# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_oajvlb
_database_code_depnum_ccdc_archive 'CCDC 2045214'
loop_
_audit_author_name
_audit_author_address
'Stephen P. Argent'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2020-11-18 deposited with the CCDC.	2020-12-04 downloaded from the CCDC.
;
_nottingham_internal_coll_name   OAJVLB
_nottingham_internal_coll_number 15456
_nottingham_internal_coll_client AJV/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 10.00, 2.50'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   18/01/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 29/02/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 26/10/16
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 26/10/16
_nottingham_internal_refinement_user pcxav1/pczspa
_nottingham_internal_self_archive_date 26/10/16
_nottingham_internal_self_validation_date 26/10/16
_nottingham_internal_self_validation_user pcxav1
_nottingham_internal_validation_date 28/04/2020
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date ?
_refine_special_details          
;
 An electron density peak of 1.39 e A^-3 is located 0.78 A
 from methyl carbon C24. The peak cannot be sensibly
 modelled as part of a disorder component nor explained by
 unaccounted twinning. It is possible the peak is a result
 of deficiency in absorption correction due to the heavy
 iodine atom in the structure.

 The anisotropic displacement parameter of methyl carbon
 C24 is restrained to be more isotropic (ISOR) and have
 a rigid bond with quaternary carbon C23. The geometry of
 the tert-butyl moiety is restrained to have three-fold
 symmetry (SADI). These restraints are applied to
 mitigate the effects of the unmodelled electron density
 peak on the geometry and displacement parameter of C24.
;
_audit_creation_date             2020-07-02
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        OAJVLB
_chemical_formula_moiety         'C26 H29 I'
_chemical_formula_sum            'C26 H29 I'
_chemical_formula_weight         468.39
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C26 H29 I1'
_chemical_oxdiff_usercomment     
'OAJVLB #15456 GVB-854 IN FOMBLIN FILM ON MICROMOUNT FOR AJV/DLK'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.1749(2)
_cell_length_b                   13.2712(2)
_cell_length_c                   13.8896(2)
_cell_angle_alpha                90
_cell_angle_beta                 109.910(2)
_cell_angle_gamma                90
_cell_volume                     2283.39(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5542
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.3950
_cell_measurement_theta_min      4.7400
_shelx_estimated_absorpt_T_max   0.597
_shelx_estimated_absorpt_T_min   0.311
_exptl_absorpt_coefficient_mu    11.046
_exptl_absorpt_correction_T_max  0.636
_exptl_absorpt_correction_T_min  0.411
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1060.000
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -9 1 0.0413
0 9 0 0.0345
4 5 3 0.0433
4 -6 3 0.0475
-4 -6 -3 0.0591
1 -7 -5 0.0456
-7 -2 7 0.0311
-8 0 7 0.0263
8 0 -6 0.0197
-5 2 -5 0.0672
-5 -1 -5 0.0591
-6 3 -3 0.0639

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 'Recrystallised from ethanol.'
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.052
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.5680 -8.5219 0.8879 0.1036 -0.0378 0.9939
0.0014 8.9886 -0.0009 0.0426 0.0231 -1.0425
3.9997 4.9966 2.9959 0.6791 -0.2358 -0.5585
3.9979 -5.9895 2.9970 0.6271 -0.2641 0.7157
-3.9998 -5.9953 -2.9958 -0.6838 0.2333 0.6743
0.6542 -7.0084 -5.1211 -0.5429 -0.2964 0.7858
-6.9926 -1.9952 6.9946 0.1895 0.9476 0.2611
-7.5049 -0.2197 6.7533 0.1296 0.9901 0.0533
7.8809 0.4330 -6.0929 -0.0254 -0.9969 -0.0740
-4.7102 1.6759 -5.1914 -0.9468 0.2269 -0.2282
-4.8451 -0.6956 -5.2138 -0.9715 0.2325 0.0465
-5.6899 3.1662 -3.4676 -0.8301 0.3957 -0.3929

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8951
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.580
_diffrn_reflns_theta_min         3.996
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9682
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     90.00 178.00   1.00   10.00    --  104.50  30.00 120.00   88
  2  ω     59.00 162.00   1.00   10.00    --  104.50  15.00-120.00  103
  3  ω     46.00  91.00   1.00   10.00    --  104.50 -45.00-120.00   45
  4  ω     36.00 106.00   1.00   10.00    --  104.50 -94.00-180.00   70
  5  ω     28.00 106.00   1.00   10.00    --  104.50 -94.00  90.00   78
  6  ω     47.00  85.00   1.00   10.00    --  104.50 -45.00 150.00   38
  7  ω    -43.00   8.00   1.00    2.50    --  -38.50  38.00 -60.00   51
  8  ω    -46.00 -12.00   1.00    2.50    --  -38.50  38.00 -90.00   34
  9  ω    -68.00 -42.00   1.00    2.50    --  -38.50  77.00 -90.00   26
 10  ω   -108.00 -12.00   1.00    2.50    --  -38.50 -57.00 -60.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0815210000
_diffrn_orient_matrix_UB_12      0.0047337000
_diffrn_orient_matrix_UB_13      0.1099416000
_diffrn_orient_matrix_UB_21      -0.0939117000
_diffrn_orient_matrix_UB_22      0.0025900000
_diffrn_orient_matrix_UB_23      0.0423352000
_diffrn_orient_matrix_UB_31      0.0011913000
_diffrn_orient_matrix_UB_32      -0.1159825000
_diffrn_orient_matrix_UB_33      0.0054394000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4017
_reflns_number_total             4470
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         1.386
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4470
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0255
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0333P)²+1.0914P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0644
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C25-C23 \\sim C26-C23 \\sim C24-C23
 with sigma of 0.02
 C24-C25 \\sim C25-C26 \\sim C26-C24
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C24, C23
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18), C19(H19)
5.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.70804(2) 0.92462(2) 0.35119(2) 0.02466(6) Uani 1 1 d . . . . .
C1 C 0.73881(19) 0.77957(17) 0.41630(18) 0.0208(4) Uani 1 1 d . . . . .
C2 C 0.83413(19) 0.73073(18) 0.41966(18) 0.0223(5) Uani 1 1 d . . . . .
C3 C 0.85318(19) 0.63521(19) 0.46401(19) 0.0244(5) Uani 1 1 d . . . . .
H3 H 0.917510 0.600942 0.467050 0.029 Uiso 1 1 calc R U . . .
C4 C 0.7817(2) 0.58768(18) 0.50420(19) 0.0247(5) Uani 1 1 d . . . . .
C5 C 0.6880(2) 0.63966(19) 0.49861(19) 0.0257(5) Uani 1 1 d . . . . .
H5 H 0.637926 0.608723 0.524991 0.031 Uiso 1 1 calc R U . . .
C6 C 0.66506(19) 0.73610(18) 0.45539(18) 0.0232(5) Uani 1 1 d . . . . .
C7 C 0.91208(19) 0.77646(18) 0.37519(19) 0.0234(5) Uani 1 1 d . . . . .
C8 C 0.9967(2) 0.8369(2) 0.4367(2) 0.0300(5) Uani 1 1 d . . . . .
C9 C 1.0668(2) 0.8804(2) 0.3930(3) 0.0397(7) Uani 1 1 d . . . . .
H9 H 1.124249 0.921824 0.433586 0.048 Uiso 1 1 calc R U . . .
C10 C 1.0537(2) 0.8639(2) 0.2910(3) 0.0419(7) Uani 1 1 d . . . . .
H10 H 1.102191 0.893928 0.262168 0.050 Uiso 1 1 calc R U . . .
C11 C 0.9705(2) 0.8040(2) 0.2311(2) 0.0365(6) Uani 1 1 d . . . . .
H11 H 0.962476 0.792640 0.161351 0.044 Uiso 1 1 calc R U . . .
C12 C 0.8982(2) 0.75999(19) 0.2721(2) 0.0281(5) Uani 1 1 d . . . . .
C13 C 1.0113(2) 0.8555(3) 0.5477(2) 0.0412(7) Uani 1 1 d . . . . .
H13A H 0.945152 0.885041 0.552830 0.062 Uiso 1 1 calc R U . . .
H13B H 1.071691 0.902087 0.577156 0.062 Uiso 1 1 calc R U . . .
H13C H 1.026541 0.791608 0.585175 0.062 Uiso 1 1 calc R U . . .
C14 C 0.8051(3) 0.6978(2) 0.2061(2) 0.0351(6) Uani 1 1 d . . . . .
H14A H 0.807007 0.631196 0.237097 0.053 Uiso 1 1 calc R U . . .
H14B H 0.810439 0.690254 0.137798 0.053 Uiso 1 1 calc R U . . .
H14C H 0.737047 0.731483 0.200341 0.053 Uiso 1 1 calc R U . . .
C15 C 0.56300(19) 0.78690(18) 0.45358(19) 0.0239(5) Uani 1 1 d . . . . .
C16 C 0.4689(2) 0.7764(2) 0.3690(2) 0.0325(6) Uani 1 1 d . . . . .
C17 C 0.3750(2) 0.8238(2) 0.3702(2) 0.0374(6) Uani 1 1 d . . . . .
H17 H 0.310416 0.817416 0.312953 0.045 Uiso 1 1 calc R U . . .
C18 C 0.3752(2) 0.8801(2) 0.4541(3) 0.0362(6) Uani 1 1 d . . . . .
H18 H 0.310515 0.911556 0.454337 0.043 Uiso 1 1 calc R U . . .
C19 C 0.4680(2) 0.8908(2) 0.5367(2) 0.0334(6) Uani 1 1 d . . . . .
H19 H 0.467117 0.929939 0.593677 0.040 Uiso 1 1 calc R U . . .
C20 C 0.5637(2) 0.84480(19) 0.5381(2) 0.0259(5) Uani 1 1 d . . . . .
C21 C 0.4680(3) 0.7153(3) 0.2769(3) 0.0545(9) Uani 1 1 d . . . . .
H21A H 0.400245 0.727164 0.220381 0.082 Uiso 1 1 calc R U . . .
H21B H 0.474251 0.643492 0.294560 0.082 Uiso 1 1 calc R U . . .
H21C H 0.528951 0.735482 0.255928 0.082 Uiso 1 1 calc R U . . .
C22 C 0.6649(2) 0.8578(3) 0.6289(2) 0.0394(7) Uani 1 1 d . . . . .
H22A H 0.681208 0.794971 0.668160 0.059 Uiso 1 1 calc R U . . .
H22B H 0.654582 0.912199 0.672419 0.059 Uiso 1 1 calc R U . . .
H22C H 0.724909 0.874889 0.605301 0.059 Uiso 1 1 calc R U . . .
C23 C 0.8076(2) 0.48201(19) 0.5510(2) 0.0292(5) Uani 1 1 d D . . . .
C24 C 0.9158(2) 0.4871(2) 0.6444(2) 0.0370(6) Uani 1 1 d D U . . .
H24A H 0.973896 0.511079 0.621236 0.055 Uiso 1 1 calc R U . . .
H24B H 0.933770 0.419755 0.674461 0.055 Uiso 1 1 calc R U . . .
H24C H 0.907197 0.533469 0.696019 0.055 Uiso 1 1 calc R U . . .
C25 C 0.8187(3) 0.4090(2) 0.4691(2) 0.0349(6) Uani 1 1 d D . . . .
H25A H 0.750386 0.406179 0.411559 0.052 Uiso 1 1 calc R U . . .
H25B H 0.836842 0.341592 0.498829 0.052 Uiso 1 1 calc R U . . .
H25C H 0.876138 0.432656 0.444618 0.052 Uiso 1 1 calc R U . . .
C26 C 0.7183(3) 0.4417(2) 0.5887(3) 0.0405(7) Uani 1 1 d D . . . .
H26A H 0.710824 0.486378 0.642060 0.061 Uiso 1 1 calc R U . . .
H26B H 0.737312 0.373823 0.616684 0.061 Uiso 1 1 calc R U . . .
H26C H 0.649830 0.439357 0.531267 0.061 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C1 2.107(2) . ?
C1 C2 1.400(3) . ?
C1 C6 1.390(3) . ?
C2 C3 1.394(3) . ?
C2 C7 1.496(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.398(4) . ?
C4 C5 1.393(3) . ?
C4 C23 1.534(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.402(4) . ?
C6 C15 1.497(3) . ?
C7 C8 1.403(4) . ?
C7 C12 1.398(4) . ?
C8 C9 1.391(4) . ?
C8 C13 1.507(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.385(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.380(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.393(4) . ?
C12 C14 1.504(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.395(4) . ?
C15 C20 1.401(4) . ?
C16 C17 1.392(4) . ?
C16 C21 1.512(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.384(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.370(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.395(4) . ?
C20 C22 1.500(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.569(4) . ?
C23 C25 1.540(4) . ?
C23 C26 1.537(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 I1 118.47(17) . . ?
C6 C1 I1 119.28(17) . . ?
C6 C1 C2 122.2(2) . . ?
C1 C2 C7 122.2(2) . . ?
C3 C2 C1 117.4(2) . . ?
C3 C2 C7 120.4(2) . . ?
C2 C3 H3 118.6 . . ?
C2 C3 C4 122.8(2) . . ?
C4 C3 H3 118.6 . . ?
C3 C4 C23 119.9(2) . . ?
C5 C4 C3 117.3(2) . . ?
C5 C4 C23 122.8(2) . . ?
C4 C5 H5 118.9 . . ?
C4 C5 C6 122.2(2) . . ?
C6 C5 H5 118.9 . . ?
C1 C6 C5 118.0(2) . . ?
C1 C6 C15 123.4(2) . . ?
C5 C6 C15 118.7(2) . . ?
C8 C7 C2 119.7(2) . . ?
C12 C7 C2 119.4(2) . . ?
C12 C7 C8 120.9(2) . . ?
C7 C8 C13 121.0(2) . . ?
C9 C8 C7 118.6(3) . . ?
C9 C8 C13 120.4(3) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 C8 120.7(3) . . ?
C10 C9 H9 119.6 . . ?
C9 C10 H10 119.8 . . ?
C11 C10 C9 120.3(3) . . ?
C11 C10 H10 119.8 . . ?
C10 C11 H11 119.7 . . ?
C10 C11 C12 120.5(3) . . ?
C12 C11 H11 119.7 . . ?
C7 C12 C14 120.3(2) . . ?
C11 C12 C7 119.0(3) . . ?
C11 C12 C14 120.7(3) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C6 120.3(2) . . ?
C16 C15 C20 120.7(2) . . ?
C20 C15 C6 118.9(2) . . ?
C15 C16 C21 121.0(2) . . ?
C17 C16 C15 118.9(3) . . ?
C17 C16 C21 120.1(3) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 C16 120.5(3) . . ?
C18 C17 H17 119.8 . . ?
C17 C18 H18 119.8 . . ?
C19 C18 C17 120.4(2) . . ?
C19 C18 H18 119.8 . . ?
C18 C19 H19 119.6 . . ?
C18 C19 C20 120.7(3) . . ?
C20 C19 H19 119.6 . . ?
C15 C20 C22 121.2(2) . . ?
C19 C20 C15 118.7(2) . . ?
C19 C20 C22 120.1(2) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C4 C23 C24 108.7(2) . . ?
C4 C23 C25 109.0(2) . . ?
C4 C23 C26 112.1(2) . . ?
C25 C23 C24 110.5(2) . . ?
C26 C23 C24 108.5(2) . . ?
C26 C23 C25 108.0(2) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
I1 C1 C2 C3 179.39(17) . . . . ?
I1 C1 C2 C7 -2.4(3) . . . . ?
I1 C1 C6 C5 -179.74(18) . . . . ?
I1 C1 C6 C15 0.3(3) . . . . ?
C1 C2 C3 C4 0.1(4) . . . . ?
C1 C2 C7 C8 90.7(3) . . . . ?
C1 C2 C7 C12 -88.0(3) . . . . ?
C1 C6 C15 C16 87.9(3) . . . . ?
C1 C6 C15 C20 -92.2(3) . . . . ?
C2 C1 C6 C5 -0.5(4) . . . . ?
C2 C1 C6 C15 179.5(2) . . . . ?
C2 C3 C4 C5 0.0(4) . . . . ?
C2 C3 C4 C23 179.4(2) . . . . ?
C2 C7 C8 C9 -178.6(2) . . . . ?
C2 C7 C8 C13 0.8(4) . . . . ?
C2 C7 C12 C11 179.2(2) . . . . ?
C2 C7 C12 C14 0.7(4) . . . . ?
C3 C2 C7 C8 -91.1(3) . . . . ?
C3 C2 C7 C12 90.2(3) . . . . ?
C3 C4 C5 C6 -0.4(4) . . . . ?
C3 C4 C23 C24 61.3(3) . . . . ?
C3 C4 C23 C25 -59.1(3) . . . . ?
C3 C4 C23 C26 -178.7(3) . . . . ?
C4 C5 C6 C1 0.7(4) . . . . ?
C4 C5 C6 C15 -179.4(2) . . . . ?
C5 C4 C23 C24 -119.3(3) . . . . ?
C5 C4 C23 C25 120.2(3) . . . . ?
C5 C4 C23 C26 0.6(4) . . . . ?
C5 C6 C15 C16 -92.1(3) . . . . ?
C5 C6 C15 C20 87.8(3) . . . . ?
C6 C1 C2 C3 0.2(4) . . . . ?
C6 C1 C2 C7 178.4(2) . . . . ?
C6 C15 C16 C17 179.4(2) . . . . ?
C6 C15 C16 C21 -1.0(4) . . . . ?
C6 C15 C20 C19 -179.1(2) . . . . ?
C6 C15 C20 C22 1.0(4) . . . . ?
C7 C2 C3 C4 -178.2(2) . . . . ?
C7 C8 C9 C10 -0.4(4) . . . . ?
C8 C7 C12 C11 0.5(4) . . . . ?
C8 C7 C12 C14 -178.0(2) . . . . ?
C8 C9 C10 C11 0.1(5) . . . . ?
C9 C10 C11 C12 0.5(5) . . . . ?
C10 C11 C12 C7 -0.8(4) . . . . ?
C10 C11 C12 C14 177.7(3) . . . . ?
C12 C7 C8 C9 0.0(4) . . . . ?
C12 C7 C8 C13 179.5(3) . . . . ?
C13 C8 C9 C10 -179.8(3) . . . . ?
C15 C16 C17 C18 -0.2(4) . . . . ?
C16 C15 C20 C19 0.8(4) . . . . ?
C16 C15 C20 C22 -179.1(3) . . . . ?
C16 C17 C18 C19 0.6(5) . . . . ?
C17 C18 C19 C20 -0.3(4) . . . . ?
C18 C19 C20 C15 -0.4(4) . . . . ?
C18 C19 C20 C22 179.5(3) . . . . ?
C20 C15 C16 C17 -0.5(4) . . . . ?
C20 C15 C16 C21 179.1(3) . . . . ?
C21 C16 C17 C18 -179.8(3) . . . . ?
C23 C4 C5 C6 -179.8(2) . . . . ?

_olex2_date_sample_data_collection 2015-01-14
_olex2_date_sample_submission    2015-01-07
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_original_sample_id OAJVLB
_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 1.574
_oxdiff_exptl_absorpt_empirical_full_min 0.687
####################################################################### 
# 
# 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_kewjma
_database_code_depnum_ccdc_archive 'CCDC 2045216'
loop_
_audit_author_name
_audit_author_address
'Stephen P. Argent'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2020-11-18 deposited with the CCDC.	2020-12-04 downloaded from the CCDC.
;
_nottingham_internal_coll_name   KEWJMA
_nottingham_internal_coll_number 16648
_nottingham_internal_coll_client KEW/JM
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 8.00, 2.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   09/11/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 09/11/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 09/11/2016
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 09/11/2016
_nottingham_internal_refinement_user pcxav1
_nottingham_internal_self_archive_date 09/11/2016
_nottingham_internal_self_validation_date 09/11/2016
_nottingham_internal_self_validation_user pcxav1
_nottingham_internal_validation_date ?
_nottingham_internal_validation_user ?
_nottingham_internal_archive_date ?
_refine_special_details          ?
_audit_creation_date             2020-06-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        KEWJMA
_chemical_formula_moiety         'C22 H20 Cl I'
_chemical_formula_sum            'C22 H20 Cl I'
_chemical_formula_weight         446.73
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C22 H20 Cl I'
_chemical_oxdiff_usercomment     
'KEWJMA #16648 GVB-1221 IN FOMBLIN FILM ON MICROMOUNT FOR KEW/JM'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.3499(2)
_cell_length_b                   34.7269(7)
_cell_length_c                   13.4766(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.064(2)
_cell_angle_gamma                90
_cell_volume                     3847.63(15)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9412
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.5030
_cell_measurement_theta_min      4.2040
_shelx_estimated_absorpt_T_max   0.397
_shelx_estimated_absorpt_T_min   0.039
_exptl_absorpt_coefficient_mu    14.332
_exptl_absorpt_correction_T_max  0.458
_exptl_absorpt_correction_T_min  0.068
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -22 -1 0.0586
-5 0 -1 0.2537
5 -3 1 0.3496
0 10 -8 0.0293
0 11 7 0.0558
-3 16 5 0.1635
0 -6 -8 0.0476
0 -16 6 0.0433
0 19 -5 0.0377
1 18 -5 0.0661
1 22 1 0.0691
1 12 -7 0.0653
0 -16 -6 0.0501
0 23 0 0.0387
0 -11 8 0.0484

_exptl_crystal_recrystallization_method 
'Crystallised from diethyl ether via slow evaporation of the solvent.'
_exptl_crystal_size_max          0.649
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.079
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0040 -21.9626 -1.0156 -0.8144 -0.1708 -0.5199
-5.0098 0.0274 -0.9664 -0.5197 -0.1426 0.8001
5.0095 -3.0238 0.9642 0.4158 0.1056 -0.8743
-0.0154 10.0738 -7.9850 -0.0755 0.9278 0.4409
0.0152 10.9115 7.0017 0.7499 -0.5682 0.1027
-2.9930 15.9369 5.0269 0.5374 -0.4513 0.7403
-0.0168 -5.9068 -7.9970 -0.6295 0.7304 0.0452
0.0108 -16.0450 5.9824 -0.2376 -0.8007 -0.5409
-0.0085 19.0306 -4.9811 0.3942 0.7371 0.5909
0.9930 18.0285 -4.9884 0.4530 0.7734 0.4110
1.0056 21.9592 1.0090 0.9078 0.2194 0.3647
0.9884 12.0573 -6.9910 0.1398 0.9005 0.3110
-0.0137 -15.9162 -6.0064 -0.8703 0.4060 -0.2505
0.0021 22.9721 0.0173 0.7964 0.2837 0.5688
0.0153 -11.0726 7.9843 0.0409 -0.9401 -0.4656

