C55(H55), C56(H56), C57(H57), C60(H60),
 C61(H61), C62(H62), C63(H63), C66(H66), C69(H69), C74(H74), C75(H75), C76(H76),
  C77(H77), C80(H80), C81(H81), C82(H82), C83(H83)
;
_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
C1 C 0.0808(2) -0.2173(14) 0.4891(2) 0.035(3) Uani 1 1 d . . . . .
H1 H 0.076647 -0.305449 0.473911 0.043 Uiso 1 1 calc R . . . .
C2 C 0.0867(3) -0.2609(14) 0.5198(2) 0.039(3) Uani 1 1 d . . . . .
H2 H 0.085930 -0.378801 0.525329 0.047 Uiso 1 1 calc R . . . .
C3 C 0.0934(2) -0.1389(13) 0.5417(2) 0.033(3) Uani 1 1 d . . . . .
C4 C 0.0965(2) 0.0413(13) 0.5340(2) 0.031(3) Uani 1 1 d . . . . .
C5 C 0.0895(2) 0.0814(13) 0.5041(3) 0.034(3) Uani 1 1 d . . . . .
C6 C 0.0809(2) -0.0473(13) 0.4809(3) 0.034(3) Uani 1 1 d . . . . .
C7 C 0.0697(2) 0.0207(12) 0.4488(2) 0.030(3) Uani 1 1 d . . . . .
H7 H 0.062991 -0.071587 0.432791 0.036 Uiso 1 1 calc R . . . .
C8 C 0.0868(2) 0.2650(12) 0.4903(2) 0.033(3) Uani 1 1 d . . . . .
H8 H 0.093473 0.358282 0.506126 0.040 Uiso 1 1 calc R . . . .
C9 C 0.0441(2) 0.1528(13) 0.4478(2) 0.029(3) Uani 1 1 d . . . . .
C10 C 0.0526(2) 0.2795(13) 0.4695(2) 0.030(3) Uani 1 1 d . . . . .
C11 C 0.0329(3) 0.4005(13) 0.4739(2) 0.034(3) Uani 1 1 d . . . . .
H11 H 0.039538 0.481612 0.490256 0.040 Uiso 1 1 calc R . . . .
C12 C 0.0027(3) 0.4003(13) 0.4534(2) 0.033(3) Uani 1 1 d . . . . .
H12 H -0.011363 0.486022 0.454977 0.039 Uiso 1 1 calc R . . . .
C13 C -0.0067(2) 0.2753(13) 0.4308(2) 0.029(3) Uani 1 1 d . . . . .
C14 C 0.0139(3) 0.1484(13) 0.4284(2) 0.034(3) Uani 1 1 d . . . . .
C15 C -0.0016(2) 0.0201(13) 0.4019(2) 0.033(3) Uani 1 1 d . . . . .
H15 H 0.012358 -0.074063 0.399983 0.040 Uiso 1 1 calc R . . . .
C16 C -0.0384(2) 0.2629(13) 0.4064(2) 0.032(3) Uani 1 1 d . . . . .
H16 H -0.052530 0.356946 0.408070 0.039 Uiso 1 1 calc R . . . .
C17 C -0.0296(2) -0.0465(13) 0.4081(2) 0.029(3) Uani 1 1 d . . . . .
C18 C -0.0348(3) -0.2223(13) 0.4125(2) 0.038(3) Uani 1 1 d . . . . .
H18 H -0.021959 -0.309972 0.409138 0.046 Uiso 1 1 calc R . . . .
C19 C -0.0592(3) -0.2632(14) 0.4216(3) 0.044(3) Uani 1 1 d . . . . .
H19 H -0.062664 -0.380574 0.425603 0.053 Uiso 1 1 calc R . . . .
C20 C -0.0792(3) -0.1336(14) 0.4253(2) 0.034(3) Uani 1 1 d . . . . .
C21 C -0.0738(2) 0.0392(12) 0.4193(2) 0.026(3) Uani 1 1 d . . . . .
C22 C -0.0498(2) 0.0800(12) 0.4107(2) 0.026(3) Uani 1 1 d . . . . .
C23 C -0.0980(2) 0.1575(14) 0.4246(2) 0.033(3) Uani 1 1 d . . . . .
H23 H -0.095643 0.280287 0.418961 0.039 Uiso 1 1 calc R . . . .
C24 C -0.1050(2) -0.1592(12) 0.4381(2) 0.025(3) Uani 1 1 d . . . . .
H24 H -0.107801 -0.282697 0.443019 0.030 Uiso 1 1 calc R . . . .
C25 C -0.1328(3) -0.0826(14) 0.4141(2) 0.037(3) Uani 1 1 d . . . . .
C26 C -0.1609(3) -0.1681(14) 0.4002(3) 0.041(3) Uani 1 1 d . . . . .
H26 H -0.164051 -0.282096 0.406224 0.049 Uiso 1 1 calc R . . . .
C27 C -0.1836(3) -0.0826(16) 0.3778(3) 0.046(3) Uani 1 1 d . . . . .
C28 C -0.1793(3) 0.0872(14) 0.3690(3) 0.039(3) Uani 1 1 d . . . . .
C29 C -0.1517(3) 0.1714(15) 0.3834(3) 0.047(3) Uani 1 1 d . . . . .
H29 H -0.148498 0.285885 0.377689 0.057 Uiso 1 1 calc R . . . .
C30 C -0.1290(2) 0.0855(14) 0.4062(2) 0.031(3) Uani 1 1 d . . . . .
C31 C -0.2076(3) 0.1568(16) 0.3436(3) 0.045(3) Uani 1 1 d . . . . .
H31 H -0.204380 0.276712 0.337151 0.054 Uiso 1 1 calc R . . . .
C32 C -0.2157(3) -0.1548(17) 0.3602(3) 0.052(3) Uani 1 1 d . . . . .
H32 H -0.218993 -0.275259 0.366396 0.062 Uiso 1 1 calc R . . . .
C33 C -0.2180(3) -0.1399(18) 0.3276(3) 0.053(4) Uani 1 1 d . . . . .
C34 C -0.2238(3) -0.275(2) 0.3070(3) 0.075(5) Uani 1 1 d . . . . .
H34 H -0.227007 -0.387991 0.313379 0.090 Uiso 1 1 calc R . . . .
C35 C -0.2252(3) -0.247(2) 0.2767(4) 0.075(5) Uani 1 1 d . . . . .
H35 H -0.229337 -0.340348 0.262546 0.090 Uiso 1 1 calc R . . . .
C36 C -0.2203(3) -0.083(2) 0.2674(3) 0.083(5) Uani 1 1 d . . . . .
H36 H -0.220814 -0.064731 0.247024 0.100 Uiso 1 1 calc R . . . .
C37 C -0.2147(3) 0.058(2) 0.2881(3) 0.059(4) Uani 1 1 d . . . . .
H37 H -0.211911 0.171674 0.281552 0.071 Uiso 1 1 calc R . . . .
C38 C -0.2133(3) 0.0284(16) 0.3178(3) 0.049(3) Uani 1 1 d . . . . .
C39 C -0.2380(3) -0.0241(19) 0.3652(3) 0.056(4) Uani 1 1 d . . . . .
C40 C -0.2615(3) -0.055(2) 0.3767(3) 0.073(5) Uani 1 1 d . . . . .
H40 H -0.265026 -0.168580 0.382589 0.088 Uiso 1 1 calc R . . . .
C41 C -0.2804(4) 0.087(3) 0.3796(4) 0.094(6) Uani 1 1 d . . . . .
H41 H -0.295639 0.071090 0.388774 0.113 Uiso 1 1 calc R . . . .
C42 C -0.2756(4) 0.250(2) 0.3685(4) 0.093(5) Uani 1 1 d . . . . .
H42 H -0.288752 0.342275 0.369274 0.111 Uiso 1 1 calc R . . . .
C43 C -0.2527(3) 0.281(2) 0.3566(3) 0.074(5) Uani 1 1 d . . . . .
H43 H -0.250256 0.391880 0.349071 0.089 Uiso 1 1 calc R . . . .
C44 C -0.2333(3) 0.1476(19) 0.3559(3) 0.052(4) Uani 1 1 d . . . . .
C45 C -0.0135(2) 0.1334(13) 0.3736(2) 0.028(3) Uani 1 1 d . . . . .
C46 C -0.0043(3) 0.1223(13) 0.3482(2) 0.035(3) Uani 1 1 d . . . . .
H46 H 0.010194 0.038150 0.347026 0.042 Uiso 1 1 calc R . . . .
C47 C -0.0170(3) 0.2383(16) 0.3247(3) 0.047(3) Uani 1 1 d . . . . .
C48 C -0.0373(3) 0.3682(14) 0.3271(3) 0.043(3) Uani 1 1 d . . . . .
C49 C -0.0448(3) 0.3792(13) 0.3529(3) 0.038(3) Uani 1 1 d . . . . .
H49 H -0.058083 0.468915 0.354715 0.045 Uiso 1 1 calc R . . . .
C50 C -0.0335(3) 0.2616(13) 0.3763(2) 0.033(3) Uani 1 1 d . . . . .
C51 C -0.0104(3) 0.2480(14) 0.2946(3) 0.044(3) Uani 1 1 d . . . . .
H51 H 0.004262 0.156743 0.292984 0.052 Uiso 1 1 calc R . . . .
C52 C -0.0473(3) 0.4848(15) 0.2990(3) 0.049(3) Uani 1 1 d . . . . .
H52 H -0.061978 0.576822 0.300288 0.058 Uiso 1 1 calc R . . . .
C53 C 0.0017(3) 0.4334(14) 0.2933(3) 0.040(3) Uani 1 1 d . . . . .
C54 C 0.0295(3) 0.4747(15) 0.2910(3) 0.047(3) Uani 1 1 d . . . . .
H54 H 0.043793 0.388148 0.290331 0.056 Uiso 1 1 calc R . . . .
C55 C 0.0359(3) 0.6533(17) 0.2898(3) 0.064(4) Uani 1 1 d . . . . .
H55 H 0.054136 0.688030 0.286514 0.077 Uiso 1 1 calc R . . . .
C56 C 0.0169(3) 0.7722(16) 0.2932(3) 0.057(4) Uani 1 1 d . . . . .
H56 H 0.022625 0.890490 0.293767 0.069 Uiso 1 1 calc R . . . .
C57 C -0.0110(4) 0.7315(17) 0.2958(3) 0.059(4) Uani 1 1 d . . . . .
H57 H -0.024729 0.819055 0.297418 0.071 Uiso 1 1 calc R . . . .
C58 C -0.0181(3) 0.5586(16) 0.2961(2) 0.044(3) Uani 1 1 d . . . . .
C59 C -0.0407(3) 0.2357(17) 0.2698(3) 0.056(4) Uani 1 1 d . . . . .
C60 C -0.0507(4) 0.1092(16) 0.2465(3) 0.063(4) Uani 1 1 d . . . . .
H60 H -0.037375 0.018447 0.245226 0.075 Uiso 1 1 calc R . . . .
C61 C -0.0802(4) 0.119(2) 0.2254(3) 0.079(5) Uani 1 1 d . . . . .
H61 H -0.087220 0.035724 0.209510 0.094 Uiso 1 1 calc R . . . .
C62 C -0.0994(4) 0.251(3) 0.2278(4) 0.084(5) Uani 1 1 d . . . . .
H62 H -0.119531 0.257637 0.213243 0.101 Uiso 1 1 calc R . . . .
C63 C -0.0903(4) 0.373(2) 0.2504(3) 0.077(5) Uani 1 1 d . . . . .
H63 H -0.104265 0.460211 0.251850 0.093 Uiso 1 1 calc R . . . .
C64 C -0.0605(3) 0.3696(18) 0.2716(3) 0.053(4) Uani 1 1 d . . . . .
C65 C 0.0949(2) 0.1393(12) 0.4454(3) 0.033(3) Uani 1 1 d . . . . .
C66 C 0.1082(3) 0.1239(14) 0.4231(3) 0.039(3) Uani 1 1 d . . . . .
H66 H 0.102335 0.034255 0.408190 0.047 Uiso 1 1 calc R . . . .
C67 C 0.1307(3) 0.2453(14) 0.4232(3) 0.044(3) Uani 1 1 d . . . . .
C68 C 0.1399(3) 0.3728(15) 0.4447(3) 0.042(3) Uani 1 1 d . . . . .
C69 C 0.1266(3) 0.3872(14) 0.4664(3) 0.043(3) Uani 1 1 d . . . . .
H69 H 0.132495 0.478432 0.480971 0.051 Uiso 1 1 calc R . . . .
C70 C 0.1040(3) 0.2669(14) 0.4675(2) 0.042(3) Uani 1 1 d . . . . .
C71 C 0.1478(3) 0.2469(15) 0.4004(3) 0.049(3) Uani 1 1 d . . . . .
H71 H 0.141497 0.151767 0.384871 0.058 Uiso 1 1 calc R . . . .
C72 C 0.1640(3) 0.4931(15) 0.4400(3) 0.052(4) Uani 1 1 d . . . . .