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16211
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.699
_diffrn_reflns_theta_min         3.566
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9971
_diffrn_measured_fraction_theta_max 0.9712
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     38.00  64.00   1.00    2.00    --   42.83 -57.00 -60.00   26
  2  ω     81.00 170.00   1.00    8.00    --  104.50  30.00-180.00   89
  3  ω    124.00 150.00   1.00    8.00    --  104.50  45.00 -90.00   26
  4  ω     74.00 157.00   1.00    8.00    --  104.50 125.00-180.00   83
  5  ω     74.00 138.00   1.00    8.00    --  104.50  77.00-120.00   64
  6  ω     57.00  91.00   1.00    8.00    --  104.50 -30.00 -60.00   34
  7  ω     36.00  88.00   1.00    8.00    --  104.50 -30.00  30.00   52
  8  ω     63.00  89.00   1.00    8.00    --  104.50 -30.00 120.00   26
  9  ω     30.00 109.00   1.00    8.00    --  104.50 -94.00-180.00   79
 10  ω    -85.00 -20.00   1.00    2.00    --  -38.50 125.00-180.00   65
 11  ω   -111.00 -85.00   1.00    2.00    --  -38.50 -19.00 150.00   26
 12  ω   -111.00  -8.00   1.00    2.00    --  -38.50 -77.00  90.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0937021000
_diffrn_orient_matrix_UB_12      0.0346178000
_diffrn_orient_matrix_UB_13      0.0529531000
_diffrn_orient_matrix_UB_21      0.0479434000
_diffrn_orient_matrix_UB_22      0.0124199000
_diffrn_orient_matrix_UB_23      -0.1006144000
_diffrn_orient_matrix_UB_31      -0.1550079000
_diffrn_orient_matrix_UB_32      0.0247939000
_diffrn_orient_matrix_UB_33      -0.0236351000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6945
_reflns_number_total             7564
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         1.171
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         7564
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0399
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0640P)²+1.9549P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1055
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18), C19(H19),
 C25(H25), C27(H27), C31(H31), C32(H32), C33(H33), C39(H39), C40(H40), C41(H41)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.59797(3) 0.25700(2) 0.51329(2) 0.01821(8) Uani 1 1 d . . . . .
Cl1 Cl 0.58539(18) 0.44688(3) 0.51936(8) 0.0444(3) Uani 1 1 d . . . . .
C1 C 0.5948(4) 0.31775(10) 0.5155(2) 0.0153(6) Uani 1 1 d . . . . .
C2 C 0.6191(4) 0.33762(10) 0.4292(2) 0.0177(7) Uani 1 1 d . . . . .
C3 C 0.6169(5) 0.37790(10) 0.4315(3) 0.0222(7) Uani 1 1 d . . . . .
H3 H 0.633884 0.392248 0.374206 0.027 Uiso 1 1 calc R U . . .
C4 C 0.5898(5) 0.39680(11) 0.5178(3) 0.0257(8) Uani 1 1 d . . . . .
C5 C 0.5639(5) 0.37674(10) 0.6029(3) 0.0225(7) Uani 1 1 d . . . . .
H5 H 0.543842 0.390292 0.660746 0.027 Uiso 1 1 calc R U . . .
C6 C 0.5676(4) 0.33636(10) 0.6028(2) 0.0170(6) Uani 1 1 d . . . . .
C7 C 0.6479(4) 0.31806(9) 0.3349(2) 0.0167(6) Uani 1 1 d . . . . .
C8 C 0.5147(5) 0.30526(10) 0.2637(3) 0.0193(7) Uani 1 1 d . . . . .
C9 C 0.5456(5) 0.28872(10) 0.1747(3) 0.0227(7) Uani 1 1 d . . . . .
H9 H 0.457176 0.279791 0.125974 0.027 Uiso 1 1 calc R U . . .
C10 C 0.7022(5) 0.28510(10) 0.1560(3) 0.0237(8) Uani 1 1 d . . . . .
H10 H 0.720929 0.274122 0.094489 0.028 Uiso 1 1 calc R U . . .
C11 C 0.8322(5) 0.29753(11) 0.2274(3) 0.0226(7) Uani 1 1 d . . . . .
H11 H 0.939948 0.294653 0.214746 0.027 Uiso 1 1 calc R U . . .
C12 C 0.8066(5) 0.31417(10) 0.3173(3) 0.0200(7) Uani 1 1 d . . . . .
C13 C 0.3427(5) 0.31012(12) 0.2808(3) 0.0272(8) Uani 1 1 d . . . . .
H13A H 0.330612 0.297846 0.344573 0.041 Uiso 1 1 calc R U . . .
H13B H 0.268006 0.298059 0.225356 0.041 Uiso 1 1 calc R U . . .
H13C H 0.317474 0.337609 0.283664 0.041 Uiso 1 1 calc R U . . .
C14 C 0.9502(5) 0.32719(13) 0.3939(3) 0.0299(8) Uani 1 1 d . . . . .
H14A H 1.050262 0.316178 0.377171 0.045 Uiso 1 1 calc R U . . .
H14B H 0.936587 0.318480 0.461077 0.045 Uiso 1 1 calc R U . . .
H14C H 0.957095 0.355353 0.393174 0.045 Uiso 1 1 calc R U . . .
C15 C 0.5419(4) 0.31587(10) 0.6964(2) 0.0170(7) Uani 1 1 d . . . . .
C16 C 0.6761(5) 0.30513(10) 0.7690(3) 0.0204(7) Uani 1 1 d . . . . .
C17 C 0.6472(5) 0.28775(11) 0.8577(3) 0.0237(7) Uani 1 1 d . . . . .
H17 H 0.736778 0.280348 0.907650 0.028 Uiso 1 1 calc R U . . .
C18 C 0.4911(5) 0.28115(11) 0.8740(3) 0.0249(8) Uani 1 1 d . . . . .
H18 H 0.473747 0.269421 0.934929 0.030 Uiso 1 1 calc R U . . .
C19 C 0.3594(5) 0.29162(11) 0.8015(3) 0.0226(7) Uani 1 1 d . . . . .
H19 H 0.252028 0.286851 0.812802 0.027 Uiso 1 1 calc R U . . .
C20 C 0.3831(5) 0.30912(10) 0.7119(3) 0.0196(7) Uani 1 1 d . . . . .
C21 C 0.8475(5) 0.31089(12) 0.7512(3) 0.0261(8) Uani 1 1 d . . . . .
H21A H 0.865871 0.294897 0.694309 0.039 Uiso 1 1 calc R U . . .
H21B H 0.924209 0.303477 0.811737 0.039 Uiso 1 1 calc R U . . .
H21C H 0.863839 0.338038 0.735820 0.039 Uiso 1 1 calc R U . . .
C22 C 0.2399(5) 0.31918(13) 0.6318(3) 0.0294(8) Uani 1 1 d . . . . .
H22A H 0.240745 0.346877 0.617934 0.044 Uiso 1 1 calc R U . . .
H22B H 0.138882 0.312391 0.655309 0.044 Uiso 1 1 calc R U . . .
H22C H 0.246763 0.304837 0.570081 0.044 Uiso 1 1 calc R U . . .
I2 I 0.75724(3) 0.51556(2) 0.03152(2) 0.02651(9) Uani 1 1 d . . . . .
Cl2 Cl 0.9348(2) 0.56857(3) 0.50728(8) 0.0526(4) Uani 1 1 d . . . . .
C23 C 0.8133(5) 0.53244(10) 0.1835(2) 0.0199(7) Uani 1 1 d . . . . .
C24 C 0.8726(5) 0.56965(10) 0.2063(3) 0.0200(7) Uani 1 1 d . . . . .
C25 C 0.9109(5) 0.58035(11) 0.3074(3) 0.0272(8) Uani 1 1 d . . . . .
H25 H 0.952353 0.605352 0.325165 0.033 Uiso 1 1 calc R U . . .
C26 C 0.8882(6) 0.55437(12) 0.3819(3) 0.0317(9) Uani 1 1 d . . . . .
C27 C 0.8289(6) 0.51770(11) 0.3586(3) 0.0265(8) Uani 1 1 d . . . . .
H27 H 0.814190 0.500426 0.410958 0.032 Uiso 1 1 calc R U . . .
C28 C 0.7908(5) 0.50613(10) 0.2583(3) 0.0213(7) Uani 1 1 d . . . . .
C29 C 0.8975(5) 0.59814(9) 0.1264(3) 0.0191(7) Uani 1 1 d . . . . .
C30 C 0.7647(5) 0.62021(10) 0.0787(3) 0.0223(7) Uani 1 1 d . . . . .
C31 C 0.7931(6) 0.64677(11) 0.0057(3) 0.0281(8) Uani 1 1 d . . . . .
H31 H 0.705710 0.662101 -0.027510 0.034 Uiso 1 1 calc R U . . .
C32 C 0.9454(6) 0.65114(11) -0.0191(3) 0.0317(9) Uani 1 1 d . . . . .
H32 H 0.962131 0.669375 -0.068844 0.038 Uiso 1 1 calc R U . . .
C33 C 1.0749(5) 0.62880(12) 0.0288(3) 0.0286(8) Uani 1 1 d . . . . .
H33 H 1.179601 0.631849 0.011317 0.034 Uiso 1 1 calc R U . . .
C34 C 1.0522(5) 0.60217(11) 0.1017(3) 0.0242(8) Uani 1 1 d . . . . .
C35 C 0.5977(5) 0.61466(12) 0.1030(3) 0.0280(8) Uani 1 1 d . . . . .
H35A H 0.527492 0.635994 0.074569 0.042 Uiso 1 1 calc R U . . .
H35B H 0.604101 0.614059 0.176255 0.042 Uiso 1 1 calc R U . . .
H35C H 0.552299 0.590305 0.073919 0.042 Uiso 1 1 calc R U . . .
C36 C 1.1908(5) 0.57704(14) 0.1503(3) 0.0339(9) Uani 1 1 d . . . . .
H36A H 1.283816 0.580612 0.115823 0.051 Uiso 1 1 calc R U . . .
H36B H 1.156659 0.550006 0.145228 0.051 Uiso 1 1 calc R U . . .
H36C H 1.222100 0.584136 0.221397 0.051 Uiso 1 1 calc R U . . .
C37 C 0.7260(5) 0.46671(10) 0.2315(3) 0.0215(7) Uani 1 1 d . . . . .
C38 C 0.8334(5) 0.43700(11) 0.2150(3) 0.0260(8) Uani 1 1 d . . . . .
C39 C 0.7666(7) 0.40122(11) 0.1843(3) 0.0337(10) Uani 1 1 d . . . . .
H39 H 0.836785 0.380560 0.174596 0.040 Uiso 1 1 calc R U . . .
C40 C 0.6021(7) 0.39525(11) 0.1678(3) 0.0368(11) Uani 1 1 d . . . . .
H40 H 0.559436 0.370879 0.144520 0.044 Uiso 1 1 calc R U . . .
C41 C 0.4972(6) 0.42446(12) 0.1849(3) 0.0332(10) Uani 1 1 d . . . . .
H41 H 0.383239 0.419984 0.174008 0.040 Uiso 1 1 calc R U . . .
C42 C 0.5592(5) 0.46062(11) 0.2184(3) 0.0248(8) Uani 1 1 d . . . . .
C43 C 1.0137(6) 0.44378(14) 0.2258(4) 0.0371(10) Uani 1 1 d . . . . .
H43A H 1.037437 0.456109 0.164541 0.056 Uiso 1 1 calc R U . . .
H43B H 1.071149 0.419095 0.235873 0.056 Uiso 1 1 calc R U . . .
H43C H 1.049934 0.460542 0.283846 0.056 Uiso 1 1 calc R U . . .
C44 C 0.4458(6) 0.49239(13) 0.2363(4) 0.0352(9) Uani 1 1 d . . . . .
H44A H 0.468480 0.499861 0.307513 0.053 Uiso 1 1 calc R U . . .
H44B H 0.333147 0.483424 0.218758 0.053 Uiso 1 1 calc R U . . .
H44C H 0.461841 0.514640 0.194390 0.053 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C1 2.110(3) . ?
Cl1 C4 1.740(4) . ?
C1 C2 1.396(5) . ?
C1 C6 1.396(5) . ?
C2 C3 1.400(5) . ?
C2 C7 1.497(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(5) . ?
C4 C5 1.391(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.403(5) . ?
C6 C15 1.495(5) . ?
C7 C8 1.408(5) . ?
C7 C12 1.394(5) . ?
C8 C9 1.395(5) . ?
C8 C13 1.503(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.380(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.387(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.392(5) . ?
C12 C14 1.508(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.404(5) . ?
C15 C20 1.398(5) . ?
C16 C17 1.396(5) . ?
C16 C21 1.505(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.379(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.386(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.396(5) . ?
C20 C22 1.505(5) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
I2 C23 2.103(3) . ?
Cl2 C26 1.738(4) . ?
C23 C24 1.399(5) . ?
C23 C28 1.398(5) . ?
C24 C25 1.394(5) . ?
C24 C29 1.504(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.387(6) . ?
C26 C27 1.383(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.393(5) . ?
C28 C37 1.493(5) . ?
C29 C30 1.408(5) . ?
C29 C34 1.396(6) . ?
C30 C31 1.399(5) . ?
C30 C35 1.499(6) . ?
C31 H31 0.9500 . ?
C31 C32 1.378(7) . ?
C32 H32 0.9500 . ?
C32 C33 1.394(7) . ?
C33 H33 0.9500 . ?
C33 C34 1.386(6) . ?
C34 C36 1.505(6) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.410(5) . ?
C37 C42 1.389(6) . ?
C38 C39 1.395(6) . ?
C38 C43 1.505(7) . ?
C39 H39 0.9500 . ?
C39 C40 1.369(8) . ?
C40 H40 0.9500 . ?
C40 C41 1.385(7) . ?
C41 H41 0.9500 . ?
C41 C42 1.402(6) . ?
C42 C44 1.500(6) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 I1 118.6(2) . . ?
C6 C1 I1 118.6(2) . . ?
C6 C1 C2 122.8(3) . . ?
C1 C2 C3 118.1(3) . . ?
C1 C2 C7 123.4(3) . . ?
C3 C2 C7 118.5(3) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.7(3) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 Cl1 119.3(3) . . ?
C3 C4 C5 121.7(3) . . ?
C5 C4 Cl1 119.0(3) . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.6(3) . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C5 118.1(3) . . ?
C1 C6 C15 124.0(3) . . ?
C5 C6 C15 117.9(3) . . ?
C8 C7 C2 119.8(3) . . ?
C12 C7 C2 119.2(3) . . ?
C12 C7 C8 121.0(3) . . ?
C7 C8 C13 121.5(3) . . ?
C9 C8 C7 118.3(3) . . ?
C9 C8 C13 120.2(3) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 C8 121.2(3) . . ?
C10 C9 H9 119.4 . . ?
C9 C10 H10 120.1 . . ?
C9 C10 C11 119.8(3) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 119.6 . . ?
C10 C11 C12 120.8(4) . . ?
C12 C11 H11 119.6 . . ?
C7 C12 C14 121.3(3) . . ?
C11 C12 C7 118.9(3) . . ?
C11 C12 C14 119.7(4) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C6 120.0(3) . . ?
C20 C15 C6 119.0(3) . . ?
C20 C15 C16 120.9(3) . . ?
C15 C16 C21 121.2(3) . . ?
C17 C16 C15 118.4(3) . . ?
C17 C16 C21 120.4(3) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 C16 121.2(4) . . ?
C18 C17 H17 119.4 . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.0(3) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 119.7 . . ?
C18 C19 C20 120.6(4) . . ?
C20 C19 H19 119.7 . . ?
C15 C20 C22 120.6(3) . . ?
C19 C20 C15 118.9(3) . . ?
C19 C20 C22 120.4(3) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 I2 118.8(3) . . ?
C28 C23 I2 119.0(3) . . ?
C28 C23 C24 122.1(3) . . ?
C23 C24 C29 122.5(3) . . ?
C25 C24 C23 118.2(3) . . ?
C25 C24 C29 119.2(3) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 C24 119.8(3) . . ?
C26 C25 H25 120.1 . . ?
C25 C26 Cl2 118.9(3) . . ?
C27 C26 Cl2 119.5(3) . . ?
C27 C26 C25 121.6(4) . . ?
C26 C27 H27 120.1 . . ?
C26 C27 C28 119.9(3) . . ?
C28 C27 H27 120.1 . . ?
C23 C28 C37 120.9(3) . . ?
C27 C28 C23 118.4(3) . . ?
C27 C28 C37 120.8(3) . . ?
C30 C29 C24 119.2(3) . . ?
C34 C29 C24 119.1(3) . . ?
C34 C29 C30 121.6(3) . . ?
C29 C30 C35 121.3(3) . . ?
C31 C30 C29 117.6(4) . . ?
C31 C30 C35 121.1(4) . . ?
C30 C31 H31 119.3 . . ?
C32 C31 C30 121.4(4) . . ?
C32 C31 H31 119.3 . . ?
C31 C32 H32 120.0 . . ?
C31 C32 C33 120.0(4) . . ?
C33 C32 H32 120.0 . . ?
C32 C33 H33 119.7 . . ?
C34 C33 C32 120.5(4) . . ?
C34 C33 H33 119.7 . . ?
C29 C34 C36 120.7(4) . . ?
C33 C34 C29 118.9(4) . . ?
C33 C34 C36 120.3(4) . . ?
C30 C35 H35A 109.5 . . ?
C30 C35 H35B 109.5 . . ?
C30 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 C28 119.7(4) . . ?
C42 C37 C28 118.9(3) . . ?
C42 C37 C38 121.3(3) . . ?
C37 C38 C43 121.6(4) . . ?
C39 C38 C37 117.8(4) . . ?
C39 C38 C43 120.6(4) . . ?
C38 C39 H39 119.3 . . ?
C40 C39 C38 121.4(4) . . ?
C40 C39 H39 119.3 . . ?
C39 C40 H40 119.7 . . ?
C39 C40 C41 120.5(4) . . ?
C41 C40 H40 119.7 . . ?
C40 C41 H41 120.0 . . ?
C40 C41 C42 120.1(4) . . ?
C42 C41 H41 120.0 . . ?
C37 C42 C41 118.8(4) . . ?
C37 C42 C44 120.9(4) . . ?
C41 C42 C44 120.2(4) . . ?
C38 C43 H43A 109.5 . . ?
C38 C43 H43B 109.5 . . ?
C38 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
I1 C1 C2 C3 -180.0(3) . . . . ?
I1 C1 C2 C7 -0.2(5) . . . . ?
I1 C1 C6 C5 -179.3(3) . . . . ?
I1 C1 C6 C15 0.7(5) . . . . ?
Cl1 C4 C5 C6 -179.8(3) . . . . ?
C1 C2 C3 C4 -0.5(6) . . . . ?
C1 C2 C7 C8 84.1(4) . . . . ?
C1 C2 C7 C12 -98.4(4) . . . . ?
C1 C6 C15 C16 86.6(4) . . . . ?
C1 C6 C15 C20 -96.0(4) . . . . ?
C2 C1 C6 C5 0.3(5) . . . . ?
C2 C1 C6 C15 -179.7(3) . . . . ?
C2 C3 C4 Cl1 -179.4(3) . . . . ?
C2 C3 C4 C5 -0.2(6) . . . . ?
C2 C7 C8 C9 177.2(3) . . . . ?
C2 C7 C8 C13 -1.1(5) . . . . ?
C2 C7 C12 C11 -177.1(3) . . . . ?
C2 C7 C12 C14 3.6(5) . . . . ?
C3 C2 C7 C8 -96.2(4) . . . . ?
C3 C2 C7 C12 81.4(4) . . . . ?
C3 C4 C5 C6 1.0(6) . . . . ?
C4 C5 C6 C1 -1.0(6) . . . . ?
C4 C5 C6 C15 179.0(4) . . . . ?
C5 C6 C15 C16 -93.4(4) . . . . ?
C5 C6 C15 C20 83.9(4) . . . . ?
C6 C1 C2 C3 0.4(5) . . . . ?
C6 C1 C2 C7 -179.8(3) . . . . ?
C6 C15 C16 C17 176.9(3) . . . . ?
C6 C15 C16 C21 -5.1(5) . . . . ?
C6 C15 C20 C19 -177.0(3) . . . . ?
C6 C15 C20 C22 5.2(5) . . . . ?
C7 C2 C3 C4 179.7(4) . . . . ?
C7 C8 C9 C10 -0.4(5) . . . . ?
C8 C7 C12 C11 0.4(5) . . . . ?
C8 C7 C12 C14 -178.9(3) . . . . ?
C8 C9 C10 C11 1.0(6) . . . . ?
C9 C10 C11 C12 -0.9(5) . . . . ?
C10 C11 C12 C7 0.3(5) . . . . ?
C10 C11 C12 C14 179.6(3) . . . . ?
C12 C7 C8 C9 -0.3(5) . . . . ?
C12 C7 C8 C13 -178.6(3) . . . . ?
C13 C8 C9 C10 177.9(3) . . . . ?
C15 C16 C17 C18 0.1(5) . . . . ?
C16 C15 C20 C19 0.4(5) . . . . ?
C16 C15 C20 C22 -177.4(3) . . . . ?
C16 C17 C18 C19 0.4(6) . . . . ?
C17 C18 C19 C20 -0.4(6) . . . . ?
C18 C19 C20 C15 0.1(5) . . . . ?
C18 C19 C20 C22 177.9(4) . . . . ?
C20 C15 C16 C17 -0.4(5) . . . . ?
C20 C15 C16 C21 177.6(3) . . . . ?
C21 C16 C17 C18 -178.0(4) . . . . ?
I2 C23 C24 C25 -179.3(3) . . . . ?
I2 C23 C24 C29 0.2(5) . . . . ?
I2 C23 C28 C27 179.8(3) . . . . ?
I2 C23 C28 C37 -0.8(5) . . . . ?
Cl2 C26 C27 C28 179.8(4) . . . . ?
C23 C24 C25 C26 -0.6(6) . . . . ?
C23 C24 C29 C30 83.7(5) . . . . ?
C23 C24 C29 C34 -96.7(4) . . . . ?
C23 C28 C37 C38 85.5(5) . . . . ?
C23 C28 C37 C42 -91.3(5) . . . . ?
C24 C23 C28 C27 0.1(6) . . . . ?
C24 C23 C28 C37 179.5(4) . . . . ?
C24 C25 C26 Cl2 -179.3(3) . . . . ?
C24 C25 C26 C27 0.3(7) . . . . ?
C24 C29 C30 C31 179.2(3) . . . . ?
C24 C29 C30 C35 -2.6(5) . . . . ?
C24 C29 C34 C33 -179.2(3) . . . . ?
C24 C29 C34 C36 3.1(5) . . . . ?
C25 C24 C29 C30 -96.8(4) . . . . ?
C25 C24 C29 C34 82.9(5) . . . . ?
C25 C26 C27 C28 0.1(7) . . . . ?
C26 C27 C28 C23 -0.4(7) . . . . ?
C26 C27 C28 C37 -179.8(4) . . . . ?
C27 C28 C37 C38 -95.1(5) . . . . ?
C27 C28 C37 C42 88.0(5) . . . . ?
C28 C23 C24 C25 0.3(6) . . . . ?
C28 C23 C24 C29 179.9(4) . . . . ?
C28 C37 C38 C39 -176.3(3) . . . . ?
C28 C37 C38 C43 1.1(5) . . . . ?
C28 C37 C42 C41 174.7(3) . . . . ?
C28 C37 C42 C44 -3.4(5) . . . . ?
C29 C24 C25 C26 179.9(4) . . . . ?
C29 C30 C31 C32 0.2(6) . . . . ?
C30 C29 C34 C33 0.4(5) . . . . ?
C30 C29 C34 C36 -177.3(3) . . . . ?
C30 C31 C32 C33 0.1(6) . . . . ?
C31 C32 C33 C34 -0.2(6) . . . . ?
C32 C33 C34 C29 -0.1(6) . . . . ?
C32 C33 C34 C36 177.6(4) . . . . ?
C34 C29 C30 C31 -0.5(5) . . . . ?
C34 C29 C30 C35 177.7(3) . . . . ?
C35 C30 C31 C32 -178.0(4) . . . . ?
C37 C38 C39 C40 1.8(5) . . . . ?
C38 C37 C42 C41 -2.1(5) . . . . ?
C38 C37 C42 C44 179.8(3) . . . . ?
C38 C39 C40 C41 -2.3(6) . . . . ?
C39 C40 C41 C42 0.7(6) . . . . ?
C40 C41 C42 C37 1.5(6) . . . . ?
C40 C41 C42 C44 179.6(4) . . . . ?
C42 C37 C38 C39 0.5(5) . . . . ?
C42 C37 C38 C43 177.9(4) . . . . ?
C43 C38 C39 C40 -175.7(4) . . . . ?

_olex2_date_sample_data_collection 2016-11-09
_olex2_date_sample_submission    2016-11-07
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_original_sample_id KEWJMA
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.083
_oxdiff_exptl_absorpt_empirical_full_min 0.552
####################################################################### 
# 
# 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_liajvf
_database_code_depnum_ccdc_archive 'CCDC 2045221'
loop_
_audit_author_name
_audit_author_address
'Stephen P. Argent'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2020-11-18 deposited with the CCDC.	2020-12-04 downloaded from the CCDC.
;
_nottingham_internal_coll_name   LIAJVF
_nottingham_internal_coll_number 16599
_nottingham_internal_coll_client AJV/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 10.00, 40.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   24/10/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 28/10/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 30/11/16
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 30/11/16
_nottingham_internal_refinement_user pcxav1/pczspa
_nottingham_internal_self_archive_date 30/11/16
_nottingham_internal_self_validation_date 30/11/16
_nottingham_internal_self_validation_user pcxav1
_nottingham_internal_validation_date 08/06/2020
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date ?
_refine_special_details          
;
 Three-fold conformational disorder is modelled for the fluorine
 atoms of the CF3 group. The occupancies of the three sets of
 three fluorine atoms were refined and constrained to sum to
 unit using a linear restraint (SUMP), resulting in values
 of 0.71(1), 0.05(1) and 0.22(1) for the three components.
 The carbon atoms of the three disorder components were
 constrained to have identical coordinates and anisotropic
 displacement parameters (EXYZ, EADP). The three sets of
 fluorine atoms were restrained to have similar bonds and
 angles to each other (SAME). The set of three fluorine
 atoms with the lowest occupancy (0.05) were refined with
 isotropic displacement parameters. Rigid bond and similarity
 restraints (SIMU, RIGU) were applied to all of the atoms
 in the disordered mopieties.
;
_audit_creation_date             2020-07-02
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C45.985 H40 F5.955 Li2'
_chemical_formula_sum            'C46 H40 F6 Li2'
_chemical_formula_weight         720.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C23 H20 F3 Li1'
_chemical_oxdiff_usercomment     
'LIAJVF #16599 SN-1067 IN FOMBLIN FILM ON MICROMOUNT FOR AJV/DLK'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 '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'

_cell_length_a                   16.2343(6)
_cell_length_b                   16.3983(5)
_cell_length_c                   15.5748(5)
_cell_angle_alpha                90
_cell_angle_beta                 115.087(4)
_cell_angle_gamma                90
_cell_volume                     3755.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10684
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.4220
_cell_measurement_theta_min      4.0640
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1504
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
8 5 -8 0.0403
-8 -5 8 0.0476
5 -9 -5 0.0364
6 -8 -5 0.0482
-4 9 5 0.0574
5 2 6 0.2316
-9 -5 1 0.1732
8 -4 -8 0.0351
-2 8 -5 0.1736
-1 4 -8 0.1954
1 11 0 0.0610
2 10 -3 0.0666
7 -6 -8 0.0293
-4 -9 6 0.0649
-4 10 3 0.0820
-6 8 6 0.0669

_exptl_crystal_recrystallization_method 'Recrystallised from hexane at -30'
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.088
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
7.9885 4.9926 -7.9909 0.1650 0.4472 0.9141
-7.9885 -4.9926 7.9909 -0.1650 -0.4472 -0.9141
4.9956 -8.9913 -4.9927 0.9831 -0.2596 0.0921
5.9941 -7.9926 -4.9925 0.9171 -0.2783 0.2148
-3.9970 8.9911 4.9931 -0.9766 0.1964 -0.0090
4.9927 1.9973 5.9963 -0.4688 -0.7748 0.4567
-8.9869 -4.9928 0.9966 0.2444 0.2551 -0.9527
7.9906 -3.9975 -7.9897 0.8182 0.0471 0.5584
-1.9990 7.9913 -4.9974 -0.2967 0.9385 0.1817
-0.9993 3.9953 -7.9939 0.1785 0.9714 0.1259
0.9961 10.9877 -0.0011 -0.7918 0.4258 0.5179
1.9951 9.9885 -2.9980 -0.5344 0.5921 0.5807
6.9924 -5.9951 -7.9898 0.9568 0.0213 0.3962
-3.9928 -8.9890 5.9945 0.2704 -0.6952 -0.7267
-3.9971 9.9899 2.9947 -0.9303 0.4234 0.0433
-5.9941 7.9927 5.9916 -0.9765 0.1870 -0.2212