H72 H 0.170335 0.587067 0.455768 0.063 Uiso 1 1 calc R . . . .
C73 C 0.1431(3) 0.4291(15) 0.3861(3) 0.044(3) Uani 1 1 d . . . . .
C74 C 0.1328(3) 0.4596(18) 0.3559(3) 0.066(4) Uani 1 1 d . . . . .
H74 H 0.128281 0.366789 0.341637 0.080 Uiso 1 1 calc R . . . .
C75 C 0.1288(3) 0.635(2) 0.3457(3) 0.063(4) Uani 1 1 d . . . . .
H75 H 0.119995 0.662565 0.324465 0.076 Uiso 1 1 calc R . . . .
C76 C 0.1378(3) 0.7611(19) 0.3669(4) 0.070(4) Uani 1 1 d . . . . .
H76 H 0.136441 0.878136 0.360287 0.085 Uiso 1 1 calc R . . . .
C77 C 0.1491(3) 0.7263(16) 0.3980(3) 0.057(4) Uani 1 1 d . . . . .
H77 H 0.155093 0.819125 0.412233 0.068 Uiso 1 1 calc R . . . .
C78 C 0.1516(3) 0.5602(16) 0.4085(3) 0.046(3) Uani 1 1 d . . . . .
C79 C 0.1817(3) 0.2412(18) 0.4203(3) 0.056(4) Uani 1 1 d . . . . .
C80 C 0.2025(4) 0.1145(19) 0.4175(4) 0.074(5) Uani 1 1 d . . . . .
H80 H 0.196209 0.025129 0.402540 0.089 Uiso 1 1 calc R . . . .
C81 C 0.2329(4) 0.126(2) 0.4377(4) 0.086(5) Uani 1 1 d . . . . .
H81 H 0.247589 0.042393 0.436852 0.103 Uiso 1 1 calc R . . . .
C82 C 0.2413(3) 0.256(2) 0.4584(4) 0.074(5) Uani 1 1 d . . . . .
H82 H 0.261957 0.261847 0.471860 0.088 Uiso 1 1 calc R . . . .
C83 C 0.2203(3) 0.3841(19) 0.4605(3) 0.069(4) Uani 1 1 d . . . . .
H83 H 0.226891 0.475961 0.474897 0.083 Uiso 1 1 calc R . . . .
C84 C 0.1895(3) 0.3737(16) 0.4412(3) 0.049(3) Uani 1 1 d . . . . .
Cl1 Cl 0.06207(11) 0.7882(6) 0.37172(11) 0.075(2) Uani 0.778(9) 1 d D . P A 1
C85 C 0.0550(5) 0.5657(13) 0.3732(4) 0.127(7) Uani 1 1 d D U . . .
H85A H 0.039966 0.527225 0.353479 0.152 Uiso 0.778(9) 1 calc R . P A 1
H85B H 0.074212 0.499963 0.376859 0.152 Uiso 0.778(9) 1 calc R . P A 1
H85C H 0.073445 0.640090 0.380198 0.152 Uiso 0.222(9) 1 calc R . P A 2
H85D H 0.039372 0.620571 0.355441 0.152 Uiso 0.222(9) 1 calc R . P A 2
Cl2 Cl 0.04067(14) 0.5258(7) 0.40293(12) 0.137(2) Uani 1 1 d D . . . .
C86 C -0.0139(5) -0.022(2) 0.4885(5) 0.056(7) Uani 0.5 1 d D U P B -1
H86A H -0.030996 -0.087992 0.491314 0.068 Uiso 0.5 1 calc R . P B -1
H86B H -0.021958 0.027453 0.467579 0.068 Uiso 0.5 1 calc R . P B -1
Cl3 Cl -0.00864(12) 0.1545(5) 0.51295(11) 0.1062(17) Uani 1 1 d D . . . .
C89 C 0.1848(15) 0.389(5) 0.2953(9) 0.26(2) Uani 0.62(3) 1 d D U P C 1
H89A H 0.167359 0.412779 0.302422 0.311 Uiso 0.62(3) 1 calc R . P C 1
H89B H 0.203965 0.411156 0.312521 0.311 Uiso 0.62(3) 1 calc R . P C 1
C90 C 0.1838(14) 0.197(5) 0.2856(9) 0.25(2) Uani 0.62(3) 1 d D U P C 1
H90A H 0.201482 0.171995 0.278903 0.297 Uiso 0.62(3) 1 calc R . P C 1
H90B H 0.164793 0.174818 0.268101 0.297 Uiso 0.62(3) 1 calc R . P C 1
C91 C 0.1849(14) 0.079(6) 0.3128(11) 0.28(2) Uani 0.62(3) 1 d D U P C 1
H91A H 0.184316 -0.042324 0.306525 0.427 Uiso 0.62(3) 1 calc R . P C 1
H91B H 0.203889 0.100850 0.330000 0.427 Uiso 0.62(3) 1 calc R . P C 1
H91C H 0.167278 0.103667 0.319221 0.427 Uiso 0.62(3) 1 calc R . P C 1
C88 C 0.1830(13) 0.510(6) 0.2685(10) 0.27(2) Uani 0.62(3) 1 d D U P C 1
H88A H 0.171159 0.453896 0.248854 0.326 Uiso 0.62(3) 1 calc R . P C 1
H88B H 0.203944 0.532879 0.268276 0.326 Uiso 0.62(3) 1 calc R . P C 1
C87 C 0.1676(14) 0.683(6) 0.2714(15) 0.27(2) Uani 0.62(3) 1 d D U P C 1
H87A H 0.166795 0.758621 0.254095 0.398 Uiso 0.62(3) 1 calc R . P C 1
H87B H 0.146811 0.661322 0.271260 0.398 Uiso 0.62(3) 1 calc R . P C 1
H87C H 0.179556 0.740211 0.290659 0.398 Uiso 0.62(3) 1 calc R . P C 1
C96 C 0.1830(4) 0.553(2) 0.5651(5) 0.141(8) Uani 1 1 d D U . . .
H96A H 0.197212 0.500080 0.583726 0.212 Uiso 1 1 calc R . . . .
H96B H 0.163148 0.572086 0.567797 0.212 Uiso 1 1 calc R . . . .
H96C H 0.180257 0.476281 0.547601 0.212 Uiso 1 1 calc R . . . .
C93 C 0.1837(5) 0.986(2) 0.5223(4) 0.157(9) Uani 1 1 d D U . . .
H93A H 0.169581 1.076932 0.524331 0.189 Uiso 1 1 calc R . . . .
H93B H 0.204699 1.014124 0.536079 0.189 Uiso 1 1 calc R . . . .
C94 C 0.1739(5) 0.808(2) 0.5307(4) 0.171(10) Uani 1 1 d D U . . .
H94A H 0.153723 0.820697 0.533372 0.206 Uiso 1 1 calc R . . . .
H94B H 0.171193 0.727940 0.513283 0.206 Uiso 1 1 calc R . . . .
C92 C 0.1828(5) 0.973(3) 0.4892(4) 0.158(9) Uani 1 1 d D U . . .
H92A H 0.188940 1.083545 0.482827 0.237 Uiso 1 1 calc R . . . .
H92B H 0.196871 0.881694 0.487543 0.237 Uiso 1 1 calc R . . . .
H92C H 0.161922 0.944200 0.475852 0.237 Uiso 1 1 calc R . . . .
C95 C 0.1960(5) 0.728(3) 0.5593(6) 0.218(13) Uani 1 1 d D U . . .
H95A H 0.198983 0.806306 0.577008 0.261 Uiso 1 1 calc R . . . .
H95B H 0.216143 0.710213 0.556751 0.261 Uiso 1 1 calc R . . . .
C100 C -0.1363(14) -0.389(5) 0.3438(10) 0.080(15) Uani 0.31(2) 1 d D U P D 1
H10A H -0.118304 -0.419848 0.361836 0.096 Uiso 0.31(2) 1 calc R . P D 1
H10B H -0.154785 -0.396309 0.349833 0.096 Uiso 0.31(2) 1 calc R . P D 1
C97 C -0.0991(12) 0.001(4) 0.3161(13) 0.083(16) Uani 0.31(2) 1 d D U P D 1
H97A H -0.081096 0.007080 0.309670 0.124 Uiso 0.31(2) 1 calc R . P D 1
H97B H -0.117109 0.043731 0.299482 0.124 Uiso 0.31(2) 1 calc R . P D 1
H97C H -0.095711 0.073350 0.334363 0.124 Uiso 0.31(2) 1 calc R . P D 1
C99 C -0.1327(9) -0.202(4) 0.3338(12) 0.075(14) Uani 0.31(2) 1 d D U P D 1
H99A H -0.151284 -0.167767 0.316640 0.091 Uiso 0.31(2) 1 calc R . P D 1
H99B H -0.130351 -0.121527 0.351111 0.091 Uiso 0.31(2) 1 calc R . P D 1
C98 C -0.1045(9) -0.187(4) 0.3236(12) 0.073(14) Uani 0.31(2) 1 d D U P D 1
H98A H -0.107641 -0.260406 0.305240 0.088 Uiso 0.31(2) 1 calc R . P D 1
H98B H -0.086219 -0.230752 0.340162 0.088 Uiso 0.31(2) 1 calc R . P D 1
C101 C -0.1392(15) -0.516(5) 0.3174(13) 0.121(19) Uani 0.31(2) 1 d D U P D 1
H10C H -0.141502 -0.633905 0.324111 0.182 Uiso 0.31(2) 1 calc R . P D 1
H10D H -0.157206 -0.485739 0.299705 0.182 Uiso 0.31(2) 1 calc R . P D 1
H10E H -0.120787 -0.509238 0.311687 0.182 Uiso 0.31(2) 1 calc R . P D 1
Cl4 Cl 0.0641(4) 0.3527(19) 0.3643(4) 0.106(9) Uani 0.222(9) 1 d D . P A 2
C97A C -0.1236(8) 0.157(4) 0.3077(9) 0.206(16) Uani 0.69(2) 1 d D U P D 2
H97D H -0.119494 0.234255 0.292730 0.310 Uiso 0.69(2) 1 calc R . P D 2
H97E H -0.145482 0.130536 0.301024 0.310 Uiso 0.69(2) 1 calc R . P D 2
H97F H -0.117385 0.214745 0.327760 0.310 Uiso 0.69(2) 1 calc R . P D 2
C98A C -0.1052(10) -0.011(4) 0.3103(11) 0.23(2) Uani 0.69(2) 1 d D U P D 2
H98C H -0.083038 0.015062 0.316924 0.273 Uiso 0.69(2) 1 calc R . P D 2
H98D H -0.111222 -0.069409 0.290105 0.273 Uiso 0.69(2) 1 calc R . P D 2
C99A C -0.1119(9) -0.130(4) 0.3340(7) 0.196(16) Uani 0.69(2) 1 d D U P D 2
H99C H -0.092313 -0.169203 0.349213 0.235 Uiso 0.69(2) 1 calc R . P D 2
H99D H -0.123212 -0.064150 0.345017 0.235 Uiso 0.69(2) 1 calc R . P D 2
C1A C -0.1308(9) -0.288(5) 0.3187(7) 0.21(2) Uani 0.69(2) 1 d D U P D 2
H1AA H -0.120572 -0.346711 0.305801 0.257 Uiso 0.69(2) 1 calc R . P D 2
H1AB H -0.151241 -0.249553 0.305163 0.257 Uiso 0.69(2) 1 calc R . P D 2
C1B C -0.1346(14) -0.417(4) 0.3424(10) 0.23(2) Uani 0.69(2) 1 d D U P D 2
H1BA H -0.146778 -0.516332 0.331681 0.348 Uiso 0.69(2) 1 calc R . P D 2
H1BB H -0.114388 -0.457522 0.355570 0.348 Uiso 0.69(2) 1 calc R . P D 2
H1BC H -0.145047 -0.360396 0.354933 0.348 Uiso 0.69(2) 1 calc R . P D 2
C89A C 0.1769(8) 0.516(4) 0.2921(8) 0.089(14) Uani 0.38(3) 1 d D U P C 2
H89C H 0.155051 0.481319 0.284575 0.107 Uiso 0.38(3) 1 calc R . P C 2
H89D H 0.183226 0.531694 0.314626 0.107 Uiso 0.38(3) 1 calc R . P C 2
C90A C 0.1962(10) 0.370(4) 0.2851(10) 0.106(16) Uani 0.38(3) 1 d D U P C 2
H90C H 0.217720 0.408979 0.290451 0.128 Uiso 0.38(3) 1 calc R . P C 2
H90D H 0.188272 0.343385 0.262878 0.128 Uiso 0.38(3) 1 calc R . P C 2
C91A C 0.1949(9) 0.206(4) 0.3036(9) 0.083(13) Uani 0.38(3) 1 d D U P C 2
H91D H 0.207226 0.114733 0.298968 0.125 Uiso 0.38(3) 1 calc R . P C 2
H91E H 0.202986 0.232916 0.325591 0.125 Uiso 0.38(3) 1 calc R . P C 2
H91F H 0.173594 0.167447 0.298071 0.125 Uiso 0.38(3) 1 calc R . P C 2
C88A C 0.1806(12) 0.688(5) 0.2771(15) 0.136(18) Uani 0.38(3) 1 d D U P C 2
H88C H 0.200720 0.739057 0.288800 0.163 Uiso 0.38(3) 1 calc R . P C 2
H88D H 0.180219 0.665107 0.255977 0.163 Uiso 0.38(3) 1 calc R . P C 2
C87A C 0.1552(11) 0.817(5) 0.2760(12) 0.137(19) Uani 0.38(3) 1 d D U P C 2
H87D H 0.158349 0.924951 0.266328 0.206 Uiso 0.38(3) 1 calc R . P C 2
H87E H 0.135196 0.768052 0.264140 0.206 Uiso 0.38(3) 1 calc R . P C 2
H87F H 0.155691 0.841983 0.296955 0.206 Uiso 0.38(3) 1 calc R . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.399(14) . ?