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21864
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.536
_diffrn_reflns_theta_min         4.038
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
'List of Runs (angles in degrees, time in seconds): # Type Start End Width tₑₓₚ ω θ κ φ Frames -------------------------------------------------------------------------- 1 ω -125.00 48.00 1.00 10.00 -- -38.50 0.00 30.00 173 2 ω 23.00 98.00 1.00 10.00 -- 43.38-125.00 30.00 75 3 ω 35.00 98.00 1.00 40.00 -- 106.13 -45.00 120.00 63 4 ω 25.00 109.00 1.00 40.00 -- 106.13 -95.00 -30.00 84 5 ω 31.00 91.00 1.00 40.00 -- 106.13 -30.00 60.00 60 6 ω 35.00 98.00 1.00 40.00 -- 106.13 -45.00 -30.00 63 7 ω 61.00 178.00 1.00 40.00 -- 106.13 15.00 30.00 117 8 ω 94.00 178.00 1.00 40.00 -- 106.13 125.00 30.00 84 9 ω 31.00 91.00 1.00 40.00 -- 106.13 -30.00-120.00 60 10 ω 35.00 121.00 1.00 40.00 -- 106.13-125.00 120.00 86 11 ω 12.00 117.00 1.00 10.00 -- 43.38 77.00 0.00 105 12 ω 12.00 117.00 1.00 10.00 -- 43.38 77.00-180.00 105 13 ω 12.00 117.00 1.00 10.00 -- 43.38 77.00 -90.00 105 14 ω 75.00 178.00 1.00 40.00 -- 106.13 77.00 -90.00 103 15 ω 79.00 176.00 1.00 40.00 -- 106.13 61.00 120.00 97 16 ω 79.00 176.00 1.00 40.00 -- 106.13 61.00 60.00 97 17 ω 79.00 176.00 1.00 40.00 -- 106.13 61.00-120.00 97 18 ω 75.00 178.00 1.00 40.00 -- 106.13 77.00 0.00 103 19 ω 61.00 178.00 1.00 40.00 -- 106.13 15.00-120.00 117'
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0065825000
_diffrn_orient_matrix_UB_12      -0.0726642000
_diffrn_orient_matrix_UB_13      -0.0594672000
_diffrn_orient_matrix_UB_21      -0.0632344000
_diffrn_orient_matrix_UB_22      0.0444794000
_diffrn_orient_matrix_UB_23      -0.0913857000
_diffrn_orient_matrix_UB_31      0.0833063000
_diffrn_orient_matrix_UB_32      0.0395835000
_diffrn_orient_matrix_UB_33      -0.0063849000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3440
_reflns_number_total             3818
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3818
_refine_ls_number_restraints     274
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0369
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0488P)²+1.8878P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0979
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C23A, C23B, C23C}
3. Uiso/Uaniso restraints and constraints
F1B \\sim F2B \\sim F3B \\sim F1A \\sim F2A \\sim F3A \\sim F1C \\sim F3C \\sim
F2C: within 2.5A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2.5A
Uanis(C23A) = Uanis(C23B) = Uanis(C23C)
4. Rigid body (RIGU) restrains
 F1B, F2B, F3B, F1A, F2A, F3A, F1C, F3C, F2C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C23B, F2B, F3B, F1B} sigma for 1-2: 0.02, 1-3: 0.04
{C23B, F1B, F3B, F2B} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C23B, F1B, F2B, F3B}
{C23B, F1B, F2B, F3B} sigma for 1-2: 0.02, 1-3: 0.04
{C23B, F2B, F3B, F1B} sigma for 1-2: 0.02, 1-3: 0.04
{C23B, F1B, F3B, F2B} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C23A, F1A, F2A, F3A}
{C23B, F1B, F2B, F3B} sigma for 1-2: 0.02, 1-3: 0.04
{C23B, F2B, F3B, F1B} sigma for 1-2: 0.02, 1-3: 0.04
{C23B, F1B, F3B, F2B} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C23C, F1C, F3C, F2C}
6. Others
 1*[Sof(C23B)+Sof(F1B)+Sof(F2B)+Sof(F3B)]+1*[Sof(C23A)+Sof(F1A)+Sof(F2A)+
 Sof(F3A)]+1*[Sof(C23C)+Sof(F1C)+Sof(F3C)+Sof(F2C)]=1 with esd of 0.002
 Sof(C23B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=FVAR(1)
 Sof(C23A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(2)
 Sof(C23C)=Sof(F1C)=Sof(F3C)=Sof(F2C)=FVAR(3)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18), C19(H19)
7.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.40179(6) 0.31740(6) 0.28085(7) 0.0221(2) Uani 1 1 d . . . . .
C2 C 0.38334(7) 0.26052(6) 0.33877(7) 0.0220(2) Uani 1 1 d . . . . .
C3 C 0.30736(7) 0.26535(6) 0.35855(7) 0.0243(2) Uani 1 1 d . . . . .
H3 H 0.297474 0.225238 0.397191 0.029 Uiso 1 1 calc R U . . .
C4 C 0.24633(7) 0.32910(6) 0.32143(7) 0.0243(2) Uani 1 1 d . . . . .
C5 C 0.26091(7) 0.38728(6) 0.26462(7) 0.0237(2) Uani 1 1 d . . . . .
H5 H 0.219520 0.431288 0.239461 0.028 Uiso 1 1 calc R U . . .
C6 C 0.33680(7) 0.38072(6) 0.24466(7) 0.0220(2) Uani 1 1 d . . . . .
C7 C 0.44541(7) 0.18855(6) 0.37774(7) 0.0231(2) Uani 1 1 d . . . . .
C8 C 0.51544(7) 0.19003(7) 0.47009(8) 0.0286(2) Uani 1 1 d . . . . .
C9 C 0.57034(8) 0.12150(8) 0.50378(8) 0.0360(3) Uani 1 1 d . . . . .
H9 H 0.618148 0.122241 0.565933 0.043 Uiso 1 1 calc R U . . .
C10 C 0.55676(9) 0.05254(8) 0.44877(9) 0.0383(3) Uani 1 1 d . . . . .
H10 H 0.595109 0.006421 0.472966 0.046 Uiso 1 1 calc R U . . .
C11 C 0.48721(8) 0.05066(7) 0.35830(9) 0.0365(3) Uani 1 1 d . . . . .
H11 H 0.477569 0.002845 0.320824 0.044 Uiso 1 1 calc R U . . .
C12 C 0.43106(7) 0.11830(7) 0.32153(8) 0.0292(2) Uani 1 1 d . . . . .
C13 C 0.52921(9) 0.26324(8) 0.53315(8) 0.0384(3) Uani 1 1 d . . . . .
H13A H 0.525540 0.313062 0.496950 0.058 Uiso 1 1 calc R U . . .
H13B H 0.589137 0.259998 0.586960 0.058 Uiso 1 1 calc R U . . .
H13C H 0.481896 0.264286 0.556548 0.058 Uiso 1 1 calc R U . . .
C14 C 0.35379(9) 0.11500(8) 0.22331(10) 0.0424(3) Uani 1 1 d . . . . .
H14A H 0.296985 0.130902 0.226550 0.064 Uiso 1 1 calc R U . . .
H14B H 0.347969 0.059386 0.198371 0.064 Uiso 1 1 calc R U . . .
H14C H 0.366369 0.152572 0.181405 0.064 Uiso 1 1 calc R U . . .
C15 C 0.34790(7) 0.44427(7) 0.18078(7) 0.0261(2) Uani 1 1 d . . . . .
C16 C 0.33130(8) 0.42359(9) 0.08710(8) 0.0370(3) Uani 1 1 d . . . . .
C17 C 0.33814(10) 0.48438(12) 0.02804(10) 0.0596(5) Uani 1 1 d . . . . .
H17 H 0.326215 0.471210 -0.035553 0.072 Uiso 1 1 calc R U . . .
C18 C 0.36166(11) 0.56273(12) 0.05945(13) 0.0686(5) Uani 1 1 d . . . . .
H18 H 0.365193 0.603272 0.017572 0.082 Uiso 1 1 calc R U . . .
C19 C 0.38012(10) 0.58264(9) 0.15148(13) 0.0566(4) Uani 1 1 d . . . . .
H19 H 0.397658 0.636810 0.173153 0.068 Uiso 1 1 calc R U . . .
C20 C 0.37345(8) 0.52426(7) 0.21376(9) 0.0361(3) Uani 1 1 d . . . . .
C21 C 0.30386(10) 0.33889(10) 0.04949(9) 0.0472(3) Uani 1 1 d . . . . .
H21A H 0.357084 0.302961 0.075061 0.071 Uiso 1 1 calc R U . . .
H21B H 0.279221 0.339666 -0.019862 0.071 Uiso 1 1 calc R U . . .
H21C H 0.257360 0.318698 0.068684 0.071 Uiso 1 1 calc R U . . .
C22 C 0.39330(10) 0.54755(8) 0.31404(12) 0.0497(4) Uani 1 1 d . . . . .
H22A H 0.336301 0.549712 0.321393 0.075 Uiso 1 1 calc R U . . .
H22B H 0.422663 0.601182 0.328343 0.075 Uiso 1 1 calc R U . . .
H22C H 0.433861 0.506923 0.357723 0.075 Uiso 1 1 calc R U . . .
Li1 Li 0.500000 0.24496(16) 0.250000 0.0325(6) Uani 1 2 d S T P . .
Li2 Li 0.500000 0.38720(16) 0.250000 0.0314(6) Uani 1 2 d S T P . .
C23B C 0.16251(8) 0.33340(7) 0.33820(8) 0.0317(3) Uani 0.717(12) 1 d D . P A 1
F1B F 0.09355(17) 0.2913(3) 0.2712(2) 0.0533(8) Uani 0.717(12) 1 d D U P A 1
F2B F 0.1324(3) 0.4081(2) 0.3391(4) 0.0526(9) Uani 0.717(12) 1 d D U P A 1
F3B F 0.1734(3) 0.2977(3) 0.4197(2) 0.0490(10) Uani 0.717(12) 1 d D U P A 1
C23A C 0.16251(8) 0.33340(7) 0.33820(8) 0.0317(3) Uani 0.052(2) 1 d D . P A 2
F1A F 0.1133(13) 0.2668(9) 0.3236(18) 0.057(4) Uiso 0.052(2) 1 d D U P A 2
F2A F 0.1010(13) 0.3899(12) 0.2849(14) 0.050(4) Uiso 0.052(2) 1 d D U P A 2
F3A F 0.1808(13) 0.3546(16) 0.4293(9) 0.062(4) Uiso 0.052(2) 1 d D U P A 2
C23C C 0.16251(8) 0.33340(7) 0.33820(8) 0.0317(3) Uani 0.224(12) 1 d D . P A 3
F1C F 0.0869(4) 0.3288(11) 0.2580(6) 0.057(2) Uani 0.224(12) 1 d D U P A 3
F3C F 0.1578(9) 0.2847(7) 0.4011(9) 0.045(2) Uani 0.224(12) 1 d D U P A 3
F2C F 0.1570(9) 0.4086(6) 0.3715(10) 0.0475(18) Uani 0.224(12) 1 d D U P A 3


_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 1.4152(14) . ?
C1 C6 1.4160(14) . ?
C1 Li1 2.1985(17) 2_655 ?
C1 Li1 2.1985(17) . ?
C1 Li2 2.1754(17) . ?
C1 Li2 2.1754(17) 2_655 ?
C2 C3 1.3946(14) . ?
C2 C7 1.5025(14) . ?
C3 H3 0.9500 . ?
C3 C4 1.3867(14) . ?
C4 C5 1.3882(15) . ?
C4 C23B 1.4920(14) . ?
C4 C23A 1.4920(14) . ?
C4 C23C 1.4920(14) . ?
C5 H5 0.9500 . ?
C5 C6 1.3967(14) . ?
C6 C15 1.5035(14) . ?
C7 C8 1.4055(15) . ?
C7 C12 1.4053(15) . ?
C7 Li1 2.6635(13) 2_655 ?
C7 Li1 2.6635(13) . ?
C8 C9 1.3913(16) . ?
C8 C13 1.5065(16) . ?
C9 H9 0.9500 . ?
C9 C10 1.3789(19) . ?
C10 H10 0.9500 . ?
C10 C11 1.3827(18) . ?
C11 H11 0.9500 . ?
C11 C12 1.3953(16) . ?
C12 C14 1.5130(16) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.4081(16) . ?
C15 C20 1.4055(16) . ?
C15 Li2 2.4245(14) 2_655 ?
C15 Li2 2.4245(14) . ?
C16 C17 1.3923(19) . ?
C16 C21 1.500(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.370(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.374(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.3994(19) . ?
C20 C22 1.504(2) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
Li1 Li1 0.000000(3) 2_655 ?
Li2 Li2 0.000(5) 2_655 ?
C23B F1B 1.352(2) . ?
C23B F2B 1.321(3) . ?
C23B F3B 1.339(3) . ?
C23A F1A 1.315(12) . ?
C23A F2A 1.357(12) . ?
C23A F3A 1.365(12) . ?
C23C F1C 1.331(7) . ?
C23C F3C 1.291(10) . ?
C23C F2C 1.355(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 114.43(9) . . ?
C2 C1 Li1 98.76(8) . 2_655 ?
C2 C1 Li1 98.76(8) . . ?
C2 C1 Li2 149.39(8) . 2_655 ?
C2 C1 Li2 149.39(8) . . ?
C6 C1 Li1 142.78(8) . . ?
C6 C1 Li1 142.78(8) . 2_655 ?
C6 C1 Li2 91.06(8) . 2_655 ?
C6 C1 Li2 91.06(8) . . ?
Li1 C1 Li1 0.00(12) 2_655 . ?
Li2 C1 Li1 64.45(9) 2_655 . ?
Li2 C1 Li1 64.45(9) 2_655 2_655 ?
Li2 C1 Li1 64.45(9) . 2_655 ?
Li2 C1 Li1 64.45(9) . . ?
Li2 C1 Li2 0.00(12) 2_655 . ?
C1 C2 C7 119.22(9) . . ?
C3 C2 C1 123.33(9) . . ?
C3 C2 C7 117.38(9) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.56(9) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 C5 119.94(9) . . ?
C3 C4 C23B 120.41(9) . . ?
C3 C4 C23A 120.41(9) . . ?
C3 C4 C23C 120.41(9) . . ?
C5 C4 C23B 119.58(9) . . ?
C5 C4 C23A 119.58(9) . . ?
C5 C4 C23C 119.58(9) . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.59(9) . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C15 119.57(9) . . ?
C5 C6 C1 123.14(9) . . ?
C5 C6 C15 117.28(9) . . ?
C2 C7 Li1 78.70(7) . . ?
C2 C7 Li1 78.70(7) . 2_655 ?
C8 C7 C2 120.85(9) . . ?
C8 C7 Li1 112.18(7) . . ?
C8 C7 Li1 112.18(7) . 2_655 ?
C12 C7 C2 119.12(9) . . ?
C12 C7 C8 120.01(10) . . ?
C12 C7 Li1 80.74(8) . . ?
C12 C7 Li1 80.74(8) . 2_655 ?
Li1 C7 Li1 0.0 2_655 . ?
C7 C8 C13 120.85(10) . . ?
C9 C8 C7 118.88(11) . . ?
C9 C8 C13 120.24(10) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 C8 121.33(11) . . ?
C10 C9 H9 119.3 . . ?
C9 C10 H10 120.1 . . ?
C9 C10 C11 119.85(11) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 119.7 . . ?
C10 C11 C12 120.64(11) . . ?
C12 C11 H11 119.7 . . ?
C7 C12 C14 120.43(10) . . ?
C11 C12 C7 119.28(10) . . ?
C11 C12 C14 120.26(10) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C15 Li2 79.83(7) . 2_655 ?
C6 C15 Li2 79.83(7) . . ?
C16 C15 C6 119.65(10) . . ?
C16 C15 Li2 94.54(7) . . ?
C16 C15 Li2 94.54(7) . 2_655 ?
C20 C15 C6 120.30(10) . . ?
C20 C15 C16 120.04(11) . . ?
C20 C15 Li2 96.35(9) . . ?
C20 C15 Li2 96.35(9) . 2_655 ?
Li2 C15 Li2 0.00(11) 2_655 . ?
C15 C16 C21 121.49(11) . . ?
C17 C16 C15 118.57(14) . . ?
C17 C16 C21 119.90(13) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 C16 121.58(15) . . ?
C18 C17 H17 119.2 . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.00(13) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 119.5 . . ?
C18 C19 C20 120.92(15) . . ?
C20 C19 H19 119.5 . . ?
C15 C20 C22 121.10(11) . . ?
C19 C20 C15 118.86(13) . . ?
C19 C20 C22 120.04(13) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 Li1 C1 114.59(13) 2_655 . ?
C1 Li1 C2 140.03(11) . 2_655 ?
C1 Li1 C2 30.09(3) 2_655 2_655 ?
C1 Li1 C7 148.51(5) 2_655 . ?
C1 Li1 C7 61.48(3) . . ?
C1 Li1 C7 148.50(5) . 2_655 ?
C1 Li1 C7 61.48(3) 2_655 2_655 ?
C7 Li1 C2 155.88(7) . 2_655 ?
C7 Li1 C2 31.88(3) 2_655 2_655 ?
C7 Li1 C7 139.36(12) 2_655 . ?
Li1 Li1 C1 0(10) 2_655 . ?
Li1 Li1 C1 0(10) 2_655 2_655 ?
Li1 Li1 C2 0(10) 2_655 2_655 ?
Li1 Li1 C7 0(10) 2_655 2_655 ?
Li1 Li1 C7 0(10) 2_655 . ?
C1 Li2 C1 116.50(13) . 2_655 ?
C1 Li2 C6 32.75(3) 2_655 2_655 ?
C1 Li2 C6 142.98(11) . 2_655 ?
C1 Li2 C15 143.95(4) . 2_655 ?
C1 Li2 C15 143.95(4) 2_655 . ?
C1 Li2 C15 66.28(4) . . ?
C1 Li2 C15 66.28(4) 2_655 2_655 ?
C1 Li2 Li1 58.25(6) 2_655 2_655 ?
C1 Li2 Li1 58.25(6) . 2_655 ?
C15 Li2 C6 34.43(3) 2_655 2_655 ?
C15 Li2 C6 148.89(8) . 2_655 ?
C15 Li2 C15 134.59(12) 2_655 . ?
Li1 Li2 C6 87.67(6) 2_655 2_655 ?
Li1 Li2 C15 112.71(6) 2_655 . ?
Li1 Li2 C15 112.71(6) 2_655 2_655 ?
Li2 Li2 C1 0(10) 2_655 2_655 ?
Li2 Li2 C1 0(10) 2_655 . ?
Li2 Li2 C6 0(10) 2_655 2_655 ?
Li2 Li2 C15 0(6) 2_655 2_655 ?
Li2 Li2 C15 0(10) 2_655 . ?
Li2 Li2 Li1 0(10) 2_655 2_655 ?
F1B C23B C4 111.05(14) . . ?
F2B C23B C4 114.51(19) . . ?
F2B C23B F1B 107.01(17) . . ?
F2B C23B F3B 107.2(2) . . ?
F3B C23B C4 112.4(2) . . ?
F3B C23B F1B 103.96(19) . . ?
F1A C23A C4 117.6(9) . . ?
F1A C23A F2A 103.0(11) . . ?
F1A C23A F3A 103.9(12) . . ?
F2A C23A C4 114.5(9) . . ?
F2A C23A F3A 104.0(12) . . ?
F3A C23A C4 112.4(8) . . ?
F1C C23C C4 112.3(4) . . ?
F1C C23C F2C 103.1(5) . . ?
F3C C23C C4 117.1(6) . . ?
F3C C23C F1C 110.4(6) . . ?
F3C C23C F2C 103.8(7) . . ?
F2C C23C C4 108.8(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -0.85(15) . . . . ?
C1 C2 C7 C8 97.11(12) . . . . ?
C1 C2 C7 C12 -84.71(12) . . . . ?
C1 C2 C7 Li1 -12.11(9) . . . . ?
C1 C2 C7 Li1 -12.11(9) . . . 2_655 ?
C1 C6 C15 C16 72.64(13) . . . . ?
C1 C6 C15 C20 -108.25(12) . . . . ?
C1 C6 C15 Li2 -16.80(9) . . . 2_655 ?
C1 C6 C15 Li2 -16.80(9) . . . . ?
C2 C1 C6 C5 0.41(14) . . . . ?
C2 C1 C6 C15 -178.98(9) . . . . ?
C2 C3 C4 C5 0.33(15) . . . . ?
C2 C3 C4 C23B 177.31(10) . . . . ?
C2 C3 C4 C23A 177.31(10) . . . . ?
C2 C3 C4 C23C 177.31(10) . . . . ?
C2 C7 C8 C9 178.97(10) . . . . ?
C2 C7 C8 C13 1.04(15) . . . . ?
C2 C7 C12 C11 -178.50(10) . . . . ?
C2 C7 C12 C14 -0.36(16) . . . . ?
C3 C2 C7 C8 -85.83(12) . . . . ?
C3 C2 C7 C12 92.35(12) . . . . ?
C3 C2 C7 Li1 164.95(9) . . . 2_655 ?
C3 C2 C7 Li1 164.95(9) . . . . ?
C3 C4 C5 C6 0.50(15) . . . . ?
C3 C4 C23B F1B -87.6(3) . . . . ?
C3 C4 C23B F2B 151.1(3) . . . . ?
C3 C4 C23B F3B 28.4(3) . . . . ?
C3 C4 C23A F1A -47.7(13) . . . . ?
C3 C4 C23A F2A -168.9(12) . . . . ?
C3 C4 C23A F3A 72.8(12) . . . . ?
C3 C4 C23C F1C -117.4(8) . . . . ?
C3 C4 C23C F3C 11.9(8) . . . . ?
C3 C4 C23C F2C 129.1(6) . . . . ?
C4 C5 C6 C1 -0.90(15) . . . . ?
C4 C5 C6 C15 178.51(9) . . . . ?
C5 C4 C23B F1B 89.4(3) . . . . ?
C5 C4 C23B F2B -31.9(3) . . . . ?
C5 C4 C23B F3B -154.6(3) . . . . ?
C5 C4 C23A F1A 129.2(13) . . . . ?
C5 C4 C23A F2A 8.1(12) . . . . ?
C5 C4 C23A F3A -110.2(12) . . . . ?
C5 C4 C23C F1C 59.5(9) . . . . ?
C5 C4 C23C F3C -171.2(8) . . . . ?
C5 C4 C23C F2C -54.0(7) . . . . ?
C5 C6 C15 C16 -106.78(11) . . . . ?
C5 C6 C15 C20 72.32(13) . . . . ?
C5 C6 C15 Li2 163.77(9) . . . 2_655 ?
C5 C6 C15 Li2 163.77(9) . . . . ?
C6 C1 C2 C3 0.47(14) . . . . ?
C6 C1 C2 C7 177.35(8) . . . . ?
C6 C15 C16 C17 177.21(11) . . . . ?
C6 C15 C16 C21 -0.85(17) . . . . ?
C6 C15 C20 C19 -177.81(11) . . . . ?
C6 C15 C20 C22 2.08(17) . . . . ?
C7 C2 C3 C4 -177.78(9) . . . . ?
C7 C8 C9 C10 -0.55(17) . . . . ?
C8 C7 C12 C11 -0.30(16) . . . . ?
C8 C7 C12 C14 177.84(11) . . . . ?
C8 C9 C10 C11 -0.21(19) . . . . ?
C9 C10 C11 C12 0.72(19) . . . . ?
C10 C11 C12 C7 -0.46(18) . . . . ?
C10 C11 C12 C14 -178.61(12) . . . . ?
C12 C7 C8 C9 0.80(15) . . . . ?
C12 C7 C8 C13 -177.12(10) . . . . ?
C13 C8 C9 C10 177.39(11) . . . . ?
C15 C16 C17 C18 0.9(2) . . . . ?
C16 C15 C20 C19 1.29(17) . . . . ?
C16 C15 C20 C22 -178.82(11) . . . . ?
C16 C17 C18 C19 0.7(3) . . . . ?
C17 C18 C19 C20 -1.4(3) . . . . ?
C18 C19 C20 C15 0.3(2) . . . . ?
C18 C19 C20 C22 -179.54(14) . . . . ?
C20 C15 C16 C17 -1.90(17) . . . . ?
C20 C15 C16 C21 -179.96(11) . . . . ?
C21 C16 C17 C18 178.99(15) . . . . ?
Li1 C1 C2 C3 -162.27(9) 2_655 . . . ?
Li1 C1 C2 C3 -162.27(9) . . . . ?
Li1 C1 C2 C7 14.60(10) 2_655 . . . ?
Li1 C1 C2 C7 14.60(10) . . . . ?
Li1 C1 C6 C5 151.41(12) 2_655 . . . ?
Li1 C1 C6 C5 151.41(12) . . . . ?
Li1 C1 C6 C15 -27.98(18) . . . . ?
Li1 C1 C6 C15 -27.98(18) 2_655 . . . ?
Li1 C7 C8 C9 -91.20(12) 2_655 . . . ?
Li1 C7 C8 C9 -91.20(12) . . . . ?
Li1 C7 C8 C13 90.88(12) . . . . ?
Li1 C7 C8 C13 90.88(12) 2_655 . . . ?
Li1 C7 C12 C11 110.04(10) . . . . ?
Li1 C7 C12 C11 110.04(10) 2_655 . . . ?
Li1 C7 C12 C14 -71.82(11) 2_655 . . . ?
Li1 C7 C12 C14 -71.82(11) . . . . ?
Li2 C1 C2 C3 144.34(15) 2_655 . . . ?
Li2 C1 C2 C3 144.34(15) . . . . ?
Li2 C1 C2 C7 -38.8(2) . . . . ?
Li2 C1 C2 C7 -38.8(2) 2_655 . . . ?
Li2 C1 C6 C5 -162.12(9) . . . . ?
Li2 C1 C6 C5 -162.12(9) 2_655 . . . ?
Li2 C1 C6 C15 18.49(10) . . . . ?
Li2 C1 C6 C15 18.49(10) 2_655 . . . ?
Li2 C15 C16 C17 -101.92(13) . . . . ?
Li2 C15 C16 C17 -101.92(13) 2_655 . . . ?
Li2 C15 C16 C21 80.02(13) . . . . ?
Li2 C15 C16 C21 80.02(13) 2_655 . . . ?
Li2 C15 C20 C19 100.29(11) . . . . ?
Li2 C15 C20 C19 100.29(11) 2_655 . . . ?
Li2 C15 C20 C22 -79.83(12) . . . . ?
Li2 C15 C20 C22 -79.83(12) 2_655 . . . ?
C23B C4 C5 C6 -176.50(9) . . . . ?
C23A C4 C5 C6 -176.50(9) . . . . ?
C23C C4 C5 C6 -176.50(9) . . . . ?

loop_
_audit_author_email
andrewvalentine93@gmail.com
_olex2_date_sample_data_collection 2016-10-24
_olex2_date_sample_submission    2016-10-21
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_original_sample_id LIAJVF
_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 1.938
_oxdiff_exptl_absorpt_empirical_full_min 0.569
####################################################################### 
# 
# 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_liajvg
_database_code_depnum_ccdc_archive 'CCDC 2045219'
loop_
_audit_author_name
_audit_author_address
'Stephen P. Argent'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2020-11-18 deposited with the CCDC.	2020-12-04 downloaded from the CCDC.
;
_nottingham_internal_coll_name   LIAJVG
_nottingham_internal_coll_number 16622
_nottingham_internal_coll_client AJV/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '90.00, 22.50'
_nottingham_internal_coll_frame_width 1.00
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   02/11/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVA, PL13110002'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 09/11/2018
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 09/11/2018
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 09/11/2018
_nottingham_internal_refinement_user pcxav1
_nottingham_internal_self_archive_date 09/11/2018
_nottingham_internal_self_validation_date 09/11/2018
_nottingham_internal_self_validation_user pcxav1
_nottingham_internal_validation_date ?
_nottingham_internal_validation_user ?
_nottingham_internal_archive_date ?
_refine_special_details          ?
_audit_creation_date             2020-06-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C50 H58 Li2 Si2'
_chemical_formula_sum            'C50 H58 Li2 Si2'
_chemical_formula_weight         729.02
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C50 H58 Li2 Si2'
_chemical_oxdiff_usercomment     
'LIAJVG #16622 GVA-1104 IN FOMBLIN FILM ON MICROMOUNT FOR AJV/DLK'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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                   11.7845(5)
_cell_length_b                   13.7778(6)
_cell_length_c                   16.2675(8)
_cell_angle_alpha                69.756(4)
_cell_angle_beta                 85.404(4)
_cell_angle_gamma                64.756(4)
_cell_volume                     2234.36(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7572
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.6570
_cell_measurement_theta_min      3.7600
_shelx_estimated_absorpt_T_max   0.936
_shelx_estimated_absorpt_T_min   0.832
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.084
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             784
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 -2 -8 0.0464
5 2 8 0.0632
-2 0 10 0.0643
6 2 -6 0.0661
1 -7 -2 0.0311
-1 7 1 0.0457
-2 4 9 0.0641
-7 -2 2 0.0827
-6 -6 1 0.0869
-1 7 -2 0.0440
2 -6 1 0.0205
1 0 -10 0.0608

_exptl_crystal_recrystallization_method 'Recrystallised from hexane at -30'
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.072
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.0015 -2.0053 -7.9976 0.0513 0.4913 0.8885
5.0015 2.0053 7.9976 -0.0513 -0.4913 -0.8885
-1.9948 0.0128 9.9994 -0.1375 -1.0168 -0.0932
5.9943 1.9877 -6.0020 0.1941 0.8492 -0.5162
1.0090 -6.9892 -1.9886 -0.8738 0.1691 -0.3156
-1.0095 6.9880 0.9886 0.8935 -0.0767 0.3518
-2.0011 4.0038 8.9930 0.3871 -0.8890 0.0879
-6.9964 -1.9925 2.0018 -0.0862 -0.5255 0.7953
-5.9912 -5.9862 1.0085 -0.6009 -0.4223 0.5522
-1.0111 6.9842 -2.0114 0.9523 0.2007 0.4603
2.0092 -5.9876 1.0100 -0.8358 -0.0533 -0.5222
0.9948 -0.0126 -9.9996 0.1669 0.9707 0.2275

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16819
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.801
_diffrn_reflns_theta_min         2.904
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 4.2207
_diffrn_detector_type            'Agilent Diffraction Titan S2 detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     21.00  47.00   1.00   22.50    --   43.31  38.00 -90.00   26
  2  ω     70.00  96.00   1.00   22.50    --   43.31  38.00 -90.00   26
  3  ω    102.00 156.00   1.00   90.00    --  103.00  77.00-180.00   54
  4  ω     99.00 153.00   1.00   90.00    --  103.00  30.00-180.00   54
  5  ω     63.00 109.00   1.00   90.00    --  103.00 -94.00-120.00   46
  6  ω     65.00 121.00   1.00   90.00    --  103.00-125.00-180.00   56
  7  ω     64.00  90.00   1.00   90.00    --  103.00 -45.00-150.00   26
  8  ω     42.00 108.00   1.00   90.00    --  103.00 -94.00 -30.00   66
  9  ω     53.00  90.00   1.00   90.00    --  103.00 -30.00  60.00   37
 10  ω     80.00 176.00   1.00   90.00    --  103.00  30.00  90.00   96
 11  ω     51.00  96.00   1.00   90.00    --  103.00 -94.00  60.00   45
 12  ω     36.00  96.00   1.00   90.00    --  103.00 -45.00  30.00   60
 13  ω     30.00  78.00   1.00   90.00    --  103.00 -30.00 -90.00   48
 14  ω     30.00  84.00   1.00   90.00    --  103.00 -30.00-180.00   54
 15  ω      3.00  91.00   1.00   22.50    --   43.31-125.00 -30.00   88
 16  ω     23.00  72.00   1.00   90.00    --  103.00 -94.00  30.00   49
 17  ω     35.00  99.00   1.00   90.00    --  103.00 -61.00 150.00   64
 18  ω   -109.00 -21.00   1.00   22.50    --  -43.31 -57.00  30.00   88
 19  ω   -115.00 -13.00   1.00   22.50    --  -43.31 -77.00 150.00  102
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Titan S2'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0293349000
_diffrn_orient_matrix_UB_12      0.1264163000
_diffrn_orient_matrix_UB_13      -0.0197673000
_diffrn_orient_matrix_UB_21      0.0461496000
_diffrn_orient_matrix_UB_22      0.0087776000
_diffrn_orient_matrix_UB_23      -0.0924946000
_diffrn_orient_matrix_UB_31      -0.1342820000
_diffrn_orient_matrix_UB_32      0.0360561000
_diffrn_orient_matrix_UB_33      -0.0361575000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7313
_reflns_number_total             8737
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.048
_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     501
_refine_ls_number_reflns         8737
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0482
_refine_ls_restrained_S_all      1.066
_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)+(0.0456P)²+1.1995P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1212
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18), C19(H19),
 C25(H25), C27(H27), C31(H31), C32(H32), C33(H33), C39(H39), C40(H40), C41(H41)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Si1 Si 0.01021(5) 0.98318(4) 0.31931(4) 0.02617(13) Uani 1 1 d . . . . .
Si2 Si 0.51465(5) 0.00514(4) 0.17546(3) 0.02231(12) Uani 1 1 d . . . . .
C1 C 0.24246(16) 0.62294(14) 0.28157(11) 0.0180(3) Uani 1 1 d . . . . .
C2 C 0.27610(16) 0.71581(14) 0.24752(11) 0.0190(3) Uani 1 1 d . . . . .
C3 C 0.21130(17) 0.81894(15) 0.26231(12) 0.0217(4) Uani 1 1 d . . . . .
H3 H 0.238776 0.877877 0.237885 0.026 Uiso 1 1 calc R U . . .
C4 C 0.10692(17) 0.83781(15) 0.31219(12) 0.0217(4) Uani 1 1 d . . . . .
C5 C 0.07205(16) 0.74761(15) 0.34747(12) 0.0203(4) Uani 1 1 d . . . . .
H5 H 0.002000 0.756789 0.382220 0.024 Uiso 1 1 calc R U . . .
C6 C 0.13788(16) 0.64389(14) 0.33287(11) 0.0187(3) Uani 1 1 d . . . . .
C7 C 0.38557(16) 0.70269(14) 0.19182(12) 0.0186(3) Uani 1 1 d . . . . .
C8 C 0.36621(17) 0.74597(14) 0.09963(12) 0.0209(4) Uani 1 1 d . . . . .
C9 C 0.47006(18) 0.72956(15) 0.04958(13) 0.0245(4) Uani 1 1 d . . . . .
H9 H 0.457653 0.756866 -0.012699 0.029 Uiso 1 1 calc R U . . .
C10 C 0.59154(18) 0.67369(16) 0.08979(13) 0.0263(4) Uani 1 1 d . . . . .
H10 H 0.661734 0.663668 0.055155 0.032 Uiso 1 1 calc R U . . .
C11 C 0.60975(18) 0.63268(16) 0.18064(13) 0.0262(4) Uani 1 1 d . . . . .
H11 H 0.692918 0.594885 0.207867 0.031 Uiso 1 1 calc R U . . .
C12 C 0.50850(17) 0.64582(15) 0.23272(12) 0.0213(4) Uani 1 1 d . . . . .
C13 C 0.23480(18) 0.81075(17) 0.05540(13) 0.0279(4) Uani 1 1 d . . . . .
H13A H 0.185661 0.767019 0.081613 0.042 Uiso 1 1 calc R U . . .
H13B H 0.238432 0.822163 -0.007482 0.042 Uiso 1 1 calc R U . . .
H13C H 0.194786 0.885224 0.063290 0.042 Uiso 1 1 calc R U . . .
C14 C 0.52982(18) 0.60255(17) 0.33187(13) 0.0281(4) Uani 1 1 d . . . . .
H14A H 0.479430 0.664826 0.353855 0.042 Uiso 1 1 calc R U . . .
H14B H 0.619150 0.575113 0.348582 0.042 Uiso 1 1 calc R U . . .
H14C H 0.504663 0.539700 0.357365 0.042 Uiso 1 1 calc R U . . .
C15 C 0.09136(16) 0.55220(15) 0.36798(11) 0.0190(3) Uani 1 1 d . . . . .
C16 C 0.16189(17) 0.45000(15) 0.43692(12) 0.0212(4) Uani 1 1 d . . . . .
C17 C 0.12098(19) 0.36315(16) 0.46436(13) 0.0261(4) Uani 1 1 d . . . . .
H17 H 0.168369 0.293905 0.510488 0.031 Uiso 1 1 calc R U . . .
C18 C 0.01281(19) 0.37615(17) 0.42562(13) 0.0283(4) Uani 1 1 d . . . . .
H18 H -0.013212 0.315921 0.444396 0.034 Uiso 1 1 calc R U . . .
C19 C -0.05737(18) 0.47770(17) 0.35919(13) 0.0275(4) Uani 1 1 d . . . . .
H19 H -0.132131 0.486795 0.332998 0.033 Uiso 1 1 calc R U . . .
C20 C -0.02028(17) 0.56693(16) 0.33003(12) 0.0224(4) Uani 1 1 d . . . . .
C21 C 0.27711(18) 0.43512(16) 0.48269(13) 0.0274(4) Uani 1 1 d . . . . .
H21A H 0.347228 0.420271 0.445083 0.041 Uiso 1 1 calc R U . . .
H21B H 0.299227 0.370476 0.538233 0.041 Uiso 1 1 calc R U . . .
H21C H 0.259992 0.504923 0.494608 0.041 Uiso 1 1 calc R U . . .
C22 C -0.1016(2) 0.67767(18) 0.25913(14) 0.0325(5) Uani 1 1 d . . . . .
H22A H -0.143067 0.737643 0.284930 0.049 Uiso 1 1 calc R U . . .
H22B H -0.165437 0.666917 0.232900 0.049 Uiso 1 1 calc R U . . .
H22C H -0.048948 0.700184 0.213646 0.049 Uiso 1 1 calc R U . . .
C23 C 0.37567(16) 0.35656(14) 0.22904(11) 0.0178(3) Uani 1 1 d . . . . .
C24 C 0.48924(16) 0.25965(14) 0.26812(11) 0.0183(3) Uani 1 1 d . . . . .
C25 C 0.53058(17) 0.15798(15) 0.25050(12) 0.0208(4) Uani 1 1 d . . . . .
H25 H 0.608088 0.096031 0.278436 0.025 Uiso 1 1 calc R U . . .
C26 C 0.46056(17) 0.14534(15) 0.19274(11) 0.0203(4) Uani 1 1 d . . . . .
C27 C 0.34803(17) 0.23984(15) 0.15285(11) 0.0197(3) Uani 1 1 d . . . . .
H27 H 0.297708 0.234695 0.113160 0.024 Uiso 1 1 calc R U . . .
C28 C 0.30776(16) 0.34184(14) 0.17002(11) 0.0185(3) Uani 1 1 d . . . . .
C29 C 0.57076(16) 0.26638(14) 0.33029(12) 0.0188(3) Uani 1 1 d . . . . .
C30 C 0.65637(17) 0.31410(15) 0.29686(12) 0.0222(4) Uani 1 1 d . . . . .
C31 C 0.73217(19) 0.31945(17) 0.35527(14) 0.0294(4) Uani 1 1 d . . . . .
H31 H 0.790881 0.350806 0.333097 0.035 Uiso 1 1 calc R U . . .
C32 C 0.72307(19) 0.27976(17) 0.44500(14) 0.0315(5) Uani 1 1 d . . . . .
H32 H 0.774678 0.284560 0.484024 0.038 Uiso 1 1 calc R U . . .
C33 C 0.63859(19) 0.23306(17) 0.47768(13) 0.0292(4) Uani 1 1 d . . . . .
H33 H 0.631765 0.206931 0.539290 0.035 Uiso 1 1 calc R U . . .
C34 C 0.56333(18) 0.22376(15) 0.42166(12) 0.0231(4) Uani 1 1 d . . . . .
C35 C 0.66810(19) 0.35606(17) 0.19915(13) 0.0288(4) Uani 1 1 d . . . . .
H35A H 0.677889 0.296844 0.175323 0.043 Uiso 1 1 calc R U . . .
H35B H 0.741797 0.373025 0.188039 0.043 Uiso 1 1 calc R U . . .
H35C H 0.592223 0.425551 0.170616 0.043 Uiso 1 1 calc R U . . .
C36 C 0.4766(2) 0.1666(2) 0.45787(14) 0.0347(5) Uani 1 1 d . . . . .
H36A H 0.392286 0.216019 0.427779 0.052 Uiso 1 1 calc R U . . .
H36B H 0.472207 0.153465 0.520988 0.052 Uiso 1 1 calc R U . . .
H36C H 0.508966 0.093285 0.448350 0.052 Uiso 1 1 calc R U . . .
C37 C 0.18594(17) 0.44023(15) 0.12442(12) 0.0205(4) Uani 1 1 d . . . . .
C38 C 0.07022(18) 0.43483(17) 0.14481(13) 0.0258(4) Uani 1 1 d . . . . .
C39 C -0.04086(19) 0.52919(19) 0.10342(15) 0.0341(5) Uani 1 1 d . . . . .
H39 H -0.119320 0.525929 0.117244 0.041 Uiso 1 1 calc R U . . .
C40 C -0.0388(2) 0.62740(19) 0.04262(15) 0.0371(5) Uani 1 1 d . . . . .
H40 H -0.115435 0.691394 0.015595 0.045 Uiso 1 1 calc R U . . .
C41 C 0.0745(2) 0.63244(17) 0.02123(14) 0.0321(5) Uani 1 1 d . . . . .
H41 H 0.075278 0.699898 -0.021181 0.039 Uiso 1 1 calc R U . . .
C42 C 0.18858(18) 0.53968(16) 0.06102(12) 0.0239(4) Uani 1 1 d . . . . .
C43 C 0.0641(2) 0.32809(19) 0.20890(15) 0.0329(5) Uani 1 1 d . . . . .
H43A H 0.088658 0.270148 0.180970 0.049 Uiso 1 1 calc R U . . .
H43B H -0.021993 0.346113 0.226474 0.049 Uiso 1 1 calc R U . . .
H43C H 0.121645 0.298616 0.260930 0.049 Uiso 1 1 calc R U . . .
C44 C 0.3111(2) 0.54518(17) 0.03349(13) 0.0300(4) Uani 1 1 d . . . . .
H44A H 0.352571 0.548719 0.081552 0.045 Uiso 1 1 calc R U . . .
H44B H 0.294993 0.613551 -0.018496 0.045 Uiso 1 1 calc R U . . .
H44C H 0.365658 0.476872 0.019451 0.045 Uiso 1 1 calc R U . . .
C45 C 0.1081(3) 1.0327(2) 0.36392(19) 0.0510(7) Uani 1 1 d . . . . .
H45A H 0.142814 0.980227 0.423693 0.077 Uiso 1 1 calc R U . . .
H45B H 0.055920 1.109720 0.365133 0.077 Uiso 1 1 calc R U . . .
H45C H 0.177129 1.034231 0.326404 0.077 Uiso 1 1 calc R U . . .
C46 C -0.1227(3) 0.9787(2) 0.38888(18) 0.0502(7) Uani 1 1 d . . . . .
H46A H -0.172246 0.951825 0.364387 0.075 Uiso 1 1 calc R U . . .
H46B H -0.176467 1.055495 0.389894 0.075 Uiso 1 1 calc R U . . .
H46C H -0.089074 0.926347 0.448866 0.075 Uiso 1 1 calc R U . . .
C47 C -0.0525(2) 1.08426(19) 0.20523(16) 0.0430(6) Uani 1 1 d . . . . .
H47A H -0.093603 1.162802 0.205388 0.065 Uiso 1 1 calc R U . . .
H47B H -0.113729 1.066269 0.183544 0.065 Uiso 1 1 calc R U . . .
H47C H 0.016922 1.076770 0.166849 0.065 Uiso 1 1 calc R U . . .
C48 C 0.6722(2) -0.03339(17) 0.12999(14) 0.0309(4) Uani 1 1 d . . . . .
H48A H 0.665147 0.023037 0.071597 0.046 Uiso 1 1 calc R U . . .
H48B H 0.702236 -0.109366 0.125388 0.046 Uiso 1 1 calc R U . . .
H48C H 0.731758 -0.034085 0.169121 0.046 Uiso 1 1 calc R U . . .
C49 C 0.3967(2) 0.01445(19) 0.09982(15) 0.0352(5) Uani 1 1 d . . . . .
H49A H 0.314499 0.035781 0.124374 0.053 Uiso 1 1 calc R U . . .
H49B H 0.423194 -0.059925 0.092972 0.053 Uiso 1 1 calc R U . . .
H49C H 0.390358 0.072376 0.042363 0.053 Uiso 1 1 calc R U . . .
C50 C 0.5309(3) -0.10820(18) 0.28446(14) 0.0400(5) Uani 1 1 d . . . . .
H50A H 0.590923 -0.110937 0.324532 0.060 Uiso 1 1 calc R U . . .
H50B H 0.561501 -0.182514 0.276781 0.060 Uiso 1 1 calc R U . . .
H50C H 0.448858 -0.090505 0.309152 0.060 Uiso 1 1 calc R U . . .
Li1 Li 0.4084(3) 0.4838(3) 0.2622(2) 0.0288(7) Uani 1 1 d . . . . .
Li2 Li 0.2081(3) 0.4955(3) 0.2492(2) 0.0261(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C4 1.8752(18) . ?
Si1 C45 1.863(3) . ?
Si1 C46 1.867(3) . ?
Si1 C47 1.866(2) . ?
Si2 C26 1.8743(18) . ?
Si2 C48 1.867(2) . ?
Si2 C49 1.864(2) . ?
Si2 C50 1.871(2) . ?
C1 C2 1.417(2) . ?
C1 C6 1.413(2) . ?
C1 Li1 2.173(4) . ?
C1 Li2 2.193(4) . ?
C2 C3 1.393(2) . ?
C2 C7 1.498(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.397(3) . ?
C4 C5 1.395(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.400(2) . ?
C6 C15 1.504(2) . ?
C6 Li2 2.650(4) . ?
C7 C8 1.406(3) . ?
C7 C12 1.407(3) . ?
C7 Li1 2.729(4) . ?
C8 C9 1.394(3) . ?
C8 C13 1.506(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.390(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.385(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.391(3) . ?
C12 C14 1.514(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.411(2) . ?
C15 C20 1.403(3) . ?
C15 Li2 2.437(4) . ?
C16 C17 1.397(3) . ?
C16 C21 1.503(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.382(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.385(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.396(3) . ?
C20 C22 1.513(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.415(2) . ?
C23 C28 1.414(2) . ?
C23 Li1 2.185(4) . ?
C23 Li2 2.186(3) . ?
C24 C25 1.398(2) . ?
C24 C29 1.500(2) . ?
C24 Li1 2.784(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.398(3) . ?
C26 C27 1.398(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.400(2) . ?
C28 C37 1.505(2) . ?
C28 Li2 2.654(4) . ?
C29 C30 1.406(3) . ?
C29 C34 1.407(3) . ?
C29 Li1 2.649(4) . ?
C30 C31 1.395(3) . ?
C30 C35 1.509(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.383(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.383(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.393(3) . ?
C34 C36 1.510(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.404(3) . ?
C37 C42 1.413(3) . ?
C37 Li2 2.468(4) . ?
C38 C39 1.393(3) . ?
C38 C43 1.507(3) . ?
C39 H39 0.9500 . ?
C39 C40 1.381(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.377(3) . ?
C41 H41 0.9500 . ?
C41 C42 1.400(3) . ?
C42 C44 1.502(3) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
Li1 Li2 2.319(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C45 Si1 C4 111.22(10) . . ?
C45 Si1 C46 111.04(15) . . ?
C45 Si1 C47 108.13(12) . . ?
C46 Si1 C4 109.14(10) . . ?
C47 Si1 C4 107.29(10) . . ?
C47 Si1 C46 109.95(13) . . ?
C48 Si2 C26 110.23(9) . . ?
C48 Si2 C50 108.00(11) . . ?
C49 Si2 C26 109.57(9) . . ?
C49 Si2 C48 110.68(10) . . ?
C49 Si2 C50 109.85(11) . . ?
C50 Si2 C26 108.46(9) . . ?
C2 C1 Li1 101.79(15) . . ?
C2 C1 Li2 144.48(16) . . ?
C6 C1 C2 113.85(15) . . ?
C6 C1 Li1 141.46(16) . . ?
C6 C1 Li2 92.01(14) . . ?
Li1 C1 Li2 64.16(13) . . ?
C1 C2 C7 118.18(15) . . ?
C3 C2 C1 123.20(16) . . ?
C3 C2 C7 118.61(16) . . ?
C2 C3 H3 119.2 . . ?
C2 C3 C4 121.63(17) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 Si1 120.43(14) . . ?
C5 C4 Si1 122.59(14) . . ?
C5 C4 C3 116.63(16) . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.54(16) . . ?
C6 C5 H5 119.2 . . ?
C1 C6 C15 117.55(15) . . ?
C1 C6 Li2 55.78(12) . . ?
C5 C6 C1 123.13(16) . . ?
C5 C6 C15 119.20(16) . . ?
C5 C6 Li2 158.31(14) . . ?
C15 C6 Li2 65.19(12) . . ?
C2 C7 Li1 77.98(12) . . ?
C8 C7 C2 120.56(16) . . ?
C8 C7 C12 120.13(17) . . ?
C8 C7 Li1 112.47(14) . . ?
C12 C7 C2 119.32(16) . . ?
C12 C7 Li1 79.45(12) . . ?
C7 C8 C13 120.40(16) . . ?
C9 C8 C7 119.24(17) . . ?
C9 C8 C13 120.35(17) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 C8 120.73(18) . . ?
C10 C9 H9 119.6 . . ?
C9 C10 H10 120.2 . . ?
C11 C10 C9 119.66(18) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 119.4 . . ?
C10 C11 C12 121.20(17) . . ?
C12 C11 H11 119.4 . . ?
C7 C12 C14 120.39(17) . . ?
C11 C12 C7 119.02(17) . . ?
C11 C12 C14 120.57(17) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C15 Li2 80.73(13) . . ?
C16 C15 C6 120.14(16) . . ?
C16 C15 Li2 96.58(13) . . ?
C20 C15 C6 119.84(16) . . ?
C20 C15 C16 119.98(17) . . ?
C20 C15 Li2 90.84(14) . . ?
C15 C16 C21 121.04(17) . . ?
C17 C16 C15 118.99(17) . . ?
C17 C16 C21 119.94(16) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 C16 121.20(17) . . ?
C18 C17 H17 119.4 . . ?
C17 C18 H18 120.3 . . ?
C17 C18 C19 119.47(18) . . ?
C19 C18 H18 120.3 . . ?
C18 C19 H19 119.4 . . ?
C18 C19 C20 121.23(18) . . ?
C20 C19 H19 119.4 . . ?
C15 C20 C22 121.38(17) . . ?
C19 C20 C15 119.09(17) . . ?
C19 C20 C22 119.53(17) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 Li1 99.05(14) . . ?
C24 C23 Li2 146.16(16) . . ?
C28 C23 C24 114.05(15) . . ?
C28 C23 Li1 143.93(16) . . ?
C28 C23 Li2 92.45(14) . . ?
Li1 C23 Li2 64.08(13) . . ?
C23 C24 C29 118.76(15) . . ?
C23 C24 Li1 50.82(11) . . ?
C25 C24 C23 123.12(16) . . ?
C25 C24 C29 118.11(15) . . ?
C25 C24 Li1 166.96(15) . . ?
C29 C24 Li1 69.05(11) . . ?
C24 C25 H25 119.2 . . ?
C26 C25 C24 121.57(16) . . ?
C26 C25 H25 119.2 . . ?
C25 C26 Si2 120.32(13) . . ?
C25 C26 C27 116.62(16) . . ?
C27 C26 Si2 123.00(14) . . ?
C26 C27 H27 119.2 . . ?
C26 C27 C28 121.57(16) . . ?
C28 C27 H27 119.2 . . ?
C23 C28 C37 118.26(15) . . ?
C23 C28 Li2 55.38(11) . . ?
C27 C28 C23 123.06(16) . . ?
C27 C28 C37 118.68(16) . . ?
C27 C28 Li2 161.12(15) . . ?
C37 C28 Li2 66.25(11) . . ?
C24 C29 Li1 79.01(12) . . ?
C30 C29 C24 119.60(16) . . ?
C30 C29 C34 119.94(17) . . ?
C30 C29 Li1 81.16(12) . . ?
C34 C29 C24 120.45(16) . . ?
C34 C29 Li1 110.83(14) . . ?
C29 C30 C35 120.18(17) . . ?
C31 C30 C29 119.14(18) . . ?
C31 C30 C35 120.65(18) . . ?
C30 C31 H31 119.5 . . ?
C32 C31 C30 120.96(19) . . ?
C32 C31 H31 119.5 . . ?
C31 C32 H32 120.1 . . ?
C33 C32 C31 119.76(18) . . ?
C33 C32 H32 120.1 . . ?
C32 C33 H33 119.5 . . ?
C32 C33 C34 121.02(19) . . ?
C34 C33 H33 119.5 . . ?
C29 C34 C36 119.99(17) . . ?
C33 C34 C29 119.14(18) . . ?
C33 C34 C36 120.86(18) . . ?
C30 C35 H35A 109.5 . . ?
C30 C35 H35B 109.5 . . ?
C30 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C28 C37 Li2 79.83(12) . . ?
C38 C37 C28 120.91(17) . . ?
C38 C37 C42 119.84(17) . . ?
C38 C37 Li2 96.12(14) . . ?
C42 C37 C28 119.25(16) . . ?
C42 C37 Li2 93.37(14) . . ?
C37 C38 C43 121.30(17) . . ?
C39 C38 C37 119.25(19) . . ?
C39 C38 C43 119.44(19) . . ?
C38 C39 H39 119.5 . . ?
C40 C39 C38 121.1(2) . . ?
C40 C39 H39 119.5 . . ?
C39 C40 H40 120.0 . . ?
C41 C40 C39 119.92(18) . . ?
C41 C40 H40 120.0 . . ?
C40 C41 H41 119.5 . . ?
C40 C41 C42 121.0(2) . . ?
C42 C41 H41 119.5 . . ?
C37 C42 C44 121.08(16) . . ?
C41 C42 C37 118.86(19) . . ?
C41 C42 C44 120.02(18) . . ?
C38 C43 H43A 109.5 . . ?
C38 C43 H43B 109.5 . . ?
C38 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
Si1 C45 H45A 109.5 . . ?
Si1 C45 H45B 109.5 . . ?
Si1 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
Si1 C46 H46A 109.5 . . ?
Si1 C46 H46B 109.5 . . ?
Si1 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
Si1 C47 H47A 109.5 . . ?
Si1 C47 H47B 109.5 . . ?
Si1 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
Si2 C48 H48A 109.5 . . ?
Si2 C48 H48B 109.5 . . ?
Si2 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
Si2 C49 H49A 109.5 . . ?
Si2 C49 H49B 109.5 . . ?
Si2 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
Si2 C50 H50A 109.5 . . ?
Si2 C50 H50B 109.5 . . ?
Si2 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C1 Li1 C7 60.11(10) . . ?
C1 Li1 C23 116.30(16) . . ?
C1 Li1 C24 140.42(16) . . ?
C1 Li1 C29 146.32(18) . . ?
C1 Li1 Li2 58.33(12) . . ?
C7 Li1 C24 154.66(15) . . ?
C23 Li1 C7 141.73(17) . . ?
C23 Li1 C24 30.14(7) . . ?
C23 Li1 C29 61.67(10) . . ?
C23 Li1 Li2 57.97(12) . . ?
C29 Li1 C7 144.29(14) . . ?
C29 Li1 C24 31.94(6) . . ?
Li2 Li1 C7 106.10(15) . . ?
Li2 Li1 C24 84.63(14) . . ?
Li2 Li1 C29 109.48(16) . . ?
C1 Li2 C6 32.20(7) . . ?
C1 Li2 C15 64.98(11) . . ?
C1 Li2 C28 141.70(16) . . ?
C1 Li2 C37 142.42(18) . . ?
C1 Li2 Li1 57.51(12) . . ?
C6 Li2 C28 172.81(15) . . ?
C15 Li2 C6 34.08(7) . . ?
C15 Li2 C28 149.37(16) . . ?
C15 Li2 C37 141.00(15) . . ?
C23 Li2 C1 115.46(16) . . ?
C23 Li2 C6 140.85(16) . . ?
C23 Li2 C15 140.16(17) . . ?
C23 Li2 C28 32.17(7) . . ?
C23 Li2 C37 64.82(10) . . ?
C23 Li2 Li1 57.95(12) . . ?
C37 Li2 C6 151.59(15) . . ?
C37 Li2 C28 33.92(7) . . ?
Li1 Li2 C6 85.91(14) . . ?
Li1 Li2 C15 108.48(16) . . ?
Li1 Li2 C28 86.98(13) . . ?
Li1 Li2 C37 110.47(16) . . ?