C1 C6 1.368(14) . ?
C2 C3 1.341(13) . ?
C3 C4 1.457(13) . ?
C3 C23 1.509(14) 5_556 ?
C4 C5 1.351(14) . ?
C4 C24 1.518(13) 5_556 ?
C5 C6 1.418(14) . ?
C5 C8 1.543(13) . ?
C6 C7 1.494(14) . ?
C7 C9 1.553(14) . ?
C7 C65 1.536(14) . ?
C8 C10 1.557(14) . ?
C8 C70 1.525(14) . ?
C9 C10 1.364(13) . ?
C9 C14 1.385(14) . ?
C10 C11 1.369(13) . ?
C11 C12 1.404(14) . ?
C12 C13 1.380(13) . ?
C13 C14 1.400(14) . ?
C13 C16 1.524(14) . ?
C14 C15 1.550(14) . ?
C15 C17 1.510(13) . ?
C15 C45 1.519(14) . ?
C16 C22 1.547(13) . ?
C16 C50 1.486(14) . ?
C17 C18 1.407(14) . ?
C17 C22 1.390(13) . ?
C18 C19 1.373(14) . ?
C19 C20 1.414(15) . ?
C20 C21 1.403(13) . ?
C20 C24 1.520(14) . ?
C21 C22 1.342(13) . ?
C21 C23 1.532(14) . ?
C23 C30 1.507(14) . ?
C24 C25 1.510(14) . ?
C25 C26 1.409(14) . ?
C25 C30 1.376(14) . ?
C26 C27 1.372(15) . ?
C27 C28 1.408(15) . ?
C27 C32 1.540(15) . ?
C28 C29 1.389(15) . ?
C28 C31 1.534(15) . ?
C29 C30 1.382(14) . ?
C31 C38 1.506(16) . ?
C31 C44 1.492(16) . ?
C32 C33 1.483(16) . ?
C32 C39 1.519(17) . ?
C33 C34 1.378(18) . ?
C33 C38 1.419(16) . ?
C34 C35 1.404(19) . ?
C35 C36 1.378(19) . ?
C36 C37 1.417(19) . ?
C37 C38 1.376(16) . ?
C39 C40 1.386(17) . ?
C39 C44 1.433(17) . ?
C40 C41 1.44(2) . ?
C41 C42 1.40(2) . ?
C42 C43 1.376(19) . ?
C43 C44 1.372(17) . ?
C45 C46 1.383(14) . ?
C45 C50 1.395(14) . ?
C46 C47 1.379(14) . ?
C47 C48 1.407(15) . ?
C47 C51 1.529(15) . ?
C48 C49 1.355(14) . ?
C48 C52 1.524(15) . ?
C49 C50 1.377(14) . ?
C51 C53 1.546(15) . ?
C51 C59 1.487(17) . ?
C52 C58 1.518(16) . ?
C52 C64 1.500(17) . ?
C53 C54 1.369(15) . ?
C53 C58 1.371(15) . ?
C54 C55 1.417(16) . ?
C55 C56 1.319(17) . ?
C56 C57 1.377(17) . ?
C57 C58 1.377(16) . ?
C59 C60 1.415(16) . ?
C59 C64 1.403(17) . ?
C60 C61 1.387(18) . ?
C61 C62 1.38(2) . ?
C62 C63 1.36(2) . ?
C63 C64 1.399(18) . ?
C65 C66 1.379(14) . ?
C65 C70 1.380(14) . ?
C66 C67 1.403(14) . ?
C67 C68 1.363(15) . ?
C67 C71 1.521(15) . ?
C68 C69 1.351(14) . ?
C68 C72 1.524(15) . ?
C69 C70 1.417(15) . ?
C71 C73 1.539(15) . ?
C71 C79 1.530(17) . ?
C72 C78 1.473(16) . ?
C72 C84 1.490(17) . ?
C73 C74 1.338(16) . ?
C73 C78 1.405(15) . ?
C74 C75 1.431(18) . ?
C75 C76 1.344(18) . ?
C76 C77 1.383(18) . ?
C77 C78 1.363(16) . ?
C79 C80 1.412(17) . ?
C79 C84 1.371(16) . ?
C80 C81 1.41(2) . ?
C81 C82 1.35(2) . ?
C82 C83 1.417(19) . ?
C83 C84 1.407(17) . ?
Cl1 C85 1.757(9) . ?
C85 Cl2 1.747(9) . ?
C85 Cl4 1.783(9) . ?
C86 Cl3 1.735(9) . ?
C86 Cl3 1.481(19) 5_556 ?
C89 C90 1.541(10) . ?
C89 C88 1.537(10) . ?
C90 C91 1.546(10) . ?
C88 C87 1.543(10) . ?
C96 C95 1.543(10) . ?
C93 C94 1.536(9) . ?
C93 C92 1.526(9) . ?
C94 C95 1.508(10) . ?
C100 C99 1.543(10) . ?
C100 C101 1.539(10) . ?
C97 C98 1.540(10) . ?
C99 C98 1.537(10) . ?
C97A C98A 1.538(10) . ?
C98A C99A 1.543(10) . ?
C99A C1A 1.528(10) . ?
C1A C1B 1.537(10) . ?
C89A C90A 1.540(10) . ?
C89A C88A 1.537(10) . ?
C90A C91A 1.543(10) . ?
C88A C87A 1.536(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 119.7(10) . . ?
C3 C2 C1 121.1(10) . . ?
C2 C3 C4 120.3(10) . . ?
C2 C3 C23 129.0(9) . 5_556 ?
C4 C3 C23 110.7(9) . 5_556 ?
C3 C4 C24 112.6(9) . 5_556 ?
C5 C4 C3 117.5(10) . . ?
C5 C4 C24 129.7(9) . 5_556 ?
C4 C5 C6 121.7(10) . . ?
C4 C5 C8 126.4(10) . . ?
C6 C5 C8 111.7(9) . . ?
C1 C6 C5 119.4(10) . . ?
C1 C6 C7 125.5(10) . . ?
C5 C6 C7 114.9(9) . . ?
C6 C7 C9 105.4(8) . . ?
C6 C7 C65 107.0(9) . . ?
C65 C7 C9 101.8(8) . . ?
C5 C8 C10 104.2(8) . . ?
C70 C8 C5 107.9(8) . . ?
C70 C8 C10 103.6(9) . . ?
C10 C9 C7 115.1(10) . . ?
C10 C9 C14 118.1(10) . . ?
C14 C9 C7 126.8(10) . . ?
C9 C10 C8 112.5(10) . . ?
C9 C10 C11 124.1(10) . . ?
C11 C10 C8 123.3(9) . . ?
C10 C11 C12 117.5(10) . . ?
C13 C12 C11 120.0(10) . . ?
C12 C13 C14 120.2(10) . . ?
C12 C13 C16 125.6(10) . . ?
C14 C13 C16 114.2(9) . . ?
C9 C14 C13 119.9(9) . . ?
C9 C14 C15 128.7(10) . . ?
C13 C14 C15 111.4(10) . . ?
C17 C15 C14 105.5(8) . . ?
C17 C15 C45 106.2(8) . . ?
C45 C15 C14 104.5(8) . . ?
C13 C16 C22 104.5(8) . . ?
C50 C16 C13 106.3(9) . . ?
C50 C16 C22 106.4(8) . . ?
C18 C17 C15 124.0(10) . . ?
C22 C17 C15 115.3(9) . . ?
C22 C17 C18 120.7(10) . . ?
C19 C18 C17 117.9(10) . . ?
C18 C19 C20 121.1(10) . . ?
C19 C20 C24 126.2(10) . . ?
C21 C20 C19 118.9(10) . . ?
C21 C20 C24 114.6(9) . . ?
C20 C21 C23 110.4(9) . . ?
C22 C21 C20 120.2(10) . . ?
C22 C21 C23 129.5(9) . . ?
C17 C22 C16 111.0(9) . . ?
C21 C22 C16 127.5(9) . . ?
C21 C22 C17 121.0(9) . . ?
C3 C23 C21 104.8(8) 5_556 . ?
C30 C23 C3 108.7(9) . 5_556 ?
C30 C23 C21 107.5(8) . . ?
C4 C24 C20 104.2(8) 5_556 . ?
C25 C24 C4 107.5(8) . 5_556 ?
C25 C24 C20 104.5(8) . . ?
C26 C25 C24 125.5(10) . . ?
C30 C25 C24 114.3(10) . . ?
C30 C25 C26 120.2(10) . . ?
C27 C26 C25 118.4(10) . . ?
C26 C27 C28 121.3(10) . . ?
C26 C27 C32 125.7(11) . . ?
C28 C27 C32 113.0(11) . . ?
C27 C28 C31 112.4(10) . . ?
C29 C28 C27 119.7(11) . . ?
C29 C28 C31 127.8(10) . . ?
C30 C29 C28 118.7(11) . . ?
C25 C30 C23 112.4(9) . . ?
C25 C30 C29 121.6(10) . . ?
C29 C30 C23 126.0(10) . . ?
C38 C31 C28 104.7(10) . . ?
C44 C31 C28 105.9(9) . . ?
C44 C31 C38 109.0(10) . . ?
C33 C32 C27 103.5(10) . . ?
C33 C32 C39 106.6(10) . . ?
C39 C32 C27 105.4(10) . . ?
C34 C33 C32 125.2(13) . . ?
C34 C33 C38 119.1(13) . . ?
C38 C33 C32 115.7(12) . . ?
C33 C34 C35 120.6(15) . . ?
C36 C35 C34 119.8(15) . . ?
C35 C36 C37 120.7(14) . . ?
C38 C37 C36 118.8(13) . . ?
C33 C38 C31 110.7(11) . . ?
C37 C38 C31 128.2(12) . . ?
C37 C38 C33 121.1(12) . . ?
C40 C39 C32 127.5(14) . . ?
C40 C39 C44 119.6(13) . . ?
C44 C39 C32 112.9(12) . . ?
C39 C40 C41 119.2(15) . . ?
C42 C41 C40 118.1(15) . . ?
C43 C42 C41 122.9(16) . . ?
C44 C43 C42 118.7(16) . . ?
C39 C44 C31 112.5(12) . . ?
C43 C44 C31 126.1(14) . . ?
C43 C44 C39 121.2(13) . . ?
C46 C45 C15 125.1(10) . . ?
C46 C45 C50 122.1(10) . . ?
C50 C45 C15 112.7(9) . . ?
C47 C46 C45 117.3(11) . . ?
C46 C47 C48 121.2(11) . . ?
C46 C47 C51 126.0(11) . . ?
C48 C47 C51 112.7(11) . . ?
C47 C48 C52 111.8(11) . . ?
C49 C48 C47 119.8(11) . . ?
C49 C48 C52 128.4(11) . . ?
C48 C49 C50 120.7(11) . . ?
C45 C50 C16 114.2(9) . . ?
C49 C50 C16 126.7(10) . . ?
C49 C50 C45 118.9(10) . . ?
C47 C51 C53 105.5(9) . . ?
C59 C51 C47 105.7(10) . . ?
C59 C51 C53 106.9(10) . . ?
C58 C52 C48 106.0(10) . . ?
C64 C52 C48 107.1(10) . . ?
C64 C52 C58 105.5(10) . . ?
C54 C53 C51 125.6(10) . . ?
C54 C53 C58 121.6(11) . . ?
C58 C53 C51 112.8(11) . . ?
C53 C54 C55 116.4(12) . . ?
C56 C55 C54 121.1(13) . . ?
C55 C56 C57 122.5(13) . . ?
C56 C57 C58 117.3(12) . . ?
C53 C58 C52 113.0(11) . . ?
C53 C58 C57 120.8(13) . . ?
C57 C58 C52 126.2(12) . . ?
C60 C59 C51 127.8(14) . . ?
C64 C59 C51 112.0(12) . . ?
C64 C59 C60 120.2(14) . . ?
C61 C60 C59 119.2(14) . . ?
C62 C61 C60 119.5(15) . . ?
C63 C62 C61 122.1(16) . . ?
C62 C63 C64 119.8(16) . . ?
C59 C64 C52 113.6(12) . . ?
C63 C64 C52 127.0(14) . . ?