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
Si1 C4 C5 C6 172.70(14) . . . . ?
Si2 C26 C27 C28 177.29(14) . . . . ?
C1 C2 C3 C4 -0.3(3) . . . . ?
C1 C2 C7 C8 97.1(2) . . . . ?
C1 C2 C7 C12 -82.6(2) . . . . ?
C1 C2 C7 Li1 -12.10(16) . . . . ?
C1 C6 C15 C16 72.3(2) . . . . ?
C1 C6 C15 C20 -105.59(19) . . . . ?
C1 C6 C15 Li2 -19.98(16) . . . . ?
C2 C1 C6 C5 1.1(2) . . . . ?
C2 C1 C6 C15 176.99(15) . . . . ?
C2 C1 C6 Li2 154.97(19) . . . . ?
C2 C3 C4 Si1 -172.47(14) . . . . ?
C2 C3 C4 C5 0.9(3) . . . . ?
C2 C7 C8 C9 -178.15(16) . . . . ?
C2 C7 C8 C13 2.7(3) . . . . ?
C2 C7 C12 C11 179.20(16) . . . . ?
C2 C7 C12 C14 -2.5(3) . . . . ?
C3 C2 C7 C8 -82.1(2) . . . . ?
C3 C2 C7 C12 98.3(2) . . . . ?
C3 C2 C7 Li1 168.79(17) . . . . ?
C3 C4 C5 C6 -0.5(3) . . . . ?
C4 C5 C6 C1 -0.5(3) . . . . ?
C4 C5 C6 C15 -176.35(16) . . . . ?
C4 C5 C6 Li2 -80.3(4) . . . . ?
C5 C6 C15 C16 -111.63(19) . . . . ?
C5 C6 C15 C20 70.5(2) . . . . ?
C5 C6 C15 Li2 156.11(17) . . . . ?
C6 C1 C2 C3 -0.7(2) . . . . ?
C6 C1 C2 C7 -179.75(15) . . . . ?
C6 C15 C16 C17 -175.79(16) . . . . ?
C6 C15 C16 C21 6.2(3) . . . . ?
C6 C15 C20 C19 175.48(17) . . . . ?
C6 C15 C20 C22 -5.2(3) . . . . ?
C7 C2 C3 C4 178.76(16) . . . . ?
C7 C8 C9 C10 -1.6(3) . . . . ?
C8 C7 C12 C11 -0.4(3) . . . . ?
C8 C7 C12 C14 177.92(16) . . . . ?
C8 C9 C10 C11 0.7(3) . . . . ?
C9 C10 C11 C12 0.3(3) . . . . ?
C10 C11 C12 C7 -0.5(3) . . . . ?
C10 C11 C12 C14 -178.82(18) . . . . ?
C12 C7 C8 C9 1.5(3) . . . . ?
C12 C7 C8 C13 -177.70(17) . . . . ?
C13 C8 C9 C10 177.53(18) . . . . ?
C15 C16 C17 C18 -0.4(3) . . . . ?
C16 C15 C20 C19 -2.4(3) . . . . ?
C16 C15 C20 C22 176.91(17) . . . . ?
C16 C17 C18 C19 -0.9(3) . . . . ?
C17 C18 C19 C20 0.6(3) . . . . ?
C18 C19 C20 C15 1.1(3) . . . . ?
C18 C19 C20 C22 -178.26(19) . . . . ?
C20 C15 C16 C17 2.1(3) . . . . ?
C20 C15 C16 C21 -175.93(17) . . . . ?
C21 C16 C17 C18 177.61(18) . . . . ?
C23 C24 C25 C26 -0.5(3) . . . . ?
C23 C24 C29 C30 -84.1(2) . . . . ?
C23 C24 C29 C34 96.9(2) . . . . ?
C23 C24 C29 Li1 -10.96(17) . . . . ?
C23 C28 C37 C38 -110.8(2) . . . . ?
C23 C28 C37 C42 68.4(2) . . . . ?
C23 C28 C37 Li2 -19.73(17) . . . . ?
C24 C23 C28 C27 1.1(3) . . . . ?
C24 C23 C28 C37 -179.58(16) . . . . ?
C24 C23 C28 Li2 158.4(2) . . . . ?
C24 C25 C26 Si2 -176.67(14) . . . . ?
C24 C25 C26 C27 0.7(3) . . . . ?
C24 C29 C30 C31 -179.70(16) . . . . ?
C24 C29 C30 C35 -1.3(2) . . . . ?
C24 C29 C34 C33 -178.85(16) . . . . ?
C24 C29 C34 C36 2.4(3) . . . . ?
C25 C24 C29 C30 94.9(2) . . . . ?
C25 C24 C29 C34 -84.2(2) . . . . ?
C25 C24 C29 Li1 168.00(17) . . . . ?
C25 C26 C27 C28 0.0(3) . . . . ?
C26 C27 C28 C23 -0.9(3) . . . . ?
C26 C27 C28 C37 179.72(16) . . . . ?
C26 C27 C28 Li2 -79.9(5) . . . . ?
C27 C28 C37 C38 68.6(2) . . . . ?
C27 C28 C37 C42 -112.2(2) . . . . ?
C27 C28 C37 Li2 159.65(17) . . . . ?
C28 C23 C24 C25 -0.4(3) . . . . ?
C28 C23 C24 C29 178.55(15) . . . . ?
C28 C23 C24 Li1 165.3(2) . . . . ?
C28 C37 C38 C39 177.77(17) . . . . ?
C28 C37 C38 C43 -3.7(3) . . . . ?
C28 C37 C42 C41 -177.70(17) . . . . ?
C28 C37 C42 C44 4.8(3) . . . . ?
C29 C24 C25 C26 -179.43(16) . . . . ?
C29 C30 C31 C32 -0.7(3) . . . . ?
C30 C29 C34 C33 2.1(3) . . . . ?
C30 C29 C34 C36 -176.64(17) . . . . ?
C30 C31 C32 C33 0.6(3) . . . . ?
C31 C32 C33 C34 0.9(3) . . . . ?
C32 C33 C34 C29 -2.2(3) . . . . ?
C32 C33 C34 C36 176.47(19) . . . . ?
C34 C29 C30 C31 -0.6(3) . . . . ?
C34 C29 C30 C35 177.79(16) . . . . ?
C35 C30 C31 C32 -179.14(18) . . . . ?
C37 C38 C39 C40 0.3(3) . . . . ?
C38 C37 C42 C41 1.6(3) . . . . ?
C38 C37 C42 C44 -175.96(17) . . . . ?
C38 C39 C40 C41 0.9(3) . . . . ?
C39 C40 C41 C42 -0.8(3) . . . . ?
C40 C41 C42 C37 -0.4(3) . . . . ?
C40 C41 C42 C44 177.12(19) . . . . ?
C42 C37 C38 C39 -1.5(3) . . . . ?
C42 C37 C38 C43 177.06(18) . . . . ?
C43 C38 C39 C40 -178.3(2) . . . . ?
C45 Si1 C4 C3 -58.29(19) . . . . ?
C45 Si1 C4 C5 128.72(18) . . . . ?
C46 Si1 C4 C3 178.87(17) . . . . ?
C46 Si1 C4 C5 5.9(2) . . . . ?
C47 Si1 C4 C3 59.77(18) . . . . ?
C47 Si1 C4 C5 -113.22(17) . . . . ?
C48 Si2 C26 C25 -61.02(17) . . . . ?
C48 Si2 C26 C27 121.79(16) . . . . ?
C49 Si2 C26 C25 176.94(15) . . . . ?
C49 Si2 C26 C27 -0.25(19) . . . . ?
C50 Si2 C26 C25 57.03(18) . . . . ?
C50 Si2 C26 C27 -120.16(17) . . . . ?
Li1 C1 C2 C3 -165.69(18) . . . . ?
Li1 C1 C2 C7 15.3(2) . . . . ?
Li1 C1 C6 C5 157.1(2) . . . . ?
Li1 C1 C6 C15 -27.0(3) . . . . ?
Li1 C1 C6 Li2 -49.0(2) . . . . ?
Li1 C7 C8 C9 -89.16(19) . . . . ?
Li1 C7 C8 C13 91.68(19) . . . . ?
Li1 C7 C12 C11 109.54(18) . . . . ?
Li1 C7 C12 C14 -72.12(18) . . . . ?
Li1 C23 C24 C25 -165.67(18) . . . . ?
Li1 C23 C24 C29 13.2(2) . . . . ?
Li1 C23 C28 C27 155.9(2) . . . . ?
Li1 C23 C28 C37 -24.8(3) . . . . ?
Li1 C23 C28 Li2 -46.8(2) . . . . ?
Li1 C24 C25 C26 -58.8(7) . . . . ?
Li1 C24 C29 C30 -73.12(16) . . . . ?
Li1 C24 C29 C34 107.82(17) . . . . ?
Li1 C29 C30 C31 108.37(18) . . . . ?
Li1 C29 C30 C35 -73.20(17) . . . . ?
Li1 C29 C34 C33 -89.59(19) . . . . ?
Li1 C29 C34 C36 91.7(2) . . . . ?
Li2 C1 C2 C3 132.6(2) . . . . ?
Li2 C1 C2 C7 -46.5(3) . . . . ?
Li2 C1 C6 C5 -153.89(18) . . . . ?
Li2 C1 C6 C15 22.03(18) . . . . ?
Li2 C6 C15 C16 92.26(17) . . . . ?
Li2 C6 C15 C20 -85.62(17) . . . . ?
Li2 C15 C16 C17 -92.71(18) . . . . ?
Li2 C15 C16 C21 89.28(19) . . . . ?
Li2 C15 C20 C19 95.69(19) . . . . ?
Li2 C15 C20 C22 -85.00(19) . . . . ?
Li2 C23 C24 C25 138.2(3) . . . . ?
Li2 C23 C24 C29 -42.9(3) . . . . ?
Li2 C23 C24 Li1 -56.1(3) . . . . ?
Li2 C23 C28 C27 -157.29(18) . . . . ?
Li2 C23 C28 C37 22.06(19) . . . . ?
Li2 C28 C37 C38 -91.08(18) . . . . ?
Li2 C28 C37 C42 88.17(17) . . . . ?
Li2 C37 C38 C39 95.98(19) . . . . ?
Li2 C37 C38 C43 -85.5(2) . . . . ?
Li2 C37 C42 C41 -97.46(18) . . . . ?
Li2 C37 C42 C44 85.01(19) . . . . ?

_olex2_date_sample_data_collection 2016-11-02
_olex2_date_sample_submission    2016-10-28
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_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 1.504
_oxdiff_exptl_absorpt_empirical_full_min 0.708
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_oajvlc
_database_code_depnum_ccdc_archive 'CCDC 2045215'
loop_
_audit_author_name
_audit_author_address
'Stephen P. Argent'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2020-11-18 deposited with the CCDC.	2020-12-04 downloaded from the CCDC.
;
_nottingham_internal_coll_name   OAJVLC
_nottingham_internal_coll_number 15517
_nottingham_internal_coll_client AJV/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '4.0000, 1.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   25/01/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 27/01/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 29/10/18
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 29/10/18
_nottingham_internal_refinement_user pcxav1
_nottingham_internal_self_archive_date 29/10/18
_nottingham_internal_self_validation_date 29/10/18
_nottingham_internal_self_validation_user pcxav1
_nottingham_internal_validation_date ?
_nottingham_internal_validation_user ?
_nottingham_internal_archive_date ?
_refine_special_details          
'Residual electron density located 0.90A From I1 (2.95 eA-3) and 1.02A From I1 (2.83 eA-3) due to insufficient absorbition correction and heavy iodine atom'
_audit_creation_date             2020-06-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C25 H29 I Si'
_chemical_formula_sum            'C25 H29 I Si'
_chemical_formula_weight         484.47
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C25 H29 I Si'
_chemical_oxdiff_usercomment     
'OAJVLC#15517 SN-840 in fomblin film on a micromount for AJV/DLK'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.3663(4)
_cell_length_b                   17.8142(9)
_cell_length_c                   20.5558(14)
_cell_angle_alpha                90
_cell_angle_beta                 96.860(6)
_cell_angle_gamma                90
_cell_volume                     2314.6(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3889
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.3570
_cell_measurement_theta_min      4.9460
_shelx_estimated_absorpt_T_max   0.499
_shelx_estimated_absorpt_T_min   0.073
_exptl_absorpt_coefficient_mu    11.395
_exptl_absorpt_correction_T_max  0.539
_exptl_absorpt_correction_T_min  0.090
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             984
_exptl_crystal_recrystallization_method 'Recrystallised from diethyl ether'
_exptl_crystal_size_max          0.4809
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.0708
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9764
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.502
_diffrn_reflns_theta_min         3.293
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9947
_diffrn_measured_fraction_theta_max 0.9569
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   56.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000    0.0000 34

#__ type_ start__ end____ width___ exp.time_
  2 omega   74.00  128.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -77.0000  -30.0000 54

#__ type_ start__ end____ width___ exp.time_
  3 omega   38.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000   90.0000 52

#__ type_ start__ end____ width___ exp.time_
  4 omega   39.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -45.0000   60.0000 59

#__ type_ start__ end____ width___ exp.time_
  5 omega   36.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322 -125.0000   30.0000 80

#__ type_ start__ end____ width___ exp.time_
  6 omega   17.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.2215  -99.0000  -30.0000 38

#__ type_ start__ end____ width___ exp.time_
  7 omega  -34.00    6.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -30.0000 40

#__ type_ start__ end____ width___ exp.time_
  8 omega  -48.00   32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   90.0000 80

#__ type_ start__ end____ width___ exp.time_
  9 omega -105.00  -77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000 -120.0000   86.8067 28

#__ type_ start__ end____ width___ exp.time_
 10 omega   70.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3777 -125.0000 -150.0000 28

#__ type_ start__ end____ width___ exp.time_
 11 omega    9.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3777  -99.0000 -180.0000 44

#__ type_ start__ end____ width___ exp.time_
 12 omega  138.00  165.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  125.0000   60.0000 27

#__ type_ start__ end____ width___ exp.time_
 13 omega   49.00   75.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 14 omega   35.00   76.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000 -150.0000 41

#__ type_ start__ end____ width___ exp.time_
 15 omega   29.00  106.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -15.0000 -120.0000 77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      0.0409552000
_diffrn_orient_matrix_UB_12      -0.0850241000
_diffrn_orient_matrix_UB_13      -0.0031750000
_diffrn_orient_matrix_UB_21      -0.0826238000
_diffrn_orient_matrix_UB_22      0.0001573000
_diffrn_orient_matrix_UB_23      -0.0735312000
_diffrn_orient_matrix_UB_31      0.2257795000
_diffrn_orient_matrix_UB_32      0.0155478000
_diffrn_orient_matrix_UB_33      -0.0166862000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3951
_reflns_number_total             4520
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         3.025
_refine_diff_density_min         -1.494
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4520
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0580
_refine_ls_restrained_S_all      1.054
_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)+(0.0616P)²+18.4310P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1524
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18), C19(H19)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.87872(6) 0.36161(2) 0.45429(2) 0.02320(15) Uani 1 1 d . . . . .
Si1 Si 0.4882(3) 0.10172(9) 0.65045(9) 0.0258(4) Uani 1 1 d . . . . .
C1 C 0.7375(10) 0.2835(3) 0.5137(3) 0.0201(12) Uani 1 1 d . . . . .
C2 C 0.7183(9) 0.3030(3) 0.5784(3) 0.0195(11) Uani 1 1 d . . . . .
C3 C 0.6395(10) 0.2481(3) 0.6184(3) 0.0216(12) Uani 1 1 d . . . . .
H3 H 0.625940 0.260260 0.662723 0.026 Uiso 1 1 calc R U . . .
C4 C 0.5805(10) 0.1763(3) 0.5952(3) 0.0230(12) Uani 1 1 d . . . . .
C5 C 0.5997(10) 0.1611(3) 0.5300(3) 0.0231(12) Uani 1 1 d . . . . .
H5 H 0.557027 0.113120 0.513035 0.028 Uiso 1 1 calc R U . . .
C6 C 0.6795(10) 0.2133(3) 0.4878(3) 0.0212(12) Uani 1 1 d . . . . .
C7 C 0.7699(10) 0.3787(3) 0.6069(3) 0.0217(12) Uani 1 1 d . . . . .
C8 C 0.6240(10) 0.4372(3) 0.5961(3) 0.0212(12) Uani 1 1 d . . . . .
C9 C 0.6722(12) 0.5070(4) 0.6245(3) 0.0288(14) Uani 1 1 d . . . . .
H9 H 0.572384 0.546698 0.617859 0.035 Uiso 1 1 calc R U . . .
C10 C 0.8652(12) 0.5192(4) 0.6623(3) 0.0320(15) Uani 1 1 d . . . . .
H10 H 0.897435 0.567040 0.681267 0.038 Uiso 1 1 calc R U . . .
C11 C 1.0098(12) 0.4613(4) 0.6722(3) 0.0311(15) Uani 1 1 d . . . . .
H11 H 1.141702 0.469872 0.697937 0.037 Uiso 1 1 calc R U . . .
C12 C 0.9651(11) 0.3902(4) 0.6448(3) 0.0262(13) Uani 1 1 d . . . . .
C13 C 0.4182(10) 0.4260(4) 0.5518(3) 0.0276(13) Uani 1 1 d . . . . .
H13A H 0.444012 0.431330 0.505953 0.041 Uiso 1 1 calc R U . . .
H13B H 0.315146 0.463763 0.562021 0.041 Uiso 1 1 calc R U . . .
H13C H 0.362619 0.375714 0.558724 0.041 Uiso 1 1 calc R U . . .
C14 C 1.1199(11) 0.3270(4) 0.6594(4) 0.0358(16) Uani 1 1 d . . . . .
H14A H 1.073495 0.294944 0.693750 0.054 Uiso 1 1 calc R U . . .
H14B H 1.260113 0.347584 0.674441 0.054 Uiso 1 1 calc R U . . .
H14C H 1.127095 0.297244 0.619671 0.054 Uiso 1 1 calc R U . . .
C15 C 0.6958(10) 0.1913(3) 0.4186(3) 0.0220(12) Uani 1 1 d . . . . .
C16 C 0.8646(11) 0.1460(3) 0.4043(3) 0.0256(13) Uani 1 1 d . . . . .
C17 C 0.8747(13) 0.1228(4) 0.3401(4) 0.0332(15) Uani 1 1 d . . . . .
H17 H 0.990965 0.093234 0.330098 0.040 Uiso 1 1 calc R U . . .
C18 C 0.7178(13) 0.1422(4) 0.2908(4) 0.0335(16) Uani 1 1 d . . . . .
H18 H 0.723927 0.125279 0.247205 0.040 Uiso 1 1 calc R U . . .
C19 C 0.5514(12) 0.1866(4) 0.3055(3) 0.0322(15) Uani 1 1 d . . . . .
H19 H 0.443903 0.199909 0.271333 0.039 Uiso 1 1 calc R U . . .
C20 C 0.5367(10) 0.2122(3) 0.3683(3) 0.0235(12) Uani 1 1 d . . . . .
C21 C 1.0348(13) 0.1228(4) 0.4583(4) 0.0376(17) Uani 1 1 d . . . . .
H21A H 1.072234 0.165620 0.487219 0.056 Uiso 1 1 calc R U . . .
H21B H 1.160228 0.105945 0.438953 0.056 Uiso 1 1 calc R U . . .
H21C H 0.982192 0.081659 0.483565 0.056 Uiso 1 1 calc R U . . .
C22 C 0.3574(11) 0.2621(4) 0.3818(4) 0.0317(15) Uani 1 1 d . . . . .
H22A H 0.313281 0.249325 0.424510 0.048 Uiso 1 1 calc R U . . .
H22B H 0.238105 0.255096 0.347555 0.048 Uiso 1 1 calc R U . . .
H22C H 0.403559 0.314627 0.382157 0.048 Uiso 1 1 calc R U . . .
C23 C 0.1964(13) 0.1074(5) 0.6534(5) 0.045(2) Uani 1 1 d . . . . .
H23A H 0.163073 0.153543 0.676028 0.068 Uiso 1 1 calc R U . . .
H23B H 0.150065 0.063846 0.677156 0.068 Uiso 1 1 calc R U . . .
H23C H 0.123113 0.107714 0.608726 0.068 Uiso 1 1 calc R U . . .
C24 C 0.6305(15) 0.1136(5) 0.7346(4) 0.045(2) Uani 1 1 d . . . . .
H24A H 0.783147 0.108589 0.733072 0.068 Uiso 1 1 calc R U . . .
H24B H 0.583252 0.075001 0.763568 0.068 Uiso 1 1 calc R U . . .
H24C H 0.599882 0.163411 0.751359 0.068 Uiso 1 1 calc R U . . .
C25 C 0.5580(18) 0.0090(4) 0.6162(5) 0.059(3) Uani 1 1 d . . . . .
H25A H 0.531497 -0.030987 0.646961 0.088 Uiso 1 1 calc R U . . .
H25B H 0.707854 0.008903 0.609606 0.088 Uiso 1 1 calc R U . . .
H25C H 0.471095 0.000538 0.574230 0.088 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C1 2.121(6) . ?
Si1 C4 1.887(6) . ?
Si1 C23 1.869(8) . ?
Si1 C24 1.866(8) . ?
Si1 C25 1.869(8) . ?
C1 C2 1.395(9) . ?
C1 C6 1.392(8) . ?
C2 C3 1.407(8) . ?
C2 C7 1.492(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.401(9) . ?
C4 C5 1.388(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.407(9) . ?
C6 C15 1.492(8) . ?
C7 C8 1.395(9) . ?
C7 C12 1.401(9) . ?
C8 C9 1.392(9) . ?
C8 C13 1.517(9) . ?
C9 H9 0.9500 . ?
C9 C10 1.391(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.380(11) . ?
C11 H11 0.9500 . ?
C11 C12 1.401(9) . ?
C12 C14 1.503(10) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.403(9) . ?
C15 C20 1.407(9) . ?
C16 C17 1.392(10) . ?
C16 C21 1.513(10) . ?
C17 H17 0.9500 . ?
C17 C18 1.379(11) . ?
C18 H18 0.9500 . ?
C18 C19 1.384(11) . ?
C19 H19 0.9500 . ?
C19 C20 1.384(10) . ?
C20 C22 1.499(9) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C23 Si1 C4 111.4(3) . . ?
C23 Si1 C25 110.0(5) . . ?
C24 Si1 C4 109.0(3) . . ?
C24 Si1 C23 109.7(4) . . ?
C24 Si1 C25 109.7(5) . . ?
C25 Si1 C4 106.9(3) . . ?
C2 C1 I1 118.5(4) . . ?
C6 C1 I1 118.8(4) . . ?
C6 C1 C2 122.6(5) . . ?
C1 C2 C3 117.6(5) . . ?
C1 C2 C7 124.0(5) . . ?
C3 C2 C7 118.4(5) . . ?
C2 C3 H3 118.8 . . ?
C4 C3 C2 122.3(6) . . ?
C4 C3 H3 118.8 . . ?
C3 C4 Si1 121.9(5) . . ?
C5 C4 Si1 120.9(5) . . ?
C5 C4 C3 117.2(6) . . ?
C4 C5 H5 118.4 . . ?
C4 C5 C6 123.1(6) . . ?
C6 C5 H5 118.4 . . ?
C1 C6 C5 117.2(6) . . ?
C1 C6 C15 123.7(5) . . ?
C5 C6 C15 119.1(5) . . ?
C8 C7 C2 120.1(6) . . ?
C8 C7 C12 120.6(6) . . ?
C12 C7 C2 119.3(6) . . ?
C7 C8 C13 120.5(5) . . ?
C9 C8 C7 119.4(6) . . ?
C9 C8 C13 120.0(6) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 C8 120.6(6) . . ?
C10 C9 H9 119.7 . . ?
C9 C10 H10 120.2 . . ?
C11 C10 C9 119.7(6) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 119.5 . . ?
C10 C11 C12 121.1(7) . . ?
C12 C11 H11 119.5 . . ?
C7 C12 C14 121.2(6) . . ?
C11 C12 C7 118.7(6) . . ?
C11 C12 C14 120.0(6) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C6 119.5(6) . . ?
C16 C15 C20 120.0(6) . . ?
C20 C15 C6 120.3(6) . . ?
C15 C16 C21 120.2(6) . . ?
C17 C16 C15 119.6(6) . . ?
C17 C16 C21 120.2(6) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 C16 120.7(7) . . ?
C18 C17 H17 119.7 . . ?
C17 C18 H18 120.4 . . ?
C17 C18 C19 119.3(7) . . ?
C19 C18 H18 120.4 . . ?
C18 C19 H19 119.0 . . ?
C20 C19 C18 122.1(7) . . ?
C20 C19 H19 119.0 . . ?
C15 C20 C22 121.2(6) . . ?
C19 C20 C15 118.4(6) . . ?
C19 C20 C22 120.4(6) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C23 H23A 109.5 . . ?
Si1 C23 H23B 109.5 . . ?
Si1 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si1 C24 H24A 109.5 . . ?
Si1 C24 H24B 109.5 . . ?
Si1 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si1 C25 H25A 109.5 . . ?
Si1 C25 H25B 109.5 . . ?
Si1 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
I1 C1 C2 C3 -175.1(4) . . . . ?
I1 C1 C2 C7 6.8(8) . . . . ?
I1 C1 C6 C5 175.7(4) . . . . ?
I1 C1 C6 C15 -4.8(8) . . . . ?
Si1 C4 C5 C6 -176.1(5) . . . . ?
C1 C2 C3 C4 -0.3(9) . . . . ?
C1 C2 C7 C8 80.9(8) . . . . ?
C1 C2 C7 C12 -99.6(8) . . . . ?
C1 C6 C15 C16 101.9(7) . . . . ?
C1 C6 C15 C20 -81.8(8) . . . . ?
C2 C1 C6 C5 -0.3(9) . . . . ?
C2 C1 C6 C15 179.2(6) . . . . ?
C2 C3 C4 Si1 176.8(5) . . . . ?
C2 C3 C4 C5 -0.9(9) . . . . ?
C2 C7 C8 C9 178.3(6) . . . . ?
C2 C7 C8 C13 -4.2(9) . . . . ?
C2 C7 C12 C11 -178.9(6) . . . . ?
C2 C7 C12 C14 -2.3(9) . . . . ?
C3 C2 C7 C8 -97.2(7) . . . . ?
C3 C2 C7 C12 82.3(8) . . . . ?
C3 C4 C5 C6 1.6(10) . . . . ?
C4 C5 C6 C1 -1.1(10) . . . . ?
C4 C5 C6 C15 179.5(6) . . . . ?
C5 C6 C15 C16 -78.7(8) . . . . ?
C5 C6 C15 C20 97.6(7) . . . . ?
C6 C1 C2 C3 0.9(9) . . . . ?
C6 C1 C2 C7 -177.2(6) . . . . ?
C6 C15 C16 C17 177.2(6) . . . . ?
C6 C15 C16 C21 -3.0(9) . . . . ?
C6 C15 C20 C19 -176.0(6) . . . . ?
C6 C15 C20 C22 5.2(9) . . . . ?
C7 C2 C3 C4 177.9(6) . . . . ?
C7 C8 C9 C10 1.0(10) . . . . ?
C8 C7 C12 C11 0.5(9) . . . . ?
C8 C7 C12 C14 177.2(6) . . . . ?
C8 C9 C10 C11 -0.4(10) . . . . ?
C9 C10 C11 C12 -0.2(11) . . . . ?
C10 C11 C12 C7 0.2(10) . . . . ?
C10 C11 C12 C14 -176.5(7) . . . . ?
C12 C7 C8 C9 -1.1(9) . . . . ?
C12 C7 C8 C13 176.4(6) . . . . ?
C13 C8 C9 C10 -176.5(6) . . . . ?
C15 C16 C17 C18 -1.7(10) . . . . ?
C16 C15 C20 C19 0.4(9) . . . . ?
C16 C15 C20 C22 -178.4(6) . . . . ?
C16 C17 C18 C19 1.4(11) . . . . ?
C17 C18 C19 C20 -0.1(11) . . . . ?
C18 C19 C20 C15 -0.7(10) . . . . ?
C18 C19 C20 C22 178.1(6) . . . . ?
C20 C15 C16 C17 0.8(9) . . . . ?
C20 C15 C16 C21 -179.4(6) . . . . ?
C21 C16 C17 C18 178.5(7) . . . . ?
C23 Si1 C4 C3 88.1(6) . . . . ?
C23 Si1 C4 C5 -94.2(6) . . . . ?
C24 Si1 C4 C3 -33.1(7) . . . . ?
C24 Si1 C4 C5 144.6(6) . . . . ?
C25 Si1 C4 C3 -151.7(6) . . . . ?
C25 Si1 C4 C5 26.0(7) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4 1 -4 0.2096 4.0297 0.6266 -4.3404 0.1255 -0.0137 0.9920
0 -2 13 0.0643 -0.3463 -1.5560 13.2153 0.0762 -0.9434 -0.3229
4 4 -5 0.2087 3.6767 4.4898 -4.5427 -0.2167 0.0309 0.9757
0 -1 13 0.0612 0.4820 -1.1818 12.9059 0.0792 -0.9890 -0.1249
-4 1 4 0.2437 -4.0420 0.5918 4.1722 -0.2291 0.0273 -0.9730
0 11 -2 0.1065 0.1996 11.4437 -1.9116 -0.9587 0.1259 0.2549
0 -11 2 0.1113 0.1479 -11.4767 1.5503 0.9769 -0.1280 -0.1709
0 1 -13 0.0084 -0.2259 1.3037 -13.0598 -0.0786 0.9792 0.1872

_olex2_date_sample_data_collection 2016-01-27
_olex2_date_sample_submission    2016-01-25
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_original_sample_id OAJVLC
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_kewjmb
_database_code_depnum_ccdc_archive 'CCDC 2045220'
loop_
_audit_author_name
_audit_author_address
'Stephen P. Argent'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2020-11-18 deposited with the CCDC.	2020-12-04 downloaded from the CCDC.
;
_nottingham_internal_coll_name   KEWJMB
_nottingham_internal_coll_number 16697
_nottingham_internal_coll_client KEW/JM
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '240.00, 60.00'
_nottingham_internal_coll_frame_width 1.00
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   22/11/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017-09'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 25/11/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 06/12/16
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 06/12/16
_nottingham_internal_refinement_user pczwl/pcxav1
_nottingham_internal_self_archive_date 06/12/16
_nottingham_internal_self_validation_date 06/12/16
_nottingham_internal_self_validation_user pcxav1
_nottingham_internal_validation_date ?
_nottingham_internal_validation_user ?
_nottingham_internal_archive_date ?
_refine_special_details          
;
 Disordered co-crystallised solvent molecule (iso-hexane) was
 constrained with all carbons (C45-C50) having similar bonds and
 angles to each other (SAME). Rigid bond restraints (RIGU) were
 applied to C45-C50.
;
_audit_creation_date             2020-06-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H40 Cl2 Li2, 0.5(C6 H14)'
_chemical_formula_sum            'C47 H47 Cl2 Li2'
_chemical_formula_weight         696.62
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C22 H20 Cl Li'
_chemical_oxdiff_usercomment     
'KEWJMB#16697 SN-1096 IN FOMBLIN FILM ON MICROMOUNT FOR KEW/JM'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.1125(11)
_cell_length_b                   16.8343(14)
_cell_length_c                   19.6420(14)
_cell_angle_alpha                90
_cell_angle_beta                 103.471(9)
_cell_angle_gamma                90
_cell_volume                     3894.9(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3993
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.2590
_cell_measurement_theta_min      3.4720
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.720
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 -9 4 0.0443
3 -5 -11 0.0901
5 -7 -6 0.0705
-5 7 6 0.0391
7 2 -6 0.0564
2 0 11 0.0965
-6 6 -2 0.0779
3 -10 -3 0.0684
6 7 -4 0.0527
-6 5 8 0.0214

_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.1
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.9935 -9.0045 4.0007 0.3441 0.9961 -0.0293
3.0081 -5.0106 -11.0022 -0.0231 -0.0220 -0.9942
5.0081 -7.0026 -6.0019 -0.4918 0.2142 -0.7987
-5.0081 7.0026 6.0019 0.4918 -0.2142 0.7987
7.0003 2.0027 -6.0017 -0.6150 -0.5660 -0.4475
1.9962 0.0158 11.0011 -0.6704 0.2510 0.6719
-6.0045 5.9914 -1.9990 0.9087 -0.3327 0.2569
3.0097 -10.0025 -3.0015 -0.3994 0.6055 -0.6934
5.9953 7.0052 -4.0009 -0.4968 -0.8710 -0.0788
-6.0071 5.0031 8.0022 0.5119 0.0356 0.8620

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20656
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.806
_diffrn_reflns_theta_min         3.500
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  34.00   1.00   60.00    --  -38.50  38.00  30.00   84
  2  ω    -50.00  34.00   1.00   60.00    --  -38.50  38.00 150.00   84
  3  ω    -50.00  34.00   1.00   60.00    --  -38.50  38.00 -90.00   84
  4  ω      1.00  83.00   1.00   60.00    --   43.32 -99.00  60.00   82
  5  ω     23.00  98.00   1.00   60.00    --   43.32-125.00 -90.00   75
  6  ω     35.00  98.00   1.00  240.00    --  106.13 -45.00  90.00   63
  7  ω     25.00 109.00   1.00  240.00    --  106.13 -95.00  30.00   84
  8  ω     57.00  91.00   1.00  240.00    --  106.13 -30.00   0.00   34
  9  ω     93.00 172.00   1.00  240.00    --  106.13  30.00-150.00   79
 10  ω     99.00 172.00   1.00  240.00    --  106.13 125.00-120.00   73
 11  ω     95.00 156.00   1.00  240.00    --  106.13 125.00  30.00   61
 12  ω     32.00  57.00   1.00  240.00    --  106.13 -30.00 -90.00   25
 13  ω     46.00  92.00   1.00  240.00    --  106.13 -45.00 150.00   46
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1246974000
_diffrn_orient_matrix_UB_12      0.0139070000
_diffrn_orient_matrix_UB_13      -0.0383290000
_diffrn_orient_matrix_UB_21      -0.0333321000
_diffrn_orient_matrix_UB_22      -0.0792592000
_diffrn_orient_matrix_UB_23      0.0289791000
_diffrn_orient_matrix_UB_31      -0.0208515000
_diffrn_orient_matrix_UB_32      0.0436083000
_diffrn_orient_matrix_UB_33      0.0647998000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4536
_reflns_number_total             7768
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         7768
_refine_ls_number_restraints     80
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0705
_refine_ls_restrained_S_all      1.037
_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)+(0.0662P)²+2.6019P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1945
_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
 C46-C45 \\sim C50-C48 \\sim C48-C49 \\sim C46-C47 \\sim C48-C47
 with sigma of 0.02
 C45-C47 \\sim C46-C48 \\sim C47-C49 \\sim C47-C50 \\sim C49-C50
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C45, C46, C47, C48, C49, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C45(0.5) H45a(0.5) H45b(0.5) H45c(0.5) C46(0.5) H46a(0.5)
 H46b(0.5) C47(0.5) H47a(0.5) H47b(0.5) C48(0.5) H48(0.5) C49(0.5) H49a(0.5)
 H49b(0.5) H49c(0.5) C50(0.5) H50a(0.5) H50b(0.5) H50c(0.5)
6.a Ternary CH refined with riding coordinates:
 C48(H48)
6.b Secondary CH2 refined with riding coordinates:
 C46(H46a,H46b), C47(H47a,H47b)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18), C19(H19),
 C25(H25), C27(H27), C31(H31), C32(H32), C33(H33), C39(H39), C40(H40), C41(H41)
6.d Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C21(H21a,H21b,H21c), C22(H22a,H22b,
 H22c), C35(H35a,H35b,H35c), C36(H36a,H36b,H36c), C43(H43a,H43b,H43c), C44(H44a,
 H44b,H44c), C45(H45a,H45b,H45c), C49(H49a,H49b,H49c), C50(H50a,H50b,H50c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.29190(12) 0.22473(8) 0.44144(6) 0.0924(4) Uani 1 1 d . . . . .
Cl2 Cl 0.25819(11) 0.81793(7) 0.02811(5) 0.0719(3) Uani 1 1 d . . . . .
C1 C 0.2936(3) 0.41846(19) 0.27828(15) 0.0375(7) Uani 1 1 d . . . . .
C2 C 0.3795(3) 0.4116(2) 0.34057(16) 0.0412(8) Uani 1 1 d . . . . .
C3 C 0.3803(4) 0.3524(2) 0.39027(17) 0.0551(10) Uani 1 1 d . . . . .
H3 H 0.439948 0.349544 0.431300 0.066 Uiso 1 1 calc R U . . .
C4 C 0.2928(4) 0.2981(2) 0.37871(19) 0.0557(10) Uani 1 1 d . . . . .
C5 C 0.2061(3) 0.3003(2) 0.31879(18) 0.0518(9) Uani 1 1 d . . . . .
H5 H 0.146291 0.262493 0.311523 0.062 Uiso 1 1 calc R U . . .
C6 C 0.2086(3) 0.3591(2) 0.26943(17) 0.0434(8) Uani 1 1 d . . . . .
C7 C 0.4790(3) 0.4683(2) 0.35350(17) 0.0491(9) Uani 1 1 d . . . . .
C8 C 0.4765(4) 0.5398(3) 0.39047(19) 0.0637(11) Uani 1 1 d . . . . .
C9 C 0.5709(5) 0.5911(3) 0.4011(2) 0.0798(15) Uani 1 1 d . . . . .
H9 H 0.570369 0.639515 0.425864 0.096 Uiso 1 1 calc R U . . .
C10 C 0.6637(5) 0.5710(4) 0.3757(3) 0.0885(16) Uani 1 1 d . . . . .
H10 H 0.726963 0.605952 0.383057 0.106 Uiso 1 1 calc R U . . .
C11 C 0.6664(4) 0.5023(3) 0.3401(3) 0.0840(15) Uani 1 1 d . . . . .
H11 H 0.731747 0.489429 0.323382 0.101 Uiso 1 1 calc R U . . .
C12 C 0.5740(3) 0.4499(3) 0.3279(2) 0.0597(10) Uani 1 1 d . . . . .
C13 C 0.3770(5) 0.5574(3) 0.4211(3) 0.0890(17) Uani 1 1 d . . . . .
H13A H 0.306723 0.552266 0.384698 0.133 Uiso 1 1 calc R U . . .
H13B H 0.383404 0.611630 0.439702 0.133 Uiso 1 1 calc R U . . .
H13C H 0.375833 0.519741 0.458995 0.133 Uiso 1 1 calc R U . . .
C14 C 0.5809(4) 0.3732(3) 0.2901(3) 0.0739(13) Uani 1 1 d . . . . .
H14A H 0.569452 0.328611 0.319778 0.111 Uiso 1 1 calc R U . . .
H14B H 0.655771 0.368691 0.279466 0.111 Uiso 1 1 calc R U . . .
H14C H 0.521976 0.372311 0.246439 0.111 Uiso 1 1 calc R U . . .
C15 C 0.1175(3) 0.3576(2) 0.20274(17) 0.0438(8) Uani 1 1 d . . . . .
C16 C 0.1455(3) 0.3314(2) 0.14057(17) 0.0503(9) Uani 1 1 d . . . . .
C17 C 0.0615(4) 0.3317(3) 0.07840(19) 0.0599(11) Uani 1 1 d . . . . .
H17 H 0.079678 0.313990 0.036408 0.072 Uiso 1 1 calc R U . . .
C18 C -0.0472(4) 0.3571(3) 0.0766(2) 0.0663(12) Uani 1 1 d . . . . .
H18 H -0.103021 0.357630 0.033678 0.080 Uiso 1 1 calc R U . . .
C19 C -0.0743(3) 0.3817(3) 0.1372(2) 0.0675(12) Uani 1 1 d . . . . .
H19 H -0.149211 0.399660 0.135561 0.081 Uiso 1 1 calc R U . . .
C20 C 0.0054(3) 0.3811(2) 0.2014(2) 0.0525(9) Uani 1 1 d . . . . .
C21 C 0.2624(4) 0.2999(3) 0.14154(19) 0.0632(11) Uani 1 1 d . . . . .
H21A H 0.317119 0.343714 0.149874 0.095 Uiso 1 1 calc R U . . .
H21B H 0.262098 0.274964 0.096390 0.095 Uiso 1 1 calc R U . . .
H21C H 0.283992 0.260412 0.178972 0.095 Uiso 1 1 calc R U . . .
C22 C -0.0291(4) 0.4023(3) 0.2678(2) 0.0674(12) Uani 1 1 d . . . . .
H22A H -0.030259 0.354262 0.295740 0.101 Uiso 1 1 calc R U . . .
H22B H -0.104939 0.426263 0.256299 0.101 Uiso 1 1 calc R U . . .
H22C H 0.025387 0.440333 0.294628 0.101 Uiso 1 1 calc R U . . .
C23 C 0.2763(3) 0.59530(19) 0.16483(15) 0.0348(7) Uani 1 1 d . . . . .
C24 C 0.3484(3) 0.6073(2) 0.11825(15) 0.0381(7) Uani 1 1 d . . . . .
C25 C 0.3440(3) 0.6752(2) 0.07681(16) 0.0442(8) Uani 1 1 d . . . . .
H25 H 0.395055 0.681498 0.047090 0.053 Uiso 1 1 calc R U . . .
C26 C 0.2648(3) 0.7328(2) 0.07961(16) 0.0464(8) Uani 1 1 d . . . . .
C27 C 0.1911(3) 0.7252(2) 0.12370(16) 0.0435(8) Uani 1 1 d . . . . .
H27 H 0.136751 0.765362 0.125558 0.052 Uiso 1 1 calc R U . . .
C28 C 0.1984(3) 0.65762(18) 0.16509(15) 0.0346(7) Uani 1 1 d . . . . .
C29 C 0.4342(3) 0.5449(2) 0.11350(16) 0.0384(7) Uani 1 1 d . . . . .
C30 C 0.5466(3) 0.5535(2) 0.15128(19) 0.0505(9) Uani 1 1 d . . . . .
C31 C 0.6239(3) 0.4939(3) 0.1464(2) 0.0641(11) Uani 1 1 d . . . . .
H31 H 0.700420 0.498750 0.172063 0.077 Uiso 1 1 calc R U . . .
C32 C 0.5913(3) 0.4278(3) 0.1050(2) 0.0624(11) Uani 1 1 d . . . . .
H32 H 0.645175 0.387536 0.102535 0.075 Uiso 1 1 calc R U . . .
C33 C 0.4817(3) 0.4202(2) 0.0677(2) 0.0530(9) Uani 1 1 d . . . . .
H33 H 0.459904 0.374750 0.039108 0.064 Uiso 1 1 calc R U . . .
C34 C 0.4017(3) 0.4783(2) 0.07104(17) 0.0440(8) Uani 1 1 d . . . . .
C35 C 0.5835(3) 0.6271(3) 0.1958(2) 0.0677(12) Uani 1 1 d . . . . .
H35A H 0.574095 0.674176 0.165562 0.102 Uiso 1 1 calc R U . . .
H35B H 0.663465 0.621851 0.220290 0.102 Uiso 1 1 calc R U . . .
H35C H 0.536802 0.632748 0.230043 0.102 Uiso 1 1 calc R U . . .
C36 C 0.2811(3) 0.4707(2) 0.02742(19) 0.0551(10) Uani 1 1 d . . . . .
H36A H 0.229344 0.461911 0.058332 0.083 Uiso 1 1 calc R U . . .
H36B H 0.276379 0.425638 -0.004740 0.083 Uiso 1 1 calc R U . . .
H36C H 0.259614 0.519553 0.000487 0.083 Uiso 1 1 calc R U . . .
C37 C 0.1162(3) 0.64951(19) 0.21137(15) 0.0360(7) Uani 1 1 d . . . . .
C38 C 0.0112(3) 0.6132(2) 0.18549(18) 0.0453(8) Uani 1 1 d . . . . .
C39 C -0.0645(3) 0.6049(3) 0.2295(2) 0.0617(11) Uani 1 1 d . . . . .
H39 H -0.136123 0.580286 0.212287 0.074 Uiso 1 1 calc R U . . .
C40 C -0.0353(4) 0.6325(3) 0.2975(2) 0.0634(11) Uani 1 1 d . . . . .
H40 H -0.086817 0.626495 0.326894 0.076 Uiso 1 1 calc R U . . .
C41 C 0.0671(4) 0.6684(2) 0.3227(2) 0.0590(11) Uani 1 1 d . . . . .
H41 H 0.085646 0.687292 0.369593 0.071 Uiso 1 1 calc R U . . .
C42 C 0.1454(3) 0.6779(2) 0.28082(17) 0.0477(9) Uani 1 1 d . . . . .
C43 C -0.0226(4) 0.5851(3) 0.1105(2) 0.0701(12) Uani 1 1 d . . . . .
H43A H -0.030457 0.631000 0.078997 0.105 Uiso 1 1 calc R U . . .
H43B H -0.095116 0.556785 0.102706 0.105 Uiso 1 1 calc R U . . .
H43C H 0.035942 0.549354 0.101029 0.105 Uiso 1 1 calc R U . . .
C44 C 0.2552(4) 0.7202(3) 0.3084(2) 0.0708(13) Uani 1 1 d . . . . .
H44A H 0.318166 0.686833 0.301860 0.106 Uiso 1 1 calc R U . . .
H44B H 0.263967 0.731101 0.358435 0.106 Uiso 1 1 calc R U . . .
H44C H 0.255295 0.770348 0.283164 0.106 Uiso 1 1 calc R U . . .
Li1 Li 0.3835(5) 0.5053(4) 0.2282(3) 0.0484(14) Uani 1 1 d . . . . .
Li2 Li 0.1877(5) 0.5048(4) 0.2107(3) 0.0466(14) Uani 1 1 d . . . . .
C45 C -0.0953(12) 0.6259(8) 0.5322(6) 0.110(4) Uani 0.5 1 d D U P A -1
H45A H -0.042431 0.630034 0.578132 0.166 Uiso 0.5 1 calc R U P A -1
H45B H -0.168314 0.605333 0.537891 0.166 Uiso 0.5 1 calc R U P A -1
H45C H -0.106439 0.678461 0.510268 0.166 Uiso 0.5 1 calc R U P A -1
C46 C -0.0491(12) 0.5724(7) 0.4883(6) 0.113(3) Uani 0.5 1 d D U P A -1
H46A H 0.018625 0.597578 0.477442 0.136 Uiso 0.5 1 calc R U P A -1
H46B H -0.106093 0.565472 0.443507 0.136 Uiso 0.5 1 calc R U P A -1
C47 C -0.0159(11) 0.4914(6) 0.5192(5) 0.104(3) Uani 0.5 1 d D U P A -1
H47A H -0.081830 0.465121 0.531395 0.125 Uiso 0.5 1 calc R U P A -1
H47B H 0.045467 0.496211 0.562211 0.125 Uiso 0.5 1 calc R U P A -1
C48 C 0.0257(9) 0.4421(6) 0.4631(6) 0.098(3) Uani 0.5 1 d D U P A -1
H48 H -0.035356 0.440099 0.418972 0.118 Uiso 0.5 1 calc R U P A -1
C49 C 0.0528(8) 0.3580(5) 0.4911(5) 0.067(2) Uani 0.5 1 d D U P A -1
H49A H 0.117483 0.359491 0.531708 0.100 Uiso 0.5 1 calc R U P A -1
H49B H 0.071707 0.324682 0.454460 0.100 Uiso 0.5 1 calc R U P A -1
H49C H -0.013421 0.335773 0.505013 0.100 Uiso 0.5 1 calc R U P A -1
C50 C 0.1286(8) 0.4807(7) 0.4489(6) 0.101(3) Uani 0.5 1 d D U P A -1
H50A H 0.183981 0.489951 0.493219 0.151 Uiso 0.5 1 calc R U P A -1
H50B H 0.107407 0.531525 0.425124 0.151 Uiso 0.5 1 calc R U P A -1
H50C H 0.162074 0.446034 0.419017 0.151 Uiso 0.5 1 calc R U 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
Cl1 C4 1.747(4) . ?
Cl2 C26 1.745(3) . ?
C1 C2 1.414(5) . ?
C1 C6 1.417(5) . ?
C1 Li1 2.188(7) . ?
C1 Li2 2.174(6) . ?
C2 C3 1.394(5) . ?
C2 C7 1.512(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.377(6) . ?
C4 C5 1.383(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.391(5) . ?
C6 C15 1.503(5) . ?
C7 C8 1.409(5) . ?
C7 C12 1.394(5) . ?
C7 Li1 2.540(7) . ?
C8 C9 1.409(7) . ?
C8 C13 1.496(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.375(7) . ?
C10 H10 0.9500 . ?
C10 C11 1.356(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.401(6) . ?
C12 C14 1.501(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.412(5) . ?
C15 C20 1.408(5) . ?
C15 Li2 2.612(7) . ?
C16 C17 1.395(5) . ?
C16 C21 1.509(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.377(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.370(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.398(5) . ?
C20 C22 1.502(5) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.420(4) . ?
C23 C28 1.411(4) . ?
C23 Li1 2.186(7) . ?
C23 Li2 2.177(6) . ?
C24 C25 1.397(5) . ?
C24 C29 1.495(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.374(5) . ?
C26 C27 1.387(5) . ?
C27 H27 0.9500 . ?
C27 C28 1.389(4) . ?
C28 C37 1.502(4) . ?
C29 C30 1.398(5) . ?
C29 C34 1.399(5) . ?
C29 Li1 2.558(6) . ?
C30 C31 1.391(5) . ?
C30 C35 1.522(5) . ?
C31 H31 0.9500 . ?
C31 C32 1.381(6) . ?
C32 H32 0.9500 . ?
C32 C33 1.365(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.389(5) . ?
C34 C36 1.517(5) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.396(5) . ?
C37 C42 1.410(4) . ?
C37 Li2 2.587(7) . ?
C38 C39 1.405(5) . ?
C38 C43 1.510(5) . ?
C38 Li2 2.766(7) . ?
C39 H39 0.9500 . ?
C39 C40 1.380(6) . ?
C40 H40 0.9500 . ?
C40 C41 1.364(6) . ?
C41 H41 0.9500 . ?
C41 C42 1.402(5) . ?
C42 C44 1.494(5) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C45 C46 1.446(11) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 C47 1.509(12) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C47 C48 1.555(11) . ?
C48 H48 1.0000 . ?
C48 C49 1.526(11) . ?
C48 C50 1.488(11) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 114.6(3) . . ?
C2 C1 Li1 95.8(3) . . ?
C2 C1 Li2 142.5(3) . . ?
C6 C1 Li1 147.1(3) . . ?
C6 C1 Li2 95.0(3) . . ?
Li2 C1 Li1 64.1(2) . . ?
C1 C2 C7 119.4(3) . . ?
C3 C2 C1 123.2(3) . . ?
C3 C2 C7 117.3(3) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 C2 118.7(3) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 Cl1 119.0(3) . . ?
C3 C4 C5 121.7(3) . . ?
C5 C4 Cl1 119.4(3) . . ?
C4 C5 H5 120.8 . . ?
C4 C5 C6 118.5(4) . . ?
C6 C5 H5 120.8 . . ?
C1 C6 C15 118.9(3) . . ?
C5 C6 C1 123.3(3) . . ?
C5 C6 C15 117.7(3) . . ?
C2 C7 Li1 80.0(2) . . ?
C8 C7 C2 120.9(4) . . ?
C8 C7 Li1 103.3(3) . . ?
C12 C7 C2 119.4(3) . . ?
C12 C7 C8 119.6(4) . . ?
C12 C7 Li1 86.2(3) . . ?
C7 C8 C13 119.5(4) . . ?
C9 C8 C7 119.1(4) . . ?
C9 C8 C13 121.4(4) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 120.0(5) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 119.4 . . ?
C11 C10 C9 121.1(5) . . ?
C11 C10 H10 119.4 . . ?
C10 C11 H11 119.6 . . ?
C10 C11 C12 120.7(5) . . ?
C12 C11 H11 119.6 . . ?
C7 C12 C11 119.5(4) . . ?
C7 C12 C14 121.0(4) . . ?
C11 C12 C14 119.5(4) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C15 Li2 76.7(2) . . ?
C16 C15 C6 118.9(3) . . ?
C16 C15 Li2 102.0(3) . . ?
C20 C15 C6 121.3(3) . . ?
C20 C15 C16 119.7(3) . . ?
C20 C15 Li2 91.9(3) . . ?
C15 C16 C21 120.9(3) . . ?
C17 C16 C15 118.9(4) . . ?
C17 C16 C21 120.2(3) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 C16 121.4(4) . . ?
C18 C17 H17 119.3 . . ?
C17 C18 H18 120.2 . . ?
C19 C18 C17 119.5(4) . . ?
C19 C18 H18 120.2 . . ?
C18 C19 H19 119.1 . . ?
C18 C19 C20 121.8(4) . . ?
C20 C19 H19 119.1 . . ?
C15 C20 C22 120.8(3) . . ?
C19 C20 C15 118.6(4) . . ?
C19 C20 C22 120.5(4) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 Li1 95.3(3) . . ?
C24 C23 Li2 143.5(3) . . ?
C28 C23 C24 114.1(3) . . ?
C28 C23 Li1 145.3(3) . . ?
C28 C23 Li2 97.2(3) . . ?
Li2 C23 Li1 64.1(2) . . ?
C23 C24 C29 118.7(3) . . ?
C25 C24 C23 123.1(3) . . ?
C25 C24 C29 118.1(3) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 C24 119.1(3) . . ?
C26 C25 H25 120.4 . . ?
C25 C26 Cl2 119.6(3) . . ?
C25 C26 C27 121.1(3) . . ?
C27 C26 Cl2 119.2(3) . . ?
C26 C27 H27 120.7 . . ?
C26 C27 C28 118.6(3) . . ?
C28 C27 H27 120.7 . . ?
C23 C28 C37 118.2(3) . . ?
C27 C28 C23 123.9(3) . . ?
C27 C28 C37 117.9(3) . . ?
C24 C29 Li1 79.4(2) . . ?
C30 C29 C24 119.9(3) . . ?
C30 C29 C34 120.3(3) . . ?
C30 C29 Li1 87.9(2) . . ?
C34 C29 C24 119.8(3) . . ?
C34 C29 Li1 103.0(3) . . ?
C29 C30 C35 120.6(3) . . ?
C31 C30 C29 118.5(3) . . ?
C31 C30 C35 120.9(3) . . ?
C30 C31 H31 119.4 . . ?
C32 C31 C30 121.2(4) . . ?
C32 C31 H31 119.4 . . ?
C31 C32 H32 120.0 . . ?
C33 C32 C31 120.0(4) . . ?
C33 C32 H32 120.0 . . ?
C32 C33 H33 119.6 . . ?
C32 C33 C34 120.8(4) . . ?
C34 C33 H33 119.6 . . ?
C29 C34 C36 120.3(3) . . ?
C33 C34 C29 119.3(3) . . ?
C33 C34 C36 120.3(3) . . ?
C30 C35 H35A 109.5 . . ?
C30 C35 H35B 109.5 . . ?
C30 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C28 C37 Li2 79.2(2) . . ?
C38 C37 C28 119.7(3) . . ?
C38 C37 C42 120.1(3) . . ?
C38 C37 Li2 82.1(2) . . ?
C42 C37 C28 120.2(3) . . ?
C42 C37 Li2 108.3(3) . . ?
C37 C38 C39 119.3(3) . . ?
C37 C38 C43 120.6(3) . . ?
C37 C38 Li2 67.9(2) . . ?
C39 C38 C43 120.1(4) . . ?
C39 C38 Li2 114.4(3) . . ?
C43 C38 Li2 89.5(3) . . ?
C38 C39 H39 119.8 . . ?
C40 C39 C38 120.3(4) . . ?
C40 C39 H39 119.8 . . ?
C39 C40 H40 119.8 . . ?
C41 C40 C39 120.5(3) . . ?
C41 C40 H40 119.8 . . ?
C40 C41 H41 119.4 . . ?
C40 C41 C42 121.2(4) . . ?
C42 C41 H41 119.4 . . ?
C37 C42 C44 120.9(3) . . ?
C41 C42 C37 118.6(3) . . ?
C41 C42 C44 120.5(3) . . ?
C38 C43 H43A 109.5 . . ?
C38 C43 H43B 109.5 . . ?
C38 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C1 Li1 C7 64.09(19) . . ?
C1 Li1 C29 144.7(3) . . ?
C7 Li1 C29 140.2(3) . . ?
C23 Li1 C1 115.3(3) . . ?
C23 Li1 C7 142.9(3) . . ?
C23 Li1 C29 63.27(18) . . ?
C1 Li2 C15 62.64(19) . . ?
C1 Li2 C23 116.3(3) . . ?
C1 Li2 C37 141.0(3) . . ?
C1 Li2 C38 150.7(3) . . ?
C15 Li2 C38 112.8(2) . . ?
C23 Li2 C15 145.5(3) . . ?
C23 Li2 C37 62.62(19) . . ?
C23 Li2 C38 84.2(2) . . ?
C37 Li2 C15 142.1(3) . . ?
C37 Li2 C38 30.00(12) . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C46 C45 H45A 109.5 . . ?
C46 C45 H45B 109.5 . . ?
C46 C45 H45C 109.5 . . ?
C45 C46 H46A 108.5 . . ?
C45 C46 H46B 108.5 . . ?
C45 C46 C47 115.3(10) . . ?
H46A C46 H46B 107.5 . . ?
C47 C46 H46A 108.5 . . ?
C47 C46 H46B 108.5 . . ?
C46 C47 H47A 110.3 . . ?
C46 C47 H47B 110.3 . . ?
C46 C47 C48 107.3(7) . . ?
H47A C47 H47B 108.5 . . ?
C48 C47 H47A 110.3 . . ?
C48 C47 H47B 110.3 . . ?
C47 C48 H48 109.6 . . ?
C49 C48 C47 108.5(7) . . ?
C49 C48 H48 109.6 . . ?
C50 C48 C47 108.8(8) . . ?
C50 C48 H48 109.6 . . ?
C50 C48 C49 110.7(8) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl1 C4 C5 C6 -179.9(3) . . . . ?
Cl2 C26 C27 C28 -179.1(3) . . . . ?
C1 C2 C3 C4 -0.5(6) . . . . ?
C1 C2 C7 C8 91.9(4) . . . . ?
C1 C2 C7 C12 -87.6(4) . . . . ?
C1 C2 C7 Li1 -7.8(3) . . . . ?
C1 C6 C15 C16 73.2(4) . . . . ?
C1 C6 C15 C20 -107.3(4) . . . . ?
C1 C6 C15 Li2 -23.3(3) . . . . ?
C2 C1 C6 C5 2.4(5) . . . . ?
C2 C1 C6 C15 -175.9(3) . . . . ?
C2 C3 C4 Cl1 -179.0(3) . . . . ?
C2 C3 C4 C5 1.1(6) . . . . ?
C2 C7 C8 C9 -179.8(4) . . . . ?
C2 C7 C8 C13 3.8(6) . . . . ?
C2 C7 C12 C11 -179.7(4) . . . . ?
C2 C7 C12 C14 -2.3(6) . . . . ?
C3 C2 C7 C8 -90.8(4) . . . . ?
C3 C2 C7 C12 89.7(4) . . . . ?
C3 C2 C7 Li1 169.6(3) . . . . ?
C3 C4 C5 C6 0.0(6) . . . . ?
C4 C5 C6 C1 -1.9(6) . . . . ?
C4 C5 C6 C15 176.4(3) . . . . ?
C5 C6 C15 C16 -105.2(4) . . . . ?
C5 C6 C15 C20 74.2(5) . . . . ?
C5 C6 C15 Li2 158.2(3) . . . . ?
C6 C1 C2 C3 -1.2(5) . . . . ?
C6 C1 C2 C7 176.0(3) . . . . ?
C6 C15 C16 C17 -178.6(3) . . . . ?
C6 C15 C16 C21 4.3(5) . . . . ?
C6 C15 C20 C19 177.3(4) . . . . ?
C6 C15 C20 C22 -4.9(6) . . . . ?
C7 C2 C3 C4 -177.8(3) . . . . ?
C7 C8 C9 C10 -0.1(7) . . . . ?
C8 C7 C12 C11 0.9(6) . . . . ?
C8 C7 C12 C14 178.2(4) . . . . ?
C8 C9 C10 C11 0.0(8) . . . . ?
C9 C10 C11 C12 0.5(8) . . . . ?
C10 C11 C12 C7 -1.0(7) . . . . ?
C10 C11 C12 C14 -178.4(5) . . . . ?
C12 C7 C8 C9 -0.3(6) . . . . ?
C12 C7 C8 C13 -176.8(4) . . . . ?
C13 C8 C9 C10 176.3(5) . . . . ?
C15 C16 C17 C18 0.2(6) . . . . ?
C16 C15 C20 C19 -3.3(6) . . . . ?
C16 C15 C20 C22 174.5(4) . . . . ?
C16 C17 C18 C19 -0.9(7) . . . . ?
C17 C18 C19 C20 -0.6(7) . . . . ?
C18 C19 C20 C15 2.6(7) . . . . ?
C18 C19 C20 C22 -175.2(4) . . . . ?
C20 C15 C16 C17 1.9(5) . . . . ?
C20 C15 C16 C21 -175.2(4) . . . . ?
C21 C16 C17 C18 177.3(4) . . . . ?
C23 C24 C25 C26 -1.4(5) . . . . ?
C23 C24 C29 C30 -97.8(4) . . . . ?
C23 C24 C29 C34 82.5(4) . . . . ?
C23 C24 C29 Li1 -16.4(3) . . . . ?
C23 C28 C37 C38 -89.4(4) . . . . ?
C23 C28 C37 C42 90.1(4) . . . . ?
C23 C28 C37 Li2 -15.0(3) . . . . ?
C24 C23 C28 C27 0.2(5) . . . . ?
C24 C23 C28 C37 178.5(3) . . . . ?
C24 C25 C26 Cl2 -180.0(3) . . . . ?
C24 C25 C26 C27 1.2(5) . . . . ?
C24 C29 C30 C31 179.2(3) . . . . ?
C24 C29 C30 C35 -1.7(5) . . . . ?
C24 C29 C34 C33 -179.2(3) . . . . ?
C24 C29 C34 C36 2.6(5) . . . . ?
C25 C24 C29 C30 81.7(4) . . . . ?
C25 C24 C29 C34 -98.0(4) . . . . ?
C25 C24 C29 Li1 163.0(3) . . . . ?
C25 C26 C27 C28 -0.3(5) . . . . ?
C26 C27 C28 C23 -0.5(5) . . . . ?
C26 C27 C28 C37 -178.7(3) . . . . ?
C27 C28 C37 C38 88.9(4) . . . . ?
C27 C28 C37 C42 -91.6(4) . . . . ?
C27 C28 C37 Li2 163.3(3) . . . . ?
C28 C23 C24 C25 0.7(5) . . . . ?
C28 C23 C24 C29 -179.8(3) . . . . ?
C28 C37 C38 C39 179.2(3) . . . . ?
C28 C37 C38 C43 -2.6(5) . . . . ?
C28 C37 C38 Li2 72.8(3) . . . . ?
C28 C37 C42 C41 -179.2(3) . . . . ?
C28 C37 C42 C44 3.3(5) . . . . ?
C29 C24 C25 C26 179.1(3) . . . . ?
C29 C30 C31 C32 0.4(6) . . . . ?
C30 C29 C34 C33 1.0(5) . . . . ?
C30 C29 C34 C36 -177.2(3) . . . . ?
C30 C31 C32 C33 0.3(7) . . . . ?
C31 C32 C33 C34 -0.4(6) . . . . ?
C32 C33 C34 C29 -0.3(6) . . . . ?
C32 C33 C34 C36 177.9(4) . . . . ?
C34 C29 C30 C31 -1.1(5) . . . . ?
C34 C29 C30 C35 178.0(3) . . . . ?
C35 C30 C31 C32 -178.7(4) . . . . ?
C37 C38 C39 C40 0.0(6) . . . . ?
C38 C37 C42 C41 0.2(5) . . . . ?
C38 C37 C42 C44 -177.2(4) . . . . ?
C38 C39 C40 C41 0.3(7) . . . . ?
C39 C40 C41 C42 -0.4(7) . . . . ?
C40 C41 C42 C37 0.1(6) . . . . ?
C40 C41 C42 C44 177.5(4) . . . . ?
C42 C37 C38 C39 -0.3(5) . . . . ?
C42 C37 C38 C43 177.9(4) . . . . ?
C42 C37 C38 Li2 -106.7(3) . . . . ?
C43 C38 C39 C40 -178.2(4) . . . . ?
Li1 C1 C2 C3 -168.2(3) . . . . ?
Li1 C1 C2 C7 8.9(4) . . . . ?
Li1 C1 C6 C5 158.2(5) . . . . ?
Li1 C1 C6 C15 -20.2(7) . . . . ?
Li1 C7 C8 C9 -93.5(4) . . . . ?
Li1 C7 C8 C13 90.0(4) . . . . ?
Li1 C7 C12 C11 104.0(4) . . . . ?
Li1 C7 C12 C14 -78.6(4) . . . . ?
Li1 C23 C24 C25 -160.3(3) . . . . ?
Li1 C23 C24 C29 19.1(3) . . . . ?
Li1 C23 C28 C27 145.7(4) . . . . ?
Li1 C23 C28 C37 -36.1(6) . . . . ?
Li1 C29 C30 C31 102.7(4) . . . . ?
Li1 C29 C30 C35 -78.2(4) . . . . ?
Li1 C29 C34 C33 -94.2(3) . . . . ?
Li1 C29 C34 C36 87.6(4) . . . . ?
Li2 C1 C2 C3 137.9(4) . . . . ?
Li2 C1 C2 C7 -45.0(6) . . . . ?
Li2 C1 C6 C5 -154.0(3) . . . . ?
Li2 C1 C6 C15 27.7(4) . . . . ?
Li2 C15 C16 C17 -97.3(4) . . . . ?
Li2 C15 C16 C21 85.5(4) . . . . ?
Li2 C15 C20 C19 101.7(4) . . . . ?
Li2 C15 C20 C22 -80.5(4) . . . . ?
Li2 C23 C24 C25 147.3(4) . . . . ?
Li2 C23 C24 C29 -33.2(6) . . . . ?
Li2 C23 C28 C27 -160.5(3) . . . . ?
Li2 C23 C28 C37 17.7(3) . . . . ?
Li2 C37 C38 C39 106.4(4) . . . . ?
Li2 C37 C38 C43 -75.4(4) . . . . ?
Li2 C37 C42 C41 -91.2(4) . . . . ?
Li2 C37 C42 C44 91.3(4) . . . . ?
Li2 C38 C39 C40 77.3(5) . . . . ?
C45 C46 C47 C48 177.3(12) . . . . ?
C46 C47 C48 C49 -176.4(10) . . . . ?
C46 C47 C48 C50 63.0(13) . . . . ?