C63 C64 C59 119.1(14) . . ?
C66 C65 C7 125.2(10) . . ?
C66 C65 C70 121.1(11) . . ?
C70 C65 C7 113.7(10) . . ?
C65 C66 C67 117.6(10) . . ?
C66 C67 C71 124.6(11) . . ?
C68 C67 C66 122.2(11) . . ?
C68 C67 C71 113.2(10) . . ?
C67 C68 C72 113.6(10) . . ?
C69 C68 C67 119.7(11) . . ?
C69 C68 C72 126.7(11) . . ?
C68 C69 C70 120.3(11) . . ?
C65 C70 C8 114.0(11) . . ?
C65 C70 C69 119.0(11) . . ?
C69 C70 C8 126.9(10) . . ?
C67 C71 C73 106.0(10) . . ?
C67 C71 C79 104.7(10) . . ?
C79 C71 C73 104.5(10) . . ?
C78 C72 C68 107.4(10) . . ?
C78 C72 C84 106.9(11) . . ?
C84 C72 C68 103.3(10) . . ?
C74 C73 C71 124.0(12) . . ?
C74 C73 C78 123.7(12) . . ?
C78 C73 C71 112.3(11) . . ?
C73 C74 C75 118.4(13) . . ?
C76 C75 C74 118.0(13) . . ?
C75 C76 C77 122.4(13) . . ?
C78 C77 C76 120.7(13) . . ?
C73 C78 C72 113.3(11) . . ?
C77 C78 C72 129.9(12) . . ?
C77 C78 C73 116.6(12) . . ?
C80 C79 C71 124.1(14) . . ?
C84 C79 C71 112.1(12) . . ?
C84 C79 C80 123.8(14) . . ?
C81 C80 C79 117.2(15) . . ?
C82 C81 C80 120.2(16) . . ?
C81 C82 C83 122.0(15) . . ?
C84 C83 C82 119.3(14) . . ?
C79 C84 C72 114.8(12) . . ?
C79 C84 C83 117.5(13) . . ?
C83 C84 C72 127.7(13) . . ?
Cl2 C85 Cl1 109.3(6) . . ?
Cl2 C85 Cl4 101.8(7) . . ?
Cl3 C86 Cl3 128.9(14) 5_556 . ?
C88 C89 C90 111.3(15) . . ?
C89 C90 C91 109.9(15) . . ?
C89 C88 C87 111.0(15) . . ?
C92 C93 C94 106.6(12) . . ?
C95 C94 C93 114.5(12) . . ?
C94 C95 C96 108.8(12) . . ?
C101 C100 C99 110.4(15) . . ?
C98 C99 C100 110.5(14) . . ?
C99 C98 C97 111.0(15) . . ?
C97A C98A C99A 108.7(14) . . ?
C1A C99A C98A 111.7(15) . . ?
C99A C1A C1B 112.0(15) . . ?
C88A C89A C90A 111.9(14) . . ?
C89A C90A C91A 110.1(14) . . ?
C87A C88A C89A 112.1(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -3.7(17) . . . . ?
C1 C2 C3 C23 174.6(10) . . . 5_556 ?
C1 C6 C7 C9 121.5(11) . . . . ?
C1 C6 C7 C65 -130.6(11) . . . . ?
C2 C1 C6 C5 5.2(16) . . . . ?
C2 C1 C6 C7 -168.6(10) . . . . ?
C2 C3 C4 C5 6.0(16) . . . . ?
C2 C3 C4 C24 -178.6(10) . . . 5_556 ?
C3 C4 C5 C6 -2.8(16) . . . . ?
C3 C4 C5 C8 171.0(10) . . . . ?
C3 C23 C30 C25 -55.1(12) 5_556 . . . ?
C3 C23 C30 C29 126.1(11) 5_556 . . . ?
C4 C5 C6 C1 -2.7(17) . . . . ?
C4 C5 C6 C7 171.7(10) . . . . ?
C4 C5 C8 C10 -116.2(12) . . . . ?
C4 C5 C8 C70 134.2(11) . . . . ?
C4 C24 C25 C26 -123.3(11) 5_556 . . . ?
C4 C24 C25 C30 56.2(12) 5_556 . . . ?
C5 C6 C7 C9 -52.5(12) . . . . ?
C5 C6 C7 C65 55.4(12) . . . . ?
C5 C8 C10 C9 -57.1(11) . . . . ?
C5 C8 C10 C11 119.3(10) . . . . ?
C5 C8 C70 C65 53.8(12) . . . . ?
C5 C8 C70 C69 -128.8(11) . . . . ?
C6 C1 C2 C3 -2.0(17) . . . . ?
C6 C5 C8 C10 58.2(11) . . . . ?
C6 C5 C8 C70 -51.4(12) . . . . ?
C6 C7 C9 C10 54.2(11) . . . . ?
C6 C7 C9 C14 -122.1(11) . . . . ?
C6 C7 C65 C66 125.6(11) . . . . ?
C6 C7 C65 C70 -53.5(11) . . . . ?
C7 C9 C10 C8 1.4(12) . . . . ?
C7 C9 C10 C11 -175.0(9) . . . . ?
C7 C9 C14 C13 178.3(9) . . . . ?
C7 C9 C14 C15 -3.9(17) . . . . ?
C7 C65 C66 C67 179.2(10) . . . . ?
C7 C65 C70 C8 -0.9(13) . . . . ?
C7 C65 C70 C69 -178.5(9) . . . . ?
C8 C5 C6 C1 -177.4(10) . . . . ?
C8 C5 C6 C7 -3.0(13) . . . . ?
C8 C10 C11 C12 179.6(9) . . . . ?
C9 C7 C65 C66 -124.0(11) . . . . ?
C9 C7 C65 C70 56.8(11) . . . . ?
C9 C10 C11 C12 -4.4(16) . . . . ?
C9 C14 C15 C17 128.1(11) . . . . ?
C9 C14 C15 C45 -120.1(11) . . . . ?
C10 C8 C70 C65 -56.2(11) . . . . ?
C10 C8 C70 C69 121.2(11) . . . . ?
C10 C9 C14 C13 2.1(15) . . . . ?
C10 C9 C14 C15 179.8(10) . . . . ?
C10 C11 C12 C13 3.4(15) . . . . ?
C11 C12 C13 C14 0.2(15) . . . . ?
C11 C12 C13 C16 -177.9(10) . . . . ?
C12 C13 C14 C9 -3.0(15) . . . . ?
C12 C13 C14 C15 178.9(9) . . . . ?
C12 C13 C16 C22 -123.1(10) . . . . ?
C12 C13 C16 C50 124.6(11) . . . . ?
C13 C14 C15 C17 -54.0(11) . . . . ?
C13 C14 C15 C45 57.7(11) . . . . ?
C13 C16 C22 C17 -56.9(11) . . . . ?
C13 C16 C22 C21 115.4(12) . . . . ?
C13 C16 C50 C45 54.5(11) . . . . ?
C13 C16 C50 C49 -120.4(12) . . . . ?
C14 C9 C10 C8 178.0(9) . . . . ?
C14 C9 C10 C11 1.7(16) . . . . ?
C14 C13 C16 C22 58.7(11) . . . . ?
C14 C13 C16 C50 -53.6(11) . . . . ?
C14 C15 C17 C18 -121.0(11) . . . . ?
C14 C15 C17 C22 56.2(11) . . . . ?
C14 C15 C45 C46 118.0(11) . . . . ?
C14 C15 C45 C50 -57.7(11) . . . . ?
C15 C17 C18 C19 172.0(10) . . . . ?
C15 C17 C22 C16 0.0(12) . . . . ?
C15 C17 C22 C21 -172.8(9) . . . . ?
C15 C45 C46 C47 -178.6(10) . . . . ?
C15 C45 C50 C16 1.4(13) . . . . ?
C15 C45 C50 C49 176.8(9) . . . . ?
C16 C13 C14 C9 175.3(9) . . . . ?
C16 C13 C14 C15 -2.8(12) . . . . ?
C17 C15 C45 C46 -130.7(10) . . . . ?
C17 C15 C45 C50 53.6(11) . . . . ?
C17 C18 C19 C20 2.8(16) . . . . ?
C18 C17 C22 C16 177.4(9) . . . . ?
C18 C17 C22 C21 4.5(16) . . . . ?
C18 C19 C20 C21 0.1(16) . . . . ?
C18 C19 C20 C24 -173.8(10) . . . . ?
C19 C20 C21 C22 -0.8(16) . . . . ?
C19 C20 C21 C23 179.9(9) . . . . ?
C19 C20 C24 C4 120.1(11) . . . 5_556 ?
C19 C20 C24 C25 -127.2(11) . . . . ?
C20 C21 C22 C16 -173.1(10) . . . . ?
C20 C21 C22 C17 -1.5(16) . . . . ?
C20 C21 C23 C3 63.0(11) . . . 5_556 ?
C20 C21 C23 C30 -52.6(11) . . . . ?
C20 C24 C25 C26 126.5(11) . . . . ?
C20 C24 C25 C30 -54.1(11) . . . . ?
C21 C20 C24 C4 -54.1(11) . . . 5_556 ?
C21 C20 C24 C25 58.6(11) . . . . ?
C21 C23 C30 C25 57.8(12) . . . . ?
C21 C23 C30 C29 -121.0(11) . . . . ?
C22 C16 C50 C45 -56.4(11) . . . . ?
C22 C16 C50 C49 128.6(11) . . . . ?
C22 C17 C18 C19 -5.1(16) . . . . ?
C22 C21 C23 C3 -116.2(12) . . . 5_556 ?
C22 C21 C23 C30 128.2(11) . . . . ?
C23 C3 C4 C5 -172.6(9) 5_556 . . . ?
C23 C3 C4 C24 2.8(12) 5_556 . . 5_556 ?
C23 C21 C22 C16 6.1(18) . . . . ?
C23 C21 C22 C17 177.7(10) . . . . ?
C24 C4 C5 C6 -177.3(10) 5_556 . . . ?
C24 C4 C5 C8 -3.4(18) 5_556 . . . ?
C24 C20 C21 C22 173.8(9) . . . . ?
C24 C20 C21 C23 -5.5(12) . . . . ?
C24 C25 C26 C27 -177.5(10) . . . . ?
C24 C25 C30 C23 -2.4(13) . . . . ?
C24 C25 C30 C29 176.5(10) . . . . ?
C25 C26 C27 C28 -0.7(17) . . . . ?
C25 C26 C27 C32 -180.0(11) . . . . ?
C26 C25 C30 C23 177.1(10) . . . . ?
C26 C25 C30 C29 -4.0(17) . . . . ?
C26 C27 C28 C29 -0.8(18) . . . . ?
C26 C27 C28 C31 179.6(11) . . . . ?
C26 C27 C32 C33 -124.0(13) . . . . ?
C26 C27 C32 C39 124.2(13) . . . . ?
C27 C28 C29 C30 -0.1(17) . . . . ?
C27 C28 C31 C38 -57.2(13) . . . . ?
C27 C28 C31 C44 57.9(13) . . . . ?
C27 C32 C33 C34 123.2(14) . . . . ?
C27 C32 C33 C38 -56.1(14) . . . . ?
C27 C32 C39 C40 -125.2(14) . . . . ?
C27 C32 C39 C44 55.8(13) . . . . ?
C28 C27 C32 C33 56.7(13) . . . . ?
C28 C27 C32 C39 -55.1(13) . . . . ?
C28 C29 C30 C23 -178.8(10) . . . . ?
C28 C29 C30 C25 2.5(17) . . . . ?
C28 C31 C38 C33 58.3(13) . . . . ?
C28 C31 C38 C37 -122.5(13) . . . . ?
C28 C31 C44 C39 -57.2(13) . . . . ?
C28 C31 C44 C43 128.0(13) . . . . ?
C29 C28 C31 C38 123.3(13) . . . . ?
C29 C28 C31 C44 -121.6(13) . . . . ?
C30 C25 C26 C27 3.1(17) . . . . ?
C31 C28 C29 C30 179.5(11) . . . . ?
C32 C27 C28 C29 178.5(10) . . . . ?
C32 C27 C28 C31 -1.0(14) . . . . ?
C32 C33 C34 C35 -179.2(13) . . . . ?
C32 C33 C38 C31 -1.1(15) . . . . ?
C32 C33 C38 C37 179.6(11) . . . . ?
C32 C39 C40 C41 -179.8(13) . . . . ?
C32 C39 C44 C31 0.1(15) . . . . ?
C32 C39 C44 C43 175.3(12) . . . . ?
C33 C32 C39 C40 125.2(14) . . . . ?
C33 C32 C39 C44 -53.7(14) . . . . ?
C33 C34 C35 C36 0(2) . . . . ?
C34 C33 C38 C31 179.5(11) . . . . ?
C34 C33 C38 C37 0.3(19) . . . . ?
C34 C35 C36 C37 -1(2) . . . . ?
C35 C36 C37 C38 2(2) . . . . ?
C36 C37 C38 C31 179.8(12) . . . . ?
C36 C37 C38 C33 -1.1(19) . . . . ?