_olex2_date_sample_data_collection 2016-11-22
_olex2_date_sample_submission    2016-11-21
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_original_sample_id KEWJMB
_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 1.436
_oxdiff_exptl_absorpt_empirical_full_min 0.756
####################################################################### 
# 
# 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_liajvb_sq
_database_code_depnum_ccdc_archive 'CCDC 2045218'
loop_
_audit_author_name
_audit_author_address
'Stephen P. Argent'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2020-11-18 deposited with the CCDC.	2020-12-04 downloaded from the CCDC.
;
_nottingham_internal_coll_name   LIAJVB
_nottingham_internal_coll_number 15492
_nottingham_internal_coll_client AJV/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 6.00, 1.50'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   21/01/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 14/03/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 14/03/2016
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 29/04/2020
_nottingham_internal_refinement_user pcxav1/pczlt/pczspa
_nottingham_internal_self_archive_date ?
_nottingham_internal_self_validation_date ?
_nottingham_internal_self_validation_user ?
_nottingham_internal_validation_date 29/04/2020
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date ?
_refine_special_details          
;
 Conformational disorder is modelled for tert-butyl moiety
 C49-C52. The occupancy of the two disorder components were
 refined and constrained to sum to unity. The geometries of
 the two disorder components are restrained to be similar
 (SAME). Rigid bond and similarity restraints are were
 applied to the anisotropic displacement parameters of the
 disordered atoms (RIGU, SIMU).

 A disordered solvent molecule could not be sensibly modelled,
 so the structure was treated with PLATON SQUEEZE (P. v.d. Sluis
 & A.L. Spek, Acta Cryst. 1990, A46, 194-201). A total of 83
 electrons were accounted from the P1 cell in this, equating to
 1.5 hexane molecules per asymmetric unit, which have been
 included in the unit cell contents and calculation of derived
 parameters. The voids in which the solvent is located forms
 a continuous channel through the structure making the non-
 integer solvent designation plausible in the context of
 non-commensurate occupancy.
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.022 0.000 0.000 356 83 '1.5(C6 H14)'

_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
_platon_squeeze_special_details  ?
_audit_creation_date             2020-07-02
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H58 Li2'
_chemical_formula_sum            'C52 H58 Li2'
_chemical_formula_weight         696.86
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C52 H58 Li2'
_chemical_oxdiff_usercomment     
'LIAJVB #15492 SN-831 IN FOMBLIN FILM ON MICROMOUNT FOR AJV/DLK'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 '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                   11.9982(4)
_cell_length_b                   15.2538(10)
_cell_length_c                   15.4697(9)
_cell_angle_alpha                113.742(6)
_cell_angle_beta                 101.077(4)
_cell_angle_gamma                104.484(4)
_cell_volume                     2368.3(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8513
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.4270
_cell_measurement_theta_min      4.1310
_shelx_estimated_absorpt_T_max   0.918
_shelx_estimated_absorpt_T_min   0.791
_exptl_absorpt_coefficient_mu    0.399
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.977
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             752
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 10 -5 0.1556
-7 4 -3 0.2618
-7 -2 0 0.2655
-2 -9 4 0.1723
0 -10 5 0.1730
2 -10 5 0.2110
7 -6 3 0.2997
5 6 -2 0.2420
0 10 -5 0.1512
-1 0 -8 0.1086
-8 0 3 0.2749
-3 0 9 0.1558
0 0 9 0.1210
-3 -6 9 0.1975
1 -6 10 0.1491
-1 6 4 0.1473
-8 4 2 0.2678
2 5 -10 0.1000
5 4 -8 0.2024
1 -5 -5 0.1780
7 -5 -4 0.2797
-2 -4 -4 0.1580
0 1 -9 0.0874
5 1 -9 0.1639

_exptl_crystal_size_max          0.615
_exptl_crystal_size_mid          0.346
_exptl_crystal_size_min          0.219
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.1054 9.6190 -4.7292 0.9258 -0.3262 -0.1912
-6.9872 4.2685 -2.6219 0.3869 -0.1392 0.9116
-6.5648 -1.7361 0.3572 -0.1898 0.0642 0.9797
-1.8990 -8.6426 4.0988 -0.8387 0.2947 0.4580
0.3210 -9.6785 4.7747 -0.9308 0.3280 0.1615
2.2858 -9.8066 4.9857 -0.9363 0.3308 -0.1178
6.5838 -5.8324 3.3591 -0.5389 0.1925 -0.8201
4.7855 5.6139 -2.3947 0.5570 -0.1943 -0.8075
-0.3783 9.6928 -4.7860 0.9319 -0.3285 -0.1536
-0.8873 0.1507 -8.3344 0.3754 0.7861 0.4910
-7.5820 0.2386 2.6738 -0.1525 -0.3264 0.9328
-2.6388 -0.0344 9.2036 -0.4293 -0.9023 -0.0407
0.3522 -0.1348 8.5906 -0.3892 -0.8156 -0.4282
-3.1346 -6.2215 8.8128 -0.8761 -0.3649 0.3150
0.5614 -5.7020 9.6171 -0.8480 -0.4608 -0.2617
-1.2714 6.2790 4.1586 0.2743 -0.9198 -0.2807
-7.5563 4.3281 2.1077 0.1774 -0.6040 0.7770
1.7035 4.9676 -9.9497 0.8235 0.5672 -0.0090
5.1170 4.0868 -8.0582 0.6971 0.4784 -0.5340
0.6726 -5.3329 -4.9677 -0.1720 0.9171 0.3597
6.6292 -5.0150 -3.9416 -0.1534 0.8308 -0.5351
-1.9137 -4.2845 -4.2898 -0.1416 0.7497 0.6464
-0.1817 1.0580 -9.0685 0.4804 0.7878 0.3856
4.6242 0.9521 -8.9542 0.5001 0.8165 -0.2887