C38 C31 C44 C39 55.0(13) . . . . ?
C38 C31 C44 C43 -119.8(14) . . . . ?
C38 C33 C34 C35 0(2) . . . . ?
C39 C32 C33 C34 -126.0(14) . . . . ?
C39 C32 C33 C38 54.7(14) . . . . ?
C39 C40 C41 C42 4(2) . . . . ?
C40 C39 C44 C31 -178.9(11) . . . . ?
C40 C39 C44 C43 -4(2) . . . . ?
C40 C41 C42 C43 -4(3) . . . . ?
C41 C42 C43 C44 -1(2) . . . . ?
C42 C43 C44 C31 179.1(13) . . . . ?
C42 C43 C44 C39 5(2) . . . . ?
C44 C31 C38 C33 -54.7(13) . . . . ?
C44 C31 C38 C37 124.5(14) . . . . ?
C44 C39 C40 C41 -1(2) . . . . ?
C45 C15 C17 C18 128.4(10) . . . . ?
C45 C15 C17 C22 -54.3(11) . . . . ?
C45 C46 C47 C48 3.2(17) . . . . ?
C45 C46 C47 C51 -179.4(10) . . . . ?
C46 C45 C50 C16 -174.4(9) . . . . ?
C46 C45 C50 C49 1.0(16) . . . . ?
C46 C47 C48 C49 -0.8(18) . . . . ?
C46 C47 C48 C52 177.8(11) . . . . ?
C46 C47 C51 C53 -121.9(12) . . . . ?
C46 C47 C51 C59 125.1(13) . . . . ?
C47 C48 C49 C50 -1.7(18) . . . . ?
C47 C48 C52 C58 -57.3(13) . . . . ?
C47 C48 C52 C64 55.0(14) . . . . ?
C47 C51 C53 C54 121.9(12) . . . . ?
C47 C51 C53 C58 -55.5(13) . . . . ?
C47 C51 C59 C60 -120.2(13) . . . . ?
C47 C51 C59 C64 59.3(13) . . . . ?
C48 C47 C51 C53 55.7(13) . . . . ?
C48 C47 C51 C59 -57.3(13) . . . . ?
C48 C49 C50 C16 176.4(11) . . . . ?
C48 C49 C50 C45 1.6(16) . . . . ?
C48 C52 C58 C53 58.3(13) . . . . ?
C48 C52 C58 C57 -122.2(13) . . . . ?
C48 C52 C64 C59 -53.6(14) . . . . ?
C48 C52 C64 C63 119.6(14) . . . . ?
C49 C48 C52 C58 121.1(13) . . . . ?
C49 C48 C52 C64 -126.6(13) . . . . ?
C50 C16 C22 C17 55.3(11) . . . . ?
C50 C16 C22 C21 -132.4(11) . . . . ?
C50 C45 C46 C47 -3.3(16) . . . . ?
C51 C47 C48 C49 -178.5(10) . . . . ?
C51 C47 C48 C52 0.1(15) . . . . ?
C51 C53 C54 C55 179.2(11) . . . . ?
C51 C53 C58 C52 -1.3(14) . . . . ?
C51 C53 C58 C57 179.2(10) . . . . ?
C51 C59 C60 C61 179.4(12) . . . . ?
C51 C59 C64 C52 -4.1(15) . . . . ?
C51 C59 C64 C63 -177.9(11) . . . . ?
C52 C48 C49 C50 180.0(11) . . . . ?
C53 C51 C59 C60 127.7(13) . . . . ?
C53 C51 C59 C64 -52.8(13) . . . . ?
C53 C54 C55 C56 5.2(19) . . . . ?
C54 C53 C58 C52 -178.8(10) . . . . ?
C54 C53 C58 C57 1.7(18) . . . . ?
C54 C55 C56 C57 -5(2) . . . . ?
C55 C56 C57 C58 2(2) . . . . ?
C56 C57 C58 C52 179.7(11) . . . . ?
C56 C57 C58 C53 -0.9(18) . . . . ?
C58 C52 C64 C59 58.9(13) . . . . ?
C58 C52 C64 C63 -127.8(13) . . . . ?
C58 C53 C54 C55 -3.7(18) . . . . ?
C59 C51 C53 C54 -126.0(13) . . . . ?
C59 C51 C53 C58 56.7(13) . . . . ?
C59 C60 C61 C62 -1(2) . . . . ?
C60 C59 C64 C52 175.5(11) . . . . ?
C60 C59 C64 C63 1.7(19) . . . . ?
C60 C61 C62 C63 0(2) . . . . ?
C61 C62 C63 C64 2(2) . . . . ?
C62 C63 C64 C52 -175.5(12) . . . . ?
C62 C63 C64 C59 -3(2) . . . . ?
C64 C52 C58 C53 -55.0(13) . . . . ?
C64 C52 C58 C57 124.5(13) . . . . ?
C64 C59 C60 C61 -0.1(19) . . . . ?
C65 C7 C9 C10 -57.4(11) . . . . ?
C65 C7 C9 C14 126.3(11) . . . . ?
C65 C66 C67 C68 1.4(17) . . . . ?
C65 C66 C67 C71 179.7(10) . . . . ?
C66 C65 C70 C8 179.9(9) . . . . ?
C66 C65 C70 C69 2.3(16) . . . . ?
C66 C67 C68 C69 -1.8(18) . . . . ?
C66 C67 C68 C72 -178.5(11) . . . . ?
C66 C67 C71 C73 125.4(12) . . . . ?
C66 C67 C71 C79 -124.4(12) . . . . ?
C67 C68 C69 C70 2.3(17) . . . . ?
C67 C68 C72 C78 54.2(14) . . . . ?
C67 C68 C72 C84 -58.6(14) . . . . ?
C67 C71 C73 C74 -127.8(13) . . . . ?
C67 C71 C73 C78 53.5(13) . . . . ?
C67 C71 C79 C80 124.2(13) . . . . ?
C67 C71 C79 C84 -55.8(13) . . . . ?
C68 C67 C71 C73 -56.2(13) . . . . ?
C68 C67 C71 C79 54.0(13) . . . . ?
C68 C69 C70 C8 -179.8(10) . . . . ?
C68 C69 C70 C65 -2.5(16) . . . . ?
C68 C72 C78 C73 -56.2(14) . . . . ?
C68 C72 C78 C77 128.5(14) . . . . ?
C68 C72 C84 C79 56.8(14) . . . . ?
C68 C72 C84 C83 -124.6(13) . . . . ?
C69 C68 C72 C78 -122.4(13) . . . . ?
C69 C68 C72 C84 124.9(13) . . . . ?
C70 C8 C10 C9 55.6(11) . . . . ?
C70 C8 C10 C11 -128.0(10) . . . . ?
C70 C65 C66 C67 -1.7(16) . . . . ?
C71 C67 C68 C69 179.8(10) . . . . ?
C71 C67 C68 C72 3.1(15) . . . . ?
C71 C73 C74 C75 178.5(12) . . . . ?
C71 C73 C78 C72 2.2(15) . . . . ?
C71 C73 C78 C77 178.2(11) . . . . ?
C71 C79 C80 C81 -179.4(12) . . . . ?
C71 C79 C84 C72 -0.3(15) . . . . ?
C71 C79 C84 C83 -179.0(10) . . . . ?
C72 C68 C69 C70 178.6(11) . . . . ?
C73 C71 C79 C80 -124.6(13) . . . . ?
C73 C71 C79 C84 55.5(13) . . . . ?
C73 C74 C75 C76 5(2) . . . . ?
C74 C73 C78 C72 -176.4(12) . . . . ?
C74 C73 C78 C77 -0.4(19) . . . . ?
C74 C75 C76 C77 -4(2) . . . . ?
C75 C76 C77 C78 0(2) . . . . ?
C76 C77 C78 C72 177.1(12) . . . . ?
C76 C77 C78 C73 1.9(19) . . . . ?
C78 C72 C84 C79 -56.2(13) . . . . ?
C78 C72 C84 C83 122.3(13) . . . . ?
C78 C73 C74 C75 -3(2) . . . . ?
C79 C71 C73 C74 121.8(14) . . . . ?
C79 C71 C73 C78 -56.8(13) . . . . ?
C79 C80 C81 C82 -1(2) . . . . ?
C80 C79 C84 C72 179.7(12) . . . . ?
C80 C79 C84 C83 1.0(19) . . . . ?
C80 C81 C82 C83 0(2) . . . . ?
C81 C82 C83 C84 2(2) . . . . ?
C82 C83 C84 C72 179.4(12) . . . . ?
C82 C83 C84 C79 -2.1(18) . . . . ?
C84 C72 C78 C73 54.1(13) . . . . ?
C84 C72 C78 C77 -121.2(15) . . . . ?
C84 C79 C80 C81 1(2) . . . . ?
C90 C89 C88 C87 151(6) . . . . ?
C88 C89 C90 C91 -179(5) . . . . ?
C93 C94 C95 C96 179.0(18) . . . . ?
C92 C93 C94 C95 127(2) . . . . ?
C100 C99 C98 C97 -175(4) . . . . ?
C101 C100 C99 C98 -58(6) . . . . ?
C97A C98A C99A C1A 110(4) . . . . ?
C98A C99A C1A C1B 174(3) . . . . ?
C90A C89A C88A C87A 164(4) . . . . ?
C88A C89A C90A C91A 173(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 1.492
_oxdiff_exptl_absorpt_empirical_full_min 0.627
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1997772'
loop_
_audit_author_name
_audit_author_address
'Yasutomo Segawa'
;Nagoya University
Japan
;
_audit_update_record             
;
2020-04-19 deposited with the CCDC.	2020-06-04 downloaded from the CCDC.
;
_audit_creation_date             2020-04-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C132 H84, 2(C4 H8 O), 0.5(C5 H12)'
_chemical_formula_sum            'C142.50 H106 O2'
_chemical_formula_weight         1850.27
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C132 H84'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0799(9)
_cell_length_b                   15.4092(15)
_cell_length_c                   16.833(2)
_cell_angle_alpha                111.731(10)
_cell_angle_beta                 95.979(8)
_cell_angle_gamma                99.110(7)
_cell_volume                     2594.1(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1628
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      24.4580
_cell_measurement_theta_min      1.8690
_shelx_estimated_absorpt_T_max   0.999
_shelx_estimated_absorpt_T_min   0.993
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             977
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1831
_diffrn_reflns_av_unetI/netI     0.3051
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.772
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24058
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.772
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.625
_diffrn_reflns_theta_min         1.891
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.772
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  86.00   0.50  102.09    --    4.93  37.00  60.00  212
  2  ω    -15.00  33.00   0.50  102.09    --   -4.53 -99.00 -30.00   96
  3  ω     38.00  88.00   0.50  102.09    --    4.93 179.00-120.00  100
  4  ω    -20.00  86.00   0.50  102.09    --    4.93  37.00 150.00  212
  5  ω    -88.00 -43.00   0.50  102.09    --   -4.53 179.00 150.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0074405000
_diffrn_orient_matrix_UB_12      0.0032963000
_diffrn_orient_matrix_UB_13      -0.0402012000
_diffrn_orient_matrix_UB_21      0.0368311000
_diffrn_orient_matrix_UB_22      0.0468426000
_diffrn_orient_matrix_UB_23      0.0225473000
_diffrn_orient_matrix_UB_31      0.0541163000
_diffrn_orient_matrix_UB_32      -0.0191749000
_diffrn_orient_matrix_UB_33      0.0001468000
_diffrn_oxdiff_digest_frames     
;
01c9afa063635abd0be0705a8aaf70d4cb000252589
;
_diffrn_oxdiff_digest_hkl        
;
0123c8304af2131c969b8c9afb18d97a254aa5
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3374
_reflns_number_total             10280
_reflns_odcompleteness_completeness 98.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.01
_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 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_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    ?
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         10280
_refine_ls_number_restraints     87
_refine_ls_R_factor_all          0.3183
_refine_ls_R_factor_gt           0.1177
_refine_ls_restrained_S_all      0.966
_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)+(0.1925P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2859
_refine_ls_wR_factor_ref         0.3871
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C67-C68 = C68-C69 = C69-C70
 1.54 with sigma of 0.01
 O1-C67 = O1-C70
 1.43 with sigma of 0.01
 C71-C72 = C72-C73 = C73-C74 = C74-C75
 1.54 with sigma of 0.01
 C71-C73
 2.54 with sigma of 0.01
 C74-C72
 2.54 with sigma of 0.01
 C73-C75
 2.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C67 \\sim C68 \\sim C69 \\sim C70: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C75) \\sim Ueq, Uanis(C71) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C71, C72, C73, C74, C75
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C75(0.25) H75A(0.25) H75B(0.25) H75C(0.25) C74(0.25) H74A(0.25)
 H74B(0.25) C73(0.25) H73A(0.25) H73B(0.25) C72(0.25) H72A(0.25) H72B(0.25)
 C71(0.25) H71A(0.25) H71B(0.25) H71C(0.25)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C11(H11), C14(H14), C21(H21), C24(H24)
6.b Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C74(H74A,
 H74B), C73(H73A,H73B), C72(H72A,H72B)
6.c Me refined with riding coordinates:
 C75(H75A,H75B,H75C), C71(H71A,H71B,H71C)
6.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C17(H17), C18(H18), C28(H28), C29(H29), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
 C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60),
  C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
;
_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
C1 C 0.5241(6) 0.1995(5) 0.7532(5) 0.0402(17) Uani 1 1 d . . . . .
C2 C 0.4894(6) 0.1379(5) 0.8053(5) 0.0436(18) Uani 1 1 d . . . . .
H2 H 0.400556 0.131670 0.812912 0.052 Uiso 1 1 calc R . . . .
C3 C 0.5805(7) 0.1766(5) 0.8919(5) 0.0459(18) Uani 1 1 d . . . . .
C4 C 0.7007(6) 0.1872(5) 0.8841(5) 0.0457(18) Uani 1 1 d . . . . .
C5 C 0.7176(6) 0.1536(5) 0.7887(5) 0.0418(18) Uani 1 1 d . . . . .
H5 H 0.807207 0.160286 0.782949 0.050 Uiso 1 1 calc R . . . .
C6 C 0.6511(6) 0.2094(5) 0.7464(5) 0.0405(17) Uani 1 1 d . . . . .
C7 C 0.7003(6) 0.2559(5) 0.6975(5) 0.0460(19) Uani 1 1 d . . . . .
H7 H 0.786225 0.263072 0.694422 0.055 Uiso 1 1 calc R . . . .
C8 C 0.6231(6) 0.2925(5) 0.6523(5) 0.0412(17) Uani 1 1 d . . . . .
H8 H 0.655804 0.324408 0.618069 0.049 Uiso 1 1 calc R . . . .
C9 C 0.4994(6) 0.2815(5) 0.6585(5) 0.0393(17) Uani 1 1 d . . . . .
C10 C 0.4504(6) 0.2358(5) 0.7099(5) 0.0401(17) Uani 1 1 d . . . . .
C11 C 0.3079(6) 0.2221(5) 0.6974(5) 0.0395(17) Uani 1 1 d . . . . .
H11 H 0.271139 0.190304 0.734081 0.047 Uiso 1 1 calc R . . . .
C12 C 0.2769(6) 0.3217(5) 0.7172(5) 0.0437(18) Uani 1 1 d . . . . .
C13 C 0.3253(6) 0.3654(5) 0.6684(5) 0.0435(18) Uani 1 1 d . . . . .
C14 C 0.3994(6) 0.3058(5) 0.6044(5) 0.0417(17) Uani 1 1 d . . . . .
H14 H 0.435230 0.339018 0.568434 0.050 Uiso 1 1 calc R . . . .
C15 C 0.3124(5) 0.2101(5) 0.5495(5) 0.0351(16) Uani 1 1 d . . . . .
C16 C 0.2620(6) 0.1639(5) 0.6014(5) 0.0405(17) Uani 1 1 d . . . . .
C17 C 0.1828(6) 0.0761(5) 0.5643(5) 0.0419(18) Uani 1 1 d . . . . .
H17 H 0.148337 0.046823 0.599860 0.050 Uiso 1 1 calc R . . . .
C18 C 0.1529(6) 0.0297(5) 0.4735(5) 0.0442(18) Uani 1 1 d . . . . .
H18 H 0.099341 -0.031805 0.447024 0.053 Uiso 1 1 calc R . . . .
C19 C 0.2030(6) 0.0751(5) 0.4223(5) 0.0404(18) Uani 1 1 d . . . . .
C20 C 0.2841(5) 0.1639(5) 0.4616(5) 0.0359(17) Uani 1 1 d . . . . .
C21 C 0.3328(6) 0.1962(5) 0.3932(5) 0.0416(18) Uani 1 1 d . . . . .
H21 H 0.390486 0.260399 0.419678 0.050 Uiso 1 1 calc R . . . .
C22 C 0.2187(6) 0.1938(5) 0.3301(5) 0.0459(19) Uani 1 1 d . . . . .
C23 C 0.1408(6) 0.1065(5) 0.2919(5) 0.0408(18) Uani 1 1 d . . . . .
C24 C 0.1831(5) 0.0332(5) 0.3247(5) 0.0377(17) Uani 1 1 d . . . . .
H24 H 0.124894 -0.030775 0.298231 0.045 Uiso 1 1 calc R . . . .
C25 C 0.6466(6) 0.0513(5) 0.7434(5) 0.0385(17) Uani 1 1 d . . . . .
C26 C 0.6862(6) -0.0293(5) 0.6963(4) 0.0367(16) Uani 1 1 d . . . . .
C27 C 0.6042(6) -0.1174(5) 0.6598(5) 0.0378(17) Uani 1 1 d . . . . .
C28 C 0.4827(6) -0.1275(5) 0.6672(5) 0.0430(18) Uani 1 1 d . . . . .
H28 H 0.427639 -0.188350 0.640835 0.052 Uiso 1 1 calc R . . . .
C29 C 0.4403(6) -0.0461(5) 0.7148(5) 0.0422(18) Uani 1 1 d . . . . .
H29 H 0.355344 -0.051239 0.720402 0.051 Uiso 1 1 calc R . . . .
C30 C 0.5212(6) 0.0415(5) 0.7534(5) 0.0403(17) Uani 1 1 d . . . . .
C31 C 0.8115(6) 0.2224(5) 0.9530(5) 0.0478(19) Uani 1 1 d . . . . .
C32 C 0.8180(7) 0.3000(6) 1.0319(5) 0.053(2) Uani 1 1 d . . . . .
H32 H 0.749699 0.330609 1.041510 0.063 Uiso 1 1 calc R . . . .
C33 C 0.9219(8) 0.3319(6) 1.0949(5) 0.059(2) Uani 1 1 d . . . . .
H33 H 0.923608 0.383215 1.148462 0.071 Uiso 1 1 calc R . . . .
C34 C 1.0239(7) 0.2913(6) 1.0825(6) 0.062(2) Uani 1 1 d . . . . .
H34 H 1.096171 0.314559 1.126225 0.075 Uiso 1 1 calc R . . . .
C35 C 1.0186(8) 0.2166(7) 1.0054(6) 0.070(2) Uani 1 1 d . . . . .
H35 H 1.088037 0.187185 0.996650 0.083 Uiso 1 1 calc R . . . .
C36 C 0.9157(7) 0.1821(6) 0.9395(6) 0.062(2) Uani 1 1 d . . . . .
H36 H 0.916013 0.131695 0.885820 0.074 Uiso 1 1 calc R . . . .
C37 C 0.5297(6) 0.1819(5) 0.9712(5) 0.0490(19) Uani 1 1 d . . . . .
C38 C 0.4365(7) 0.2305(6) 0.9978(6) 0.067(2) Uani 1 1 d . . . . .
H38 H 0.406724 0.265285 0.966461 0.080 Uiso 1 1 calc R . . . .
C39 C 0.3852(8) 0.2291(7) 1.0704(6) 0.077(3) Uani 1 1 d . . . . .
H39 H 0.322218 0.263398 1.088774 0.093 Uiso 1 1 calc R . . . .
C40 C 0.4282(8) 0.1763(7) 1.1153(6) 0.074(3) Uani 1 1 d . . . . .
H40 H 0.393163 0.173614 1.163770 0.089 Uiso 1 1 calc R . . . .
C41 C 0.5204(8) 0.1288(6) 1.0896(6) 0.068(2) Uani 1 1 d . . . . .
H41 H 0.550596 0.094105 1.120748 0.082 Uiso 1 1 calc R . . . .
C42 C 0.5688(8) 0.1311(6) 1.0198(6) 0.062(2) Uani 1 1 d . . . . .
H42 H 0.632140 0.096767 1.002707 0.075 Uiso 1 1 calc R . . . .
C43 C 0.1888(7) 0.3507(5) 0.7781(5) 0.0487(19) Uani 1 1 d . . . . .
C44 C 0.0861(7) 0.3836(6) 0.7573(6) 0.062(2) Uani 1 1 d . . . . .
H44 H 0.071991 0.390091 0.703329 0.074 Uiso 1 1 calc R . . . .
C45 C 0.0033(8) 0.4073(6) 0.8141(7) 0.077(3) Uani 1 1 d . . . . .
H45 H -0.068408 0.427942 0.798148 0.093 Uiso 1 1 calc R . . . .
C46 C 0.0246(11) 0.4010(7) 0.8923(8) 0.094(4) Uani 1 1 d . . . . .
H46 H -0.030334 0.419205 0.932348 0.113 Uiso 1 1 calc R . . . .
C47 C 0.1259(13) 0.3683(9) 0.9128(8) 0.120(5) Uani 1 1 d . . . . .
H47 H 0.140011 0.362024 0.966867 0.144 Uiso 1 1 calc R . . . .
C48 C 0.2072(11) 0.3443(8) 0.8568(7) 0.101(4) Uani 1 1 d . . . . .
H48 H 0.277901 0.322809 0.872995 0.122 Uiso 1 1 calc R . . . .
C49 C 0.3161(6) 0.4603(5) 0.6705(5) 0.0450(18) Uani 1 1 d . . . . .
C50 C 0.3005(6) 0.4749(5) 0.5936(5) 0.052(2) Uani 1 1 d . . . . .
H50 H 0.298249 0.423822 0.539748 0.062 Uiso 1 1 calc R . . . .
C51 C 0.2881(7) 0.5654(7) 0.5955(7) 0.072(3) Uani 1 1 d . . . . .
H51 H 0.279263 0.575256 0.542978 0.086 Uiso 1 1 calc R . . . .
C52 C 0.2888(8) 0.6388(6) 0.6724(8) 0.078(3) Uani 1 1 d . . . . .
H52 H 0.276913 0.698732 0.672943 0.094 Uiso 1 1 calc R . . . .
C53 C 0.3069(8) 0.6256(6) 0.7502(7) 0.072(3) Uani 1 1 d . . . . .
H53 H 0.310379 0.677010 0.804059 0.086 Uiso 1 1 calc R . . . .
C54 C 0.3196(6) 0.5377(5) 0.7482(5) 0.051(2) Uani 1 1 d . . . . .
H54 H 0.331265 0.529145 0.801313 0.061 Uiso 1 1 calc R . . . .
C55 C 0.2082(7) 0.2855(5) 0.3209(5) 0.0465(19) Uani 1 1 d . . . . .
C56 C 0.0945(7) 0.3122(5) 0.3171(5) 0.052(2) Uani 1 1 d . . . . .
H56 H 0.021317 0.269915 0.315912 0.063 Uiso 1 1 calc R . . . .
C57 C 0.0876(8) 0.3998(6) 0.3148(6) 0.063(2) Uani 1 1 d . . . . .
H57 H 0.010019 0.418690 0.314494 0.076 Uiso 1 1 calc R . . . .
C58 C 0.1916(8) 0.4597(5) 0.3131(6) 0.064(2) Uani 1 1 d . . . . .
H58 H 0.185940 0.520009 0.311706 0.077 Uiso 1 1 calc R . . . .
C59 C 0.3035(8) 0.4332(6) 0.3135(6) 0.063(2) Uani 1 1 d . . . . .
H59 H 0.375228 0.474005 0.310445 0.075 Uiso 1 1 calc R . . . .
C60 C 0.3118(7) 0.3463(6) 0.3183(5) 0.057(2) Uani 1 1 d . . . . .
H60 H 0.389979 0.328547 0.319889 0.068 Uiso 1 1 calc R . . . .
C61 C 0.0309(6) 0.0747(5) 0.2259(5) 0.0482(19) Uani 1 1 d . . . . .
C62 C 0.0206(10) 0.1002(7) 0.1557(7) 0.096(4) Uani 1 1 d . . . . .
H62 H 0.087359 0.143329 0.150169 0.115 Uiso 1 1 calc R . . . .
C63 C -0.0886(14) 0.0629(9) 0.0917(8) 0.122(5) Uani 1 1 d . . . . .
H63 H -0.095434 0.084734 0.045896 0.146 Uiso 1 1 calc R . . . .
C64 C -0.1803(9) -0.0007(8) 0.0937(8) 0.085(3) Uani 1 1 d . . . . .
H64 H -0.252758 -0.024272 0.050127 0.102 Uiso 1 1 calc R . . . .
C65 C -0.1710(8) -0.0325(9) 0.1582(7) 0.090(3) Uani 1 1 d . . . . .
H65 H -0.234363 -0.081840 0.158249 0.108 Uiso 1 1 calc R . . . .
C66 C -0.0687(7) 0.0073(8) 0.2245(6) 0.084(3) Uani 1 1 d . . . . .
H66 H -0.066896 -0.012844 0.271469 0.100 Uiso 1 1 calc R . . . .
O1 O 0.1796(6) 0.6980(5) 0.4879(6) 0.127(3) Uani 1 1 d D . . . .
C67 C 0.0582(7) 0.6479(6) 0.4823(7) 0.078(2) Uani 1 1 d D U . . .
H67A H 0.056059 0.623147 0.528773 0.093 Uiso 1 1 calc R . . . .
H67B H 0.031057 0.593232 0.425343 0.093 Uiso 1 1 calc R . . . .
C68 C -0.0268(7) 0.7189(5) 0.4927(6) 0.070(2) Uani 1 1 d D U . . .
H68A H -0.075938 0.708233 0.436055 0.084 Uiso 1 1 calc R . . . .
H68B H -0.083945 0.714574 0.533162 0.084 Uiso 1 1 calc R . . . .
C69 C 0.0643(8) 0.8138(7) 0.5296(9) 0.114(3) Uani 1 1 d D U . . .
H69A H 0.037991 0.856501 0.502576 0.137 Uiso 1 1 calc R . . . .
H69B H 0.067418 0.844766 0.593052 0.137 Uiso 1 1 calc R . . . .
C70 C 0.1866(8) 0.7972(6) 0.5117(8) 0.091(3) Uani 1 1 d D U . . .
H70A H 0.207423 0.816090 0.463756 0.110 Uiso 1 1 calc R . . . .
H70B H 0.251044 0.834696 0.563935 0.110 Uiso 1 1 calc R . . . .
C75 C 0.345(4) 0.554(3) 1.045(3) 0.144(16) Uani 0.25 1 d D U P A -1
H75A H 0.302514 0.583788 1.093573 0.215 Uiso 0.25 1 calc R . P A -1
H75B H 0.366435 0.597492 1.016810 0.215 Uiso 0.25 1 calc R . P A -1
H75C H 0.289300 0.494580 1.003362 0.215 Uiso 0.25 1 calc R . P A -1
C74 C 0.462(3) 0.530(3) 1.0803(17) 0.122(15) Uani 0.25 1 d D U P A -1
H74A H 0.440071 0.486987 1.110197 0.147 Uiso 0.25 1 calc R . P A -1
H74B H 0.517199 0.589888 1.123644 0.147 Uiso 0.25 1 calc R . P A -1
C73 C 0.534(3) 0.483(2) 1.008(2) 0.083(10) Uani 0.25 1 d D U P A -1
H73A H 0.617214 0.481599 1.035283 0.099 Uiso 0.25 1 calc R . P A -1
H73B H 0.489327 0.415528 0.974446 0.099 Uiso 0.25 1 calc R . P A -1
C72 C 0.548(5) 0.535(2) 0.947(2) 0.113(14) Uani 0.25 1 d D U P A -1
H72A H 0.593285 0.601636 0.980771 0.135 Uiso 0.25 1 calc R . P A -1
H72B H 0.465017 0.535831 0.920119 0.135 Uiso 0.25 1 calc R . P A -1
C71 C 0.619(4) 0.486(3) 0.875(2) 0.124(15) Uani 0.25 1 d D U P A -1
H71A H 0.627105 0.520643 0.837201 0.186 Uiso 0.25 1 calc R . P A -1
H71B H 0.702453 0.485487 0.901750 0.186 Uiso 0.25 1 calc R . P A -1
H71C H 0.574286 0.419734 0.841146 0.186 Uiso 0.25 1 calc R . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.545(9) . ?
C1 C6 1.412(8) . ?
C1 C10 1.354(9) . ?
C2 C3 1.536(10) . ?
C2 C30 1.537(10) . ?
C3 C4 1.342(9) . ?
C3 C37 1.482(10) . ?
C4 C5 1.537(10) . ?
C4 C31 1.474(10) . ?
C5 C6 1.527(9) . ?
C5 C25 1.509(10) . ?
C6 C7 1.376(9) . ?
C7 C8 1.402(9) . ?
C8 C9 1.374(9) . ?
C9 C10 1.404(9) . ?
C9 C14 1.539(9) . ?
C10 C11 1.541(9) . ?
C11 C12 1.548(9) . ?
C11 C16 1.512(10) . ?
C12 C13 1.344(9) . ?
C12 C43 1.487(10) . ?
C13 C14 1.539(9) . ?
C13 C49 1.469(9) . ?
C14 C15 1.521(10) . ?
C15 C16 1.420(9) . ?
C15 C20 1.360(9) . ?
C16 C17 1.368(9) . ?
C17 C18 1.403(10) . ?
C18 C19 1.401(9) . ?
C19 C20 1.390(9) . ?
C19 C24 1.504(10) . ?
C20 C21 1.526(9) . ?
C21 C22 1.551(9) . ?
C21 C27 1.534(9) 2_656 ?
C22 C23 1.358(10) . ?
C22 C55 1.498(9) . ?
C23 C24 1.542(9) . ?
C23 C61 1.442(10) . ?
C24 C26 1.531(8) 2_656 ?
C25 C26 1.371(9) . ?
C25 C30 1.408(8) . ?
C26 C27 1.386(9) . ?
C27 C28 1.355(8) . ?
C28 C29 1.399(9) . ?
C29 C30 1.376(10) . ?
C31 C32 1.405(10) . ?
C31 C36 1.395(10) . ?
C32 C33 1.369(10) . ?
C33 C34 1.374(10) . ?
C34 C35 1.367(11) . ?
C35 C36 1.386(11) . ?
C37 C38 1.385(10) . ?
C37 C42 1.406(10) . ?
C38 C39 1.407(11) . ?
C39 C40 1.401(12) . ?
C40 C41 1.364(12) . ?
C41 C42 1.351(11) . ?
C43 C44 1.380(10) . ?
C43 C48 1.361(11) . ?
C44 C45 1.385(12) . ?
C45 C46 1.355(14) . ?
C46 C47 1.365(14) . ?
C47 C48 1.364(13) . ?
C49 C50 1.391(10) . ?
C49 C54 1.397(10) . ?
C50 C51 1.412(11) . ?
C51 C52 1.366(13) . ?
C52 C53 1.398(13) . ?
C53 C54 1.372(11) . ?
C55 C56 1.388(9) . ?
C55 C60 1.378(10) . ?
C56 C57 1.379(10) . ?
C57 C58 1.368(11) . ?
C58 C59 1.366(10) . ?
C59 C60 1.388(10) . ?
C61 C62 1.376(11) . ?
C61 C66 1.383(11) . ?
C62 C63 1.415(14) . ?
C63 C64 1.308(14) . ?
C64 C65 1.347(13) . ?
C65 C66 1.383(13) . ?
O1 C67 1.417(7) . ?
O1 C70 1.416(8) . ?
C67 C68 1.528(7) . ?
C68 C69 1.506(8) . ?
C69 C70 1.459(8) . ?
C75 C74 1.525(10) . ?
C74 C73 1.534(10) . ?
C73 C72 1.531(10) . ?
C72 C71 1.537(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 111.2(5) . . ?
C10 C1 C2 129.7(6) . . ?
C10 C1 C6 118.8(6) . . ?
C3 C2 C1 109.6(5) . . ?
C3 C2 C30 103.9(5) . . ?
C30 C2 C1 104.1(5) . . ?
C4 C3 C2 114.4(6) . . ?
C4 C3 C37 126.6(7) . . ?
C37 C3 C2 118.1(6) . . ?
C3 C4 C5 112.2(6) . . ?
C3 C4 C31 128.7(7) . . ?
C31 C4 C5 119.1(6) . . ?
C6 C5 C4 108.4(5) . . ?
C25 C5 C4 106.9(5) . . ?
C25 C5 C6 105.0(5) . . ?
C1 C6 C5 112.5(5) . . ?
C7 C6 C1 121.0(6) . . ?
C7 C6 C5 126.0(6) . . ?
C6 C7 C8 119.7(6) . . ?
C9 C8 C7 118.9(6) . . ?
C8 C9 C10 121.1(6) . . ?
C8 C9 C14 125.4(6) . . ?
C10 C9 C14 113.2(6) . . ?
C1 C10 C9 120.4(6) . . ?
C1 C10 C11 128.0(6) . . ?
C9 C10 C11 110.9(6) . . ?
C10 C11 C12 107.4(5) . . ?
C16 C11 C10 105.4(5) . . ?
C16 C11 C12 106.8(5) . . ?
C13 C12 C11 113.2(6) . . ?
C13 C12 C43 129.0(6) . . ?
C43 C12 C11 117.4(6) . . ?
C12 C13 C14 113.3(6) . . ?
C12 C13 C49 127.9(7) . . ?
C49 C13 C14 118.8(6) . . ?
C9 C14 C13 106.9(6) . . ?
C15 C14 C9 104.5(5) . . ?
C15 C14 C13 106.8(5) . . ?
C16 C15 C14 112.1(6) . . ?
C20 C15 C14 129.2(6) . . ?
C20 C15 C16 118.7(6) . . ?
C15 C16 C11 112.1(6) . . ?
C17 C16 C11 126.7(6) . . ?
C17 C16 C15 121.1(7) . . ?
C16 C17 C18 119.7(6) . . ?
C19 C18 C17 119.1(7) . . ?
C18 C19 C24 125.3(6) . . ?
C20 C19 C18 120.1(7) . . ?
C20 C19 C24 114.5(6) . . ?
C15 C20 C19 121.2(6) . . ?
C15 C20 C21 128.1(6) . . ?
C19 C20 C21 110.7(6) . . ?
C20 C21 C22 107.5(5) . . ?
C20 C21 C27 105.6(5) . 2_656 ?
C27 C21 C22 106.0(6) 2_656 . ?
C23 C22 C21 113.3(6) . . ?
C23 C22 C55 129.5(7) . . ?
C55 C22 C21 117.2(6) . . ?
C22 C23 C24 112.2(6) . . ?
C22 C23 C61 129.6(6) . . ?
C61 C23 C24 118.2(6) . . ?
C19 C24 C23 108.5(5) . . ?
C19 C24 C26 104.2(5) . 2_656 ?
C26 C24 C23 105.1(5) 2_656 . ?
C26 C25 C5 129.9(6) . . ?
C26 C25 C30 118.0(6) . . ?
C30 C25 C5 112.0(6) . . ?
C25 C26 C24 126.0(6) . 2_656 ?
C25 C26 C27 120.4(6) . . ?
C27 C26 C24 113.5(6) . 2_656 ?
C26 C27 C21 111.3(5) . 2_656 ?
C28 C27 C21 126.4(6) . 2_656 ?
C28 C27 C26 122.1(6) . . ?
C27 C28 C29 118.3(7) . . ?
C30 C29 C28 120.3(6) . . ?
C25 C30 C2 112.2(6) . . ?
C29 C30 C2 126.9(6) . . ?
C29 C30 C25 120.8(6) . . ?
C32 C31 C4 121.4(7) . . ?
C36 C31 C4 120.4(7) . . ?
C36 C31 C32 118.2(7) . . ?
C33 C32 C31 120.5(7) . . ?
C32 C33 C34 121.5(8) . . ?
C35 C34 C33 118.2(7) . . ?
C34 C35 C36 122.4(8) . . ?
C35 C36 C31 119.2(8) . . ?
C38 C37 C3 122.6(7) . . ?
C38 C37 C42 116.8(7) . . ?
C42 C37 C3 120.5(7) . . ?
C37 C38 C39 121.0(8) . . ?
C40 C39 C38 119.1(8) . . ?
C41 C40 C39 120.0(8) . . ?
C42 C41 C40 120.1(8) . . ?
C41 C42 C37 123.0(8) . . ?
C44 C43 C12 122.1(7) . . ?
C48 C43 C12 120.1(7) . . ?
C48 C43 C44 117.8(8) . . ?
C43 C44 C45 120.9(9) . . ?
C46 C45 C44 120.0(9) . . ?
C45 C46 C47 119.1(9) . . ?
C48 C47 C46 121.0(10) . . ?
C43 C48 C47 121.1(10) . . ?
C50 C49 C13 120.2(7) . . ?
C50 C49 C54 117.9(7) . . ?
C54 C49 C13 121.9(7) . . ?
C49 C50 C51 120.1(8) . . ?
C52 C51 C50 120.5(9) . . ?
C51 C52 C53 119.8(8) . . ?
C54 C53 C52 119.5(9) . . ?
C53 C54 C49 122.2(8) . . ?
C56 C55 C22 120.8(6) . . ?
C60 C55 C22 120.7(6) . . ?
C60 C55 C56 118.5(6) . . ?
C57 C56 C55 120.2(7) . . ?
C58 C57 C56 120.4(7) . . ?
C59 C58 C57 120.3(7) . . ?
C58 C59 C60 119.5(7) . . ?
C55 C60 C59 121.0(7) . . ?
C62 C61 C23 124.0(7) . . ?
C62 C61 C66 114.5(8) . . ?
C66 C61 C23 121.2(7) . . ?
C61 C62 C63 120.7(10) . . ?
C64 C63 C62 122.1(10) . . ?
C63 C64 C65 119.3(10) . . ?
C64 C65 C66 119.6(10) . . ?
C61 C66 C65 123.5(9) . . ?
C70 O1 C67 112.3(6) . . ?
O1 C67 C68 106.8(6) . . ?
C69 C68 C67 102.5(6) . . ?
C70 C69 C68 108.6(8) . . ?
O1 C70 C69 106.2(7) . . ?
C75 C74 C73 112.5(10) . . ?
C72 C73 C74 112.2(10) . . ?
C73 C72 C71 111.5(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -52.4(8) . . . . ?
C1 C2 C3 C37 138.1(6) . . . . ?
C1 C2 C30 C25 57.4(7) . . . . ?
C1 C2 C30 C29 -118.7(7) . . . . ?
C1 C6 C7 C8 -1.2(11) . . . . ?
C1 C10 C11 C12 133.6(7) . . . . ?
C1 C10 C11 C16 -112.8(8) . . . . ?
C2 C1 C6 C5 2.4(8) . . . . ?
C2 C1 C6 C7 175.4(7) . . . . ?
C2 C1 C10 C9 -173.0(7) . . . . ?
C2 C1 C10 C11 -2.7(12) . . . . ?
C2 C3 C4 C5 -2.4(8) . . . . ?
C2 C3 C4 C31 179.8(7) . . . . ?
C2 C3 C37 C38 -55.3(10) . . . . ?
C2 C3 C37 C42 120.0(8) . . . . ?
C3 C2 C30 C25 -57.3(7) . . . . ?
C3 C2 C30 C29 126.5(7) . . . . ?
C3 C4 C5 C6 57.0(8) . . . . ?
C3 C4 C5 C25 -55.7(7) . . . . ?
C3 C4 C31 C32 -40.4(11) . . . . ?
C3 C4 C31 C36 142.9(8) . . . . ?
C3 C37 C38 C39 176.0(8) . . . . ?
C3 C37 C42 C41 -176.0(8) . . . . ?
C4 C3 C37 C38 136.5(8) . . . . ?
C4 C3 C37 C42 -48.2(11) . . . . ?
C4 C5 C6 C1 -56.6(8) . . . . ?
C4 C5 C6 C7 130.8(8) . . . . ?
C4 C5 C25 C26 -124.5(7) . . . . ?
C4 C5 C25 C30 55.3(7) . . . . ?
C4 C31 C32 C33 -179.7(7) . . . . ?
C4 C31 C36 C35 180.0(7) . . . . ?
C5 C4 C31 C32 142.0(7) . . . . ?
C5 C4 C31 C36 -34.7(10) . . . . ?
C5 C6 C7 C8 170.8(7) . . . . ?
C5 C25 C26 C24 -2.6(11) . . . 2_656 ?
C5 C25 C26 C27 180.0(6) . . . . ?
C5 C25 C30 C2 1.8(8) . . . . ?
C5 C25 C30 C29 178.2(6) . . . . ?
C6 C1 C2 C3 51.3(8) . . . . ?
C6 C1 C2 C30 -59.3(7) . . . . ?
C6 C1 C10 C9 0.7(10) . . . . ?
C6 C1 C10 C11 170.9(7) . . . . ?
C6 C5 C25 C26 120.5(7) . . . . ?
C6 C5 C25 C30 -59.7(7) . . . . ?
C6 C7 C8 C9 0.4(10) . . . . ?
C7 C8 C9 C10 1.0(10) . . . . ?
C7 C8 C9 C14 -171.8(6) . . . . ?
C8 C9 C10 C1 -1.5(11) . . . . ?
C8 C9 C10 C11 -173.3(6) . . . . ?
C8 C9 C14 C13 -131.7(7) . . . . ?
C8 C9 C14 C15 115.2(7) . . . . ?
C9 C10 C11 C12 -55.4(7) . . . . ?
C9 C10 C11 C16 58.2(7) . . . . ?
C9 C14 C15 C16 57.6(6) . . . . ?
C9 C14 C15 C20 -118.8(7) . . . . ?
C10 C1 C2 C3 -134.7(8) . . . . ?
C10 C1 C2 C30 114.7(8) . . . . ?
C10 C1 C6 C5 -172.4(7) . . . . ?
C10 C1 C6 C7 0.7(11) . . . . ?
C10 C9 C14 C13 55.1(7) . . . . ?
C10 C9 C14 C15 -58.0(7) . . . . ?
C10 C11 C12 C13 56.3(8) . . . . ?
C10 C11 C12 C43 -130.4(7) . . . . ?
C10 C11 C16 C15 -58.6(6) . . . . ?
C10 C11 C16 C17 120.3(7) . . . . ?
C11 C12 C13 C14 0.2(9) . . . . ?
C11 C12 C13 C49 -179.1(7) . . . . ?
C11 C12 C43 C44 -128.3(7) . . . . ?
C11 C12 C43 C48 50.9(11) . . . . ?
C11 C16 C17 C18 -177.5(6) . . . . ?
C12 C11 C16 C15 55.4(6) . . . . ?
C12 C11 C16 C17 -125.7(7) . . . . ?
C12 C13 C14 C9 -55.5(8) . . . . ?
C12 C13 C14 C15 55.9(8) . . . . ?
C12 C13 C49 C50 -141.2(8) . . . . ?
C12 C13 C49 C54 37.3(11) . . . . ?
C12 C43 C44 C45 177.9(7) . . . . ?
C12 C43 C48 C47 -178.3(10) . . . . ?
C13 C12 C43 C44 43.7(12) . . . . ?
C13 C12 C43 C48 -137.0(10) . . . . ?
C13 C14 C15 C16 -55.5(7) . . . . ?
C13 C14 C15 C20 128.1(7) . . . . ?
C13 C49 C50 C51 178.2(6) . . . . ?
C13 C49 C54 C53 -177.8(7) . . . . ?
C14 C9 C10 C1 172.0(6) . . . . ?
C14 C9 C10 C11 0.2(8) . . . . ?
C14 C13 C49 C50 39.5(9) . . . . ?
C14 C13 C49 C54 -142.0(7) . . . . ?
C14 C15 C16 C11 0.0(7) . . . . ?
C14 C15 C16 C17 -179.0(6) . . . . ?
C14 C15 C20 C19 179.0(6) . . . . ?
C14 C15 C20 C21 0.0(10) . . . . ?
C15 C16 C17 C18 1.4(9) . . . . ?
C15 C20 C21 C22 -126.0(7) . . . . ?
C15 C20 C21 C27 121.1(7) . . . 2_656 ?
C16 C11 C12 C13 -56.4(7) . . . . ?
C16 C11 C12 C43 116.9(7) . . . . ?
C16 C15 C20 C19 2.9(9) . . . . ?
C16 C15 C20 C21 -176.1(5) . . . . ?
C16 C17 C18 C19 -1.2(9) . . . . ?
C17 C18 C19 C20 1.8(9) . . . . ?
C17 C18 C19 C24 177.8(6) . . . . ?
C18 C19 C20 C15 -2.7(9) . . . . ?
C18 C19 C20 C21 176.4(5) . . . . ?
C18 C19 C24 C23 129.2(6) . . . . ?
C18 C19 C24 C26 -119.3(6) . . . 2_656 ?
C19 C20 C21 C22 55.0(7) . . . . ?
C19 C20 C21 C27 -57.9(6) . . . 2_656 ?
C20 C15 C16 C11 176.8(5) . . . . ?
C20 C15 C16 C17 -2.3(9) . . . . ?
C20 C19 C24 C23 -54.6(7) . . . . ?
C20 C19 C24 C26 56.9(7) . . . 2_656 ?
C20 C21 C22 C23 -57.3(8) . . . . ?
C20 C21 C22 C55 121.6(6) . . . . ?
C21 C22 C23 C24 2.7(8) . . . . ?
C21 C22 C23 C61 -175.4(7) . . . . ?
C21 C22 C55 C56 -138.4(7) . . . . ?
C21 C22 C55 C60 39.9(10) . . . . ?
C21 C27 C28 C29 -176.4(6) 2_656 . . . ?
C22 C23 C24 C19 52.5(7) . . . . ?
C22 C23 C24 C26 -58.5(7) . . . 2_656 ?
C22 C23 C61 C62 40.1(13) . . . . ?
C22 C23 C61 C66 -146.6(8) . . . . ?
C22 C55 C56 C57 175.4(7) . . . . ?
C22 C55 C60 C59 -177.3(8) . . . . ?
C23 C22 C55 C56 40.3(12) . . . . ?
C23 C22 C55 C60 -141.3(8) . . . . ?
C23 C61 C62 C63 177.4(10) . . . . ?
C23 C61 C66 C65 -173.6(9) . . . . ?
C24 C19 C20 C15 -179.1(5) . . . . ?
C24 C19 C20 C21 0.0(7) . . . . ?
C24 C23 C61 C62 -137.9(8) . . . . ?
C24 C23 C61 C66 35.4(10) . . . . ?
C24 C26 C27 C21 -0.5(8) 2_656 . . 2_656 ?
C24 C26 C27 C28 -176.4(6) 2_656 . . . ?
C25 C5 C6 C1 57.4(7) . . . . ?
C25 C5 C6 C7 -115.2(8) . . . . ?
C25 C26 C27 C21 177.3(6) . . . 2_656 ?
C25 C26 C27 C28 1.4(10) . . . . ?
C26 C25 C30 C2 -178.4(6) . . . . ?
C26 C25 C30 C29 -2.0(10) . . . . ?
C26 C27 C28 C29 -1.2(10) . . . . ?
C27 C21 C22 C23 55.3(7) 2_656 . . . ?
C27 C21 C22 C55 -125.8(6) 2_656 . . . ?
C27 C28 C29 C30 -0.6(10) . . . . ?
C28 C29 C30 C2 178.1(6) . . . . ?
C28 C29 C30 C25 2.2(10) . . . . ?
C30 C2 C3 C4 58.4(7) . . . . ?
C30 C2 C3 C37 -111.2(6) . . . . ?
C30 C25 C26 C24 177.7(6) . . . 2_656 ?
C30 C25 C26 C27 0.2(10) . . . . ?
C31 C4 C5 C6 -124.9(6) . . . . ?
C31 C4 C5 C25 122.3(7) . . . . ?
C31 C32 C33 C34 1.9(12) . . . . ?
C32 C31 C36 C35 3.2(11) . . . . ?
C32 C33 C34 C35 -1.0(12) . . . . ?
C33 C34 C35 C36 1.3(13) . . . . ?
C34 C35 C36 C31 -2.4(13) . . . . ?
C36 C31 C32 C33 -2.9(11) . . . . ?
C37 C3 C4 C5 166.2(6) . . . . ?
C37 C3 C4 C31 -11.6(12) . . . . ?
C37 C38 C39 C40 -1.0(14) . . . . ?
C38 C37 C42 C41 -0.5(12) . . . . ?
C38 C39 C40 C41 1.3(14) . . . . ?
C39 C40 C41 C42 -1.2(14) . . . . ?
C40 C41 C42 C37 0.8(14) . . . . ?
C42 C37 C38 C39 0.6(12) . . . . ?
C43 C12 C13 C14 -172.1(7) . . . . ?
C43 C12 C13 C49 8.6(13) . . . . ?
C43 C44 C45 C46 2.0(14) . . . . ?
C44 C43 C48 C47 1.0(16) . . . . ?
C44 C45 C46 C47 -2.1(16) . . . . ?
C45 C46 C47 C48 1.7(19) . . . . ?
C46 C47 C48 C43 -1(2) . . . . ?
C48 C43 C44 C45 -1.4(13) . . . . ?
C49 C13 C14 C9 123.8(7) . . . . ?
C49 C13 C14 C15 -124.7(7) . . . . ?
C49 C50 C51 C52 -1.3(11) . . . . ?
C50 C49 C54 C53 0.8(11) . . . . ?
C50 C51 C52 C53 2.6(13) . . . . ?
C51 C52 C53 C54 -2.2(13) . . . . ?
C52 C53 C54 C49 0.5(12) . . . . ?
C54 C49 C50 C51 -0.4(10) . . . . ?
C55 C22 C23 C24 -176.1(7) . . . . ?
C55 C22 C23 C61 5.8(13) . . . . ?
C55 C56 C57 C58 2.5(13) . . . . ?
C56 C55 C60 C59 1.1(12) . . . . ?
C56 C57 C58 C59 0.1(13) . . . . ?
C57 C58 C59 C60 -2.0(13) . . . . ?
C58 C59 C60 C55 1.4(13) . . . . ?
C60 C55 C56 C57 -3.0(12) . . . . ?
C61 C23 C24 C19 -129.2(6) . . . . ?
C61 C23 C24 C26 119.8(6) . . . 2_656 ?
C61 C62 C63 C64 -4(2) . . . . ?
C62 C61 C66 C65 0.3(14) . . . . ?
C62 C63 C64 C65 0(2) . . . . ?
C63 C64 C65 C66 4.4(17) . . . . ?
C64 C65 C66 C61 -4.5(16) . . . . ?
C66 C61 C62 C63 3.7(15) . . . . ?
O1 C67 C68 C69 -15.9(11) . . . . ?
C67 O1 C70 C69 4.8(13) . . . . ?
C67 C68 C69 C70 19.1(12) . . . . ?
C68 C69 C70 O1 -15.4(13) . . . . ?
C70 O1 C67 C68 7.4(11) . . . . ?
C75 C74 C73 C72 47(4) . . . . ?
C74 C73 C72 C71 -180(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.974
_oxdiff_exptl_absorpt_empirical_full_min 0.478