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18068
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.363
_diffrn_reflns_theta_min         3.307
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     61.00 178.00   1.00    6.00    --  106.13  15.00 120.00  117
  2  ω     79.00 119.00   1.00    6.00    --  106.13-125.00 -30.00   40
  3  ω     62.00  97.00   1.00    6.00    --  106.13 -45.00 -60.00   35
  4  ω     50.00  83.00   1.00    6.00    --  106.13 -30.00 -90.00   33
  5  ω     94.00 177.00   1.00    6.00    --  106.13  30.00-180.00   83
  6  ω     66.00  96.00   1.00    1.50    --   43.22-125.00-180.00   30
  7  ω     52.00  83.00   1.00    6.00    --  106.13 -30.00-180.00   31
  8  ω     28.00  97.00   1.00    6.00    --  106.13 -95.00 -30.00   69
  9  ω     62.00  89.00   1.00    6.00    --  106.13 -30.00  30.00   27
 10  ω     35.00 100.00   1.00    6.00    --  106.13 -95.00  90.00   65
 11  ω     74.00 104.00   1.00    6.00    --  106.13 -95.00 150.00   30
 12  ω     54.00 119.00   1.00    6.00    --  106.13-125.00  90.00   65
 13  ω     44.00 129.00   1.00    6.00    --  106.13 -77.00 150.00   85
 14  ω     31.00  82.00   1.00    6.00    --  106.13 -30.00 150.00   51
 15  ω     30.00  60.00   1.00    6.00    --  106.13 -95.00 150.00   30
 16  ω     23.00  88.00   1.00    1.50    --   43.22-125.00  90.00   65
 17  ω     35.00  73.00   1.00    6.00    --  106.13-125.00 -30.00   38
 18  ω    -71.00  39.00   1.00    1.50    --  -38.50  19.00 -90.00  110
 19  ω    -47.00  34.00   1.00    1.50    --  -38.50  38.00 -30.00   81
 20  ω    -97.00 -16.00   1.00    1.50    --  -38.50 -38.00  90.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0067976000
_diffrn_orient_matrix_UB_12      0.0744820000
_diffrn_orient_matrix_UB_13      -0.0444159000
_diffrn_orient_matrix_UB_21      0.0064710000
_diffrn_orient_matrix_UB_22      -0.0812732000
_diffrn_orient_matrix_UB_23      -0.0964810000
_diffrn_orient_matrix_UB_31      -0.1401907000
_diffrn_orient_matrix_UB_32      -0.0434283000
_diffrn_orient_matrix_UB_33      -0.0447762000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8068
_reflns_number_total             9359
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       '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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         9359
_refine_ls_number_restraints     169
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0484
_refine_ls_restrained_S_all      1.021
_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)+(0.0752P)²+0.4271P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1392
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C49A-C26 \\sim C49B-C26
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C49A \\sim C50A \\sim C51A \\sim C52A \\sim C49B \\sim C50B \\sim C51B \\sim
C52B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
Uanis(C49A) = Uanis(C49B)
Uanis(C52A) = Uanis(C52B)
4. Rigid body (RIGU) restrains
 C26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49A, C50A, C51A, C52A, C49B, C50B, C51B, C52B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C49A, C52A, C50A, C51A} sigma for 1-2: 0.02, 1-3: 0.04
{C49A, C52A, C51A, C50A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C49A, C50A, C51A, C52A}
{C49A, C50A, C51A, C52A} sigma for 1-2: 0.02, 1-3: 0.04
{C49A, C52A, C50A, C51A} sigma for 1-2: 0.02, 1-3: 0.04
{C49A, C52A, C51A, C50A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C49B, C50B, C51B, C52B}
6. Others
 Sof(C49B)=Sof(C50B)=Sof(H50d)=Sof(H50e)=Sof(H50f)=Sof(C51B)=Sof(H51d)=
 Sof(H51e)=Sof(H51f)=Sof(C52B)=Sof(H52d)=Sof(H52e)=Sof(H52f)=1-FVAR(1)
 Sof(C49A)=Sof(C50A)=Sof(H50a)=Sof(H50b)=Sof(H50c)=Sof(C51A)=Sof(H51a)=
 Sof(H51b)=Sof(H51c)=Sof(C52A)=Sof(H52a)=Sof(H52b)=Sof(H52c)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18), C19(H19),
 C25(H25), C27(H27), C31(H31), C32(H32), C33(H33), C39(H39), C40(H40), C41(H41)
7.b Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C21(H21a,H21b,H21c), C22(H22a,H22b,
 H22c), C35(H35a,H35b,H35c), C36(H36a,H36b,H36c), C43(H43a,H43b,H43c), C44(H44a,
 H44b,H44c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c), C48(H48a,H48b,H48c),
 C50A(H50a,H50b,H50c), C51A(H51a,H51b,H51c), C52A(H52a,H52b,H52c), C50B(H50d,
 H50e,H50f), C51B(H51d,H51e,H51f), C52B(H52d,H52e,H52f)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.30847(10) 0.26614(9) 0.55388(9) 0.0296(2) Uani 1 1 d . . . . .
C2 C 0.39361(10) 0.22129(9) 0.57398(9) 0.0303(2) Uani 1 1 d . . . . .
C3 C 0.41924(11) 0.14791(10) 0.49972(9) 0.0337(3) Uani 1 1 d . . . . .
H3 H 0.477326 0.120903 0.518564 0.040 Uiso 1 1 calc R U . . .
C4 C 0.36173(11) 0.11303(9) 0.39829(9) 0.0337(3) Uani 1 1 d . . . . .
C5 C 0.27783(11) 0.15582(9) 0.37537(9) 0.0325(3) Uani 1 1 d . . . . .
H5 H 0.236698 0.134416 0.307270 0.039 Uiso 1 1 calc R U . . .
C6 C 0.25289(10) 0.22982(9) 0.45074(9) 0.0298(2) Uani 1 1 d . . . . .
C7 C 0.46724(11) 0.25899(10) 0.68036(9) 0.0330(3) Uani 1 1 d . . . . .
C8 C 0.42255(13) 0.21621(11) 0.73808(10) 0.0391(3) Uani 1 1 d . . . . .
C9 C 0.49429(15) 0.25365(13) 0.83664(11) 0.0486(4) Uani 1 1 d . . . . .
H9 H 0.464382 0.225771 0.876226 0.058 Uiso 1 1 calc R U . . .
C10 C 0.60764(15) 0.33021(15) 0.87775(11) 0.0536(4) Uani 1 1 d . . . . .
H10 H 0.655260 0.354903 0.945143 0.064 Uiso 1 1 calc R U . . .
C11 C 0.65188(14) 0.37098(14) 0.82073(11) 0.0522(4) Uani 1 1 d . . . . .
H11 H 0.730737 0.423048 0.849086 0.063 Uiso 1 1 calc R U . . .
C12 C 0.58272(12) 0.33700(12) 0.72213(10) 0.0412(3) Uani 1 1 d . . . . .
C13 C 0.30214(15) 0.12873(12) 0.69191(13) 0.0493(3) Uani 1 1 d . . . . .
H13A H 0.238606 0.148626 0.663524 0.074 Uiso 1 1 calc R U . . .
H13B H 0.282089 0.111913 0.743229 0.074 Uiso 1 1 calc R U . . .
H13C H 0.307042 0.068488 0.638812 0.074 Uiso 1 1 calc R U . . .
C14 C 0.63282(14) 0.38170(15) 0.66045(12) 0.0575(4) Uani 1 1 d . . . . .
H14A H 0.640975 0.327523 0.603251 0.086 Uiso 1 1 calc R U . . .
H14B H 0.712939 0.436235 0.701765 0.086 Uiso 1 1 calc R U . . .
H14C H 0.577082 0.410374 0.636273 0.086 Uiso 1 1 calc R U . . .
C15 C 0.16556(10) 0.27617(9) 0.41989(9) 0.0308(2) Uani 1 1 d . . . . .
C16 C 0.21038(11) 0.37880(9) 0.43870(10) 0.0327(3) Uani 1 1 d . . . . .
C17 C 0.12932(12) 0.42179(10) 0.41076(11) 0.0402(3) Uani 1 1 d . . . . .
H17 H 0.159647 0.491372 0.424168 0.048 Uiso 1 1 calc R U . . .
C18 C 0.00625(13) 0.36531(12) 0.36412(12) 0.0465(3) Uani 1 1 d . . . . .
H18 H -0.047700 0.395604 0.345320 0.056 Uiso 1 1 calc R U . . .
C19 C -0.03802(12) 0.26435(12) 0.34495(13) 0.0490(4) Uani 1 1 d . . . . .
H19 H -0.122861 0.225306 0.312533 0.059 Uiso 1 1 calc R U . . .
C20 C 0.03982(12) 0.21856(10) 0.37239(11) 0.0412(3) Uani 1 1 d . . . . .
C21 C 0.34492(11) 0.44244(10) 0.48527(11) 0.0400(3) Uani 1 1 d . . . . .
H21A H 0.369649 0.467274 0.557671 0.060 Uiso 1 1 calc R U . . .
H21B H 0.361682 0.501261 0.472056 0.060 Uiso 1 1 calc R U . . .
H21C H 0.390874 0.400164 0.456357 0.060 Uiso 1 1 calc R U . . .
C22 C -0.01181(14) 0.10758(12) 0.34911(16) 0.0577(4) Uani 1 1 d . . . . .
H22A H 0.012627 0.065227 0.294857 0.087 Uiso 1 1 calc R U . . .
H22B H -0.100997 0.084147 0.328492 0.087 Uiso 1 1 calc R U . . .
H22C H 0.019436 0.101305 0.408873 0.087 Uiso 1 1 calc R U . . .
C23 C 0.22514(10) 0.45508(9) 0.74250(9) 0.0303(2) Uani 1 1 d . . . . .
C24 C 0.28924(10) 0.56227(9) 0.79688(9) 0.0293(2) Uani 1 1 d . . . . .
C25 C 0.24495(10) 0.63124(9) 0.85831(9) 0.0323(3) Uani 1 1 d . . . . .
H25 H 0.292686 0.702683 0.892774 0.039 Uiso 1 1 calc R U . . .
C26 C 0.13237(10) 0.59744(10) 0.87005(9) 0.0330(3) Uani 1 1 d D . . . .
C27 C 0.06729(11) 0.49168(10) 0.81862(10) 0.0333(3) Uani 1 1 d . . . . .
H27 H -0.009410 0.465331 0.825189 0.040 Uiso 1 1 calc R U . . .
C28 C 0.11236(11) 0.42378(9) 0.75777(10) 0.0319(3) Uani 1 1 d . . . . .
C29 C 0.41308(10) 0.60377(9) 0.79016(9) 0.0313(2) Uani 1 1 d . . . . .
C30 C 0.51308(11) 0.59166(11) 0.84249(10) 0.0380(3) Uani 1 1 d . . . . .
C31 C 0.62652(12) 0.62663(13) 0.83239(12) 0.0494(4) Uani 1 1 d . . . . .
H31 H 0.694361 0.618628 0.867258 0.059 Uiso 1 1 calc R U . . .
C32 C 0.64184(13) 0.67255(13) 0.77273(13) 0.0531(4) Uani 1 1 d . . . . .
H32 H 0.719576 0.695496 0.766316 0.064 Uiso 1 1 calc R U . . .
C33 C 0.54352(13) 0.68522(11) 0.72204(12) 0.0466(3) Uani 1 1 d . . . . .
H33 H 0.554563 0.717498 0.681448 0.056 Uiso 1 1 calc R U . . .
C34 C 0.42913(12) 0.65122(10) 0.73000(11) 0.0377(3) Uani 1 1 d . . . . .
C35 C 0.50156(13) 0.54533(14) 0.91160(11) 0.0476(3) Uani 1 1 d . . . . .
H35A H 0.446506 0.567888 0.947289 0.071 Uiso 1 1 calc R U . . .
H35B H 0.582059 0.567879 0.959998 0.071 Uiso 1 1 calc R U . . .
H35C H 0.468626 0.470147 0.872378 0.071 Uiso 1 1 calc R U . . .
C36 C 0.32283(14) 0.66367(13) 0.67244(13) 0.0482(3) Uani 1 1 d . . . . .
H36A H 0.254158 0.597646 0.635064 0.072 Uiso 1 1 calc R U . . .
H36B H 0.346819 0.686496 0.625665 0.072 Uiso 1 1 calc R U . . .
H36C H 0.298476 0.714945 0.719195 0.072 Uiso 1 1 calc R U . . .
C37 C 0.03882(11) 0.31054(10) 0.70486(11) 0.0358(3) Uani 1 1 d . . . . .
C38 C -0.05669(12) 0.26624(10) 0.61376(12) 0.0434(3) Uani 1 1 d . . . . .
C39 C -0.11882(13) 0.15986(12) 0.56295(16) 0.0571(4) Uani 1 1 d . . . . .
H39 H -0.182499 0.129242 0.500868 0.069 Uiso 1 1 calc R U . . .
C40 C -0.08855(14) 0.09864(12) 0.60213(17) 0.0621(5) Uani 1 1 d . . . . .
H40 H -0.130853 0.026258 0.566757 0.074 Uiso 1 1 calc R U . . .
C41 C 0.00336(15) 0.14290(12) 0.69285(16) 0.0557(4) Uani 1 1 d . . . . .
H41 H 0.022164 0.100403 0.719951 0.067 Uiso 1 1 calc R U . . .
C42 C 0.06876(13) 0.24814(11) 0.74518(12) 0.0432(3) Uani 1 1 d . . . . .
C43 C -0.09401(14) 0.33281(12) 0.57238(14) 0.0517(4) Uani 1 1 d . . . . .
H43A H -0.120939 0.380909 0.620016 0.078 Uiso 1 1 calc R U . . .
H43B H -0.160979 0.289221 0.508635 0.078 Uiso 1 1 calc R U . . .
H43C H -0.024327 0.371496 0.561635 0.078 Uiso 1 1 calc R U . . .
C44 C 0.17047(16) 0.29500(13) 0.84328(13) 0.0532(4) Uani 1 1 d . . . . .
H44A H 0.249296 0.313276 0.832913 0.080 Uiso 1 1 calc R U . . .
H44B H 0.164895 0.245184 0.868644 0.080 Uiso 1 1 calc R U . . .
H44C H 0.163200 0.356925 0.891937 0.080 Uiso 1 1 calc R U . . .
C45 C 0.39472(14) 0.03320(11) 0.31924(10) 0.0423(3) Uani 1 1 d . . . . .
C46 C 0.3332(2) 0.01374(18) 0.21420(13) 0.0826(7) Uani 1 1 d . . . . .
H46A H 0.244463 -0.015102 0.197093 0.124 Uiso 1 1 calc R U . . .
H46B H 0.359319 -0.034902 0.166339 0.124 Uiso 1 1 calc R U . . .
H46C H 0.356117 0.078699 0.211510 0.124 Uiso 1 1 calc R U . . .
C47 C 0.35452(19) -0.06855(13) 0.32219(15) 0.0625(5) Uani 1 1 d . . . . .
H47A H 0.392180 -0.057136 0.389781 0.094 Uiso 1 1 calc R U . . .
H47B H 0.380044 -0.117981 0.274541 0.094 Uiso 1 1 calc R U . . .
H47C H 0.265541 -0.095789 0.304133 0.094 Uiso 1 1 calc R U . . .
C48 C 0.53195(17) 0.07090(15) 0.34100(15) 0.0671(5) Uani 1 1 d . . . . .
H48A H 0.558866 0.136335 0.339565 0.101 Uiso 1 1 calc R U . . .
H48B H 0.552365 0.019861 0.290196 0.101 Uiso 1 1 calc R U . . .
H48C H 0.573044 0.080790 0.407248 0.101 Uiso 1 1 calc R U . . .
Li1 Li 0.36780(19) 0.40028(19) 0.70114(17) 0.0407(5) Uani 1 1 d . . . . .
Li2 Li 0.16778(19) 0.32009(18) 0.59699(18) 0.0399(5) Uani 1 1 d . . . . .
C49A C 0.0775(8) 0.6653(5) 0.9389(6) 0.0376(9) Uani 0.602(10) 1 d D U P A 1
C50A C 0.1684(3) 0.7756(3) 0.9967(4) 0.0560(14) Uani 0.602(10) 1 d D U P A 1
H50A H 0.242916 0.778516 1.038976 0.084 Uiso 0.602(10) 1 calc R U P A 1
H50B H 0.132680 0.819748 1.038725 0.084 Uiso 0.602(10) 1 calc R U P A 1
H50C H 0.188314 0.799475 0.949475 0.084 Uiso 0.602(10) 1 calc R U P A 1
C51A C 0.0505(4) 0.6296(5) 1.0147(3) 0.0564(10) Uani 0.602(10) 1 d D U P A 1
H51A H -0.009800 0.559282 0.979070 0.085 Uiso 0.602(10) 1 calc R U P A 1
H51B H 0.018103 0.675484 1.058931 0.085 Uiso 0.602(10) 1 calc R U P A 1
H51C H 0.125789 0.631281 1.054642 0.085 Uiso 0.602(10) 1 calc R U P A 1
C52A C -0.0392(9) 0.6609(14) 0.8737(12) 0.0572(17) Uani 0.602(10) 1 d D U P A 1
H52A H -0.019695 0.686714 0.827693 0.086 Uiso 0.602(10) 1 calc R U P A 1
H52B H -0.075822 0.703555 0.916415 0.086 Uiso 0.602(10) 1 calc R U P A 1
H52C H -0.097023 0.589619 0.835225 0.086 Uiso 0.602(10) 1 calc R U P A 1
C49B C 0.0850(13) 0.6794(8) 0.9322(9) 0.0376(9) Uani 0.398(10) 1 d D U P A 2
C50B C 0.1454(6) 0.7894(3) 0.9497(6) 0.0538(15) Uani 0.398(10) 1 d D U P A 2
H50D H 0.232115 0.816115 0.988476 0.081 Uiso 0.398(10) 1 calc R U P A 2
H50E H 0.105732 0.833473 0.986736 0.081 Uiso 0.398(10) 1 calc R U P A 2
H50F H 0.136653 0.788699 0.885131 0.081 Uiso 0.398(10) 1 calc R U P A 2
C51B C 0.0992(9) 0.6827(8) 1.0333(5) 0.0609(18) Uani 0.398(10) 1 d D U P A 2
H51D H 0.061473 0.613073 1.023497 0.091 Uiso 0.398(10) 1 calc R U P A 2
H51E H 0.059252 0.726984 1.069522 0.091 Uiso 0.398(10) 1 calc R U P A 2
H51F H 0.186084 0.710289 1.072063 0.091 Uiso 0.398(10) 1 calc R U P A 2
C52B C -0.0516(15) 0.649(2) 0.8808(19) 0.0572(17) Uani 0.398(10) 1 d D U P A 2
H52D H -0.065275 0.641379 0.813160 0.086 Uiso 0.398(10) 1 calc R U P A 2
H52E H -0.079465 0.702772 0.919551 0.086 Uiso 0.398(10) 1 calc R U P A 2
H52F H -0.097230 0.583825 0.876834 0.086 Uiso 0.398(10) 1 calc R U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.4167(15) . ?
C1 C6 1.4113(17) . ?
C1 Li1 2.186(3) . ?
C1 Li2 2.158(2) . ?
C2 C3 1.3928(17) . ?
C2 C7 1.4982(17) . ?
C2 Li1 2.784(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.3962(18) . ?
C4 C5 1.3940(16) . ?
C4 C45 1.5372(17) . ?
C5 H5 0.9500 . ?
C5 C6 1.4023(17) . ?
C6 C15 1.5086(15) . ?
C6 Li2 2.672(3) . ?
C7 C8 1.4100(19) . ?
C7 C12 1.402(2) . ?
C7 Li1 2.655(3) . ?
C8 C9 1.393(2) . ?
C8 C13 1.500(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.376(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.379(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.395(2) . ?
C12 C14 1.509(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.4060(17) . ?
C15 C20 1.4068(17) . ?
C15 Li2 2.538(3) . ?
C16 C17 1.3958(17) . ?
C16 C21 1.5078(17) . ?
C17 H17 0.9500 . ?
C17 C18 1.377(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.380(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.3975(18) . ?
C20 C22 1.5094(19) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.4098(17) . ?
C23 C28 1.4161(16) . ?
C23 Li1 2.178(2) . ?
C23 Li2 2.178(3) . ?
C24 C25 1.4003(16) . ?
C24 C29 1.5037(16) . ?
C25 H25 0.9500 . ?
C25 C26 1.3945(17) . ?
C26 C27 1.3939(18) . ?
C26 C49A 1.537(7) . ?
C26 C49B 1.551(11) . ?
C27 H27 0.9500 . ?
C27 C28 1.3935(17) . ?
C28 C37 1.5013(17) . ?
C28 Li2 2.669(3) . ?
C29 C30 1.4097(18) . ?
C29 C34 1.4031(19) . ?
C29 Li1 2.693(3) . ?
C30 C31 1.395(2) . ?
C30 C35 1.509(2) . ?
C30 Li1 2.682(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.377(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.387(2) . ?
C33 H33 0.9500 . ?
C33 C34 1.3886(19) . ?
C34 C36 1.5089(19) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.408(2) . ?
C37 C42 1.4098(19) . ?
C37 Li2 2.505(3) . ?
C38 C39 1.396(2) . ?
C38 C43 1.511(2) . ?
C38 Li2 2.707(3) . ?
C39 H39 0.9500 . ?
C39 C40 1.383(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.383(3) . ?
C41 H41 0.9500 . ?
C41 C42 1.388(2) . ?
C42 C44 1.511(2) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.521(2) . ?
C45 C47 1.528(2) . ?
C45 C48 1.521(2) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
Li1 Li2 2.304(3) . ?
C49A C50A 1.522(7) . ?
C49A C51A 1.532(7) . ?
C49A C52A 1.530(8) . ?
C50A H50A 0.9800 . ?
C50A H50B 0.9800 . ?
C50A H50C 0.9800 . ?
C51A H51A 0.9800 . ?
C51A H51B 0.9800 . ?
C51A H51C 0.9800 . ?
C52A H52A 0.9800 . ?
C52A H52B 0.9800 . ?
C52A H52C 0.9800 . ?
C49B C50B 1.537(10) . ?
C49B C51B 1.518(11) . ?
C49B C52B 1.535(12) . ?
C50B H50D 0.9800 . ?
C50B H50E 0.9800 . ?
C50B H50F 0.9800 . ?
C51B H51D 0.9800 . ?
C51B H51E 0.9800 . ?
C51B H51F 0.9800 . ?
C52B H52D 0.9800 . ?
C52B H52E 0.9800 . ?
C52B H52F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 Li1 98.98(10) . . ?
C2 C1 Li2 145.79(11) . . ?
C6 C1 C2 113.21(10) . . ?
C6 C1 Li1 143.21(11) . . ?
C6 C1 Li2 94.63(10) . . ?
Li2 C1 Li1 64.07(9) . . ?
C1 C2 C7 119.05(10) . . ?
C1 C2 Li1 50.85(8) . . ?
C3 C2 C1 123.61(11) . . ?
C3 C2 C7 117.20(10) . . ?
C3 C2 Li1 164.86(11) . . ?
C7 C2 Li1 69.30(8) . . ?
C2 C3 H3 119.2 . . ?
C2 C3 C4 121.66(10) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C45 119.66(11) . . ?
C5 C4 C3 116.50(11) . . ?
C5 C4 C45 123.82(11) . . ?
C4 C5 H5 119.3 . . ?
C4 C5 C6 121.36(11) . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C15 118.21(10) . . ?
C1 C6 Li2 53.61(8) . . ?
C5 C6 C1 123.65(10) . . ?
C5 C6 C15 118.09(10) . . ?
C5 C6 Li2 162.49(10) . . ?
C15 C6 Li2 68.34(8) . . ?
C2 C7 Li1 78.83(8) . . ?
C8 C7 C2 120.92(12) . . ?
C8 C7 Li1 102.93(9) . . ?
C12 C7 C2 119.16(12) . . ?
C12 C7 C8 119.92(12) . . ?
C12 C7 Li1 88.84(9) . . ?
C7 C8 C13 120.05(12) . . ?
C9 C8 C7 118.89(14) . . ?
C9 C8 C13 121.00(14) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 C8 121.27(15) . . ?
C10 C9 H9 119.4 . . ?
C9 C10 H10 120.1 . . ?
C9 C10 C11 119.75(13) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 119.5 . . ?
C10 C11 C12 121.08(15) . . ?
C12 C11 H11 119.5 . . ?
C7 C12 C14 120.45(12) . . ?
C11 C12 C7 119.08(14) . . ?
C11 C12 C14 120.45(14) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C6 C15 Li2 78.12(8) . . ?
C16 C15 C6 119.54(10) . . ?
C16 C15 C20 119.22(11) . . ?
C16 C15 Li2 95.31(10) . . ?
C20 C15 C6 121.25(11) . . ?
C20 C15 Li2 96.73(10) . . ?
C15 C16 C21 121.33(10) . . ?
C17 C16 C15 119.46(11) . . ?
C17 C16 C21 119.17(11) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 C16 121.30(12) . . ?
C18 C17 H17 119.3 . . ?
C17 C18 H18 120.3 . . ?
C17 C18 C19 119.43(12) . . ?
C19 C18 H18 120.3 . . ?
C18 C19 H19 119.4 . . ?
C18 C19 C20 121.13(12) . . ?
C20 C19 H19 119.4 . . ?
C15 C20 C22 120.94(11) . . ?
C19 C20 C15 119.46(12) . . ?
C19 C20 C22 119.59(12) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C28 113.23(10) . . ?
C24 C23 Li1 101.38(10) . . ?
C24 C23 Li2 144.16(11) . . ?
C28 C23 Li1 142.11(11) . . ?
C28 C23 Li2 93.48(10) . . ?
Li1 C23 Li2 63.88(9) . . ?
C23 C24 C29 117.84(10) . . ?
C25 C24 C23 123.49(11) . . ?
C25 C24 C29 118.65(10) . . ?
C24 C25 H25 119.2 . . ?
C26 C25 C24 121.50(11) . . ?
C26 C25 H25 119.2 . . ?
C25 C26 C49A 126.0(3) . . ?
C25 C26 C49B 118.3(5) . . ?
C27 C26 C25 116.58(11) . . ?
C27 C26 C49A 117.3(3) . . ?
C27 C26 C49B 125.0(5) . . ?
C26 C27 H27 119.3 . . ?
C28 C27 C26 121.39(11) . . ?
C28 C27 H27 119.3 . . ?
C23 C28 C37 117.13(10) . . ?
C23 C28 Li2 54.54(8) . . ?
C27 C28 C23 123.78(11) . . ?
C27 C28 C37 119.09(10) . . ?
C27 C28 Li2 158.78(10) . . ?
C37 C28 Li2 67.22(8) . . ?
C24 C29 Li1 78.81(8) . . ?
C30 C29 C24 119.36(11) . . ?
C30 C29 Li1 74.35(9) . . ?
C34 C29 C24 120.75(11) . . ?
C34 C29 C30 119.86(11) . . ?
C34 C29 Li1 115.55(10) . . ?
C29 C30 C35 121.78(12) . . ?
C29 C30 Li1 75.24(9) . . ?
C31 C30 C29 118.87(13) . . ?
C31 C30 C35 119.31(12) . . ?
C31 C30 Li1 114.58(11) . . ?
C35 C30 Li1 83.02(10) . . ?
C30 C31 H31 119.4 . . ?
C32 C31 C30 121.15(13) . . ?
C32 C31 H31 119.4 . . ?
C31 C32 H32 120.1 . . ?
C31 C32 C33 119.86(13) . . ?
C33 C32 H32 120.1 . . ?
C32 C33 H33 119.7 . . ?
C32 C33 C34 120.69(14) . . ?
C34 C33 H33 119.7 . . ?
C29 C34 C36 120.60(11) . . ?
C33 C34 C29 119.56(13) . . ?
C33 C34 C36 119.82(13) . . ?
C30 C35 H35A 109.5 . . ?
C30 C35 H35B 109.5 . . ?
C30 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C28 C37 Li2 79.24(9) . . ?
C38 C37 C28 120.29(11) . . ?
C38 C37 C42 120.11(12) . . ?
C38 C37 Li2 82.45(10) . . ?
C42 C37 C28 119.56(13) . . ?
C42 C37 Li2 106.70(10) . . ?
C37 C38 C43 120.66(12) . . ?
C37 C38 Li2 66.53(9) . . ?
C39 C38 C37 119.17(14) . . ?
C39 C38 C43 120.15(14) . . ?
C39 C38 Li2 112.24(11) . . ?
C43 C38 Li2 92.40(10) . . ?
C38 C39 H39 119.7 . . ?
C40 C39 C38 120.63(16) . . ?
C40 C39 H39 119.7 . . ?
C39 C40 H40 120.0 . . ?
C41 C40 C39 119.92(14) . . ?
C41 C40 H40 120.0 . . ?
C40 C41 H41 119.3 . . ?
C40 C41 C42 121.39(14) . . ?
C42 C41 H41 119.3 . . ?
C37 C42 C44 120.54(13) . . ?
C41 C42 C37 118.75(15) . . ?
C41 C42 C44 120.71(14) . . ?
C38 C43 H43A 109.5 . . ?
C38 C43 H43B 109.5 . . ?
C38 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 C4 111.79(11) . . ?
C46 C45 C47 108.40(15) . . ?
C47 C45 C4 109.69(13) . . ?
C48 C45 C4 109.85(12) . . ?
C48 C45 C46 108.31(17) . . ?
C48 C45 C47 108.73(14) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C1 Li1 C2 30.17(5) . . ?
C1 Li1 C7 61.64(7) . . ?
C1 Li1 C29 141.96(12) . . ?
C1 Li1 C30 153.43(12) . . ?
C1 Li1 Li2 57.38(8) . . ?
C7 Li1 C2 31.87(4) . . ?
C7 Li1 C29 144.26(10) . . ?
C7 Li1 C30 114.61(9) . . ?
C23 Li1 C1 115.43(10) . . ?
C23 Li1 C2 139.69(11) . . ?
C23 Li1 C7 146.30(12) . . ?
C23 Li1 C29 60.55(7) . . ?
C23 Li1 C30 82.55(8) . . ?
C23 Li1 Li2 58.06(8) . . ?
C29 Li1 C2 154.88(11) . . ?
C30 Li1 C2 137.71(9) . . ?
C30 Li1 C29 30.41(5) . . ?
Li2 Li1 C2 84.00(9) . . ?
Li2 Li1 C7 108.82(11) . . ?
Li2 Li1 C29 106.81(10) . . ?
Li2 Li1 C30 136.37(12) . . ?
C1 Li2 C6 31.76(5) . . ?
C1 Li2 C15 63.91(7) . . ?
C1 Li2 C23 116.60(11) . . ?
C1 Li2 C28 141.87(11) . . ?
C1 Li2 C37 139.12(12) . . ?
C1 Li2 C38 145.50(11) . . ?
C1 Li2 Li1 58.55(8) . . ?
C6 Li2 C38 131.04(10) . . ?
C15 Li2 C6 33.54(4) . . ?
C15 Li2 C28 150.21(10) . . ?
C15 Li2 C38 114.03(9) . . ?
C23 Li2 C6 141.16(10) . . ?
C23 Li2 C15 139.19(12) . . ?
C23 Li2 C28 31.98(5) . . ?
C23 Li2 C37 63.78(7) . . ?
C23 Li2 C38 87.79(9) . . ?
C23 Li2 Li1 58.06(8) . . ?
C28 Li2 C6 172.72(10) . . ?
C28 Li2 C38 55.97(6) . . ?
C37 Li2 C6 151.06(11) . . ?
C37 Li2 C15 145.03(10) . . ?
C37 Li2 C28 33.54(5) . . ?
C37 Li2 C38 31.02(5) . . ?
Li1 Li2 C6 86.56(9) . . ?
Li1 Li2 C15 108.26(11) . . ?
Li1 Li2 C28 86.19(10) . . ?
Li1 Li2 C37 106.71(12) . . ?
Li1 Li2 C38 137.70(13) . . ?
C50A C49A C26 109.1(5) . . ?
C50A C49A C51A 108.1(5) . . ?
C50A C49A C52A 109.5(7) . . ?
C51A C49A C26 111.2(5) . . ?
C52A C49A C26 108.3(10) . . ?
C52A C49A C51A 110.6(7) . . ?
C49A C50A H50A 109.5 . . ?
C49A C50A H50B 109.5 . . ?
C49A C50A H50C 109.5 . . ?
H50A C50A H50B 109.5 . . ?
H50A C50A H50C 109.5 . . ?
H50B C50A H50C 109.5 . . ?
C49A C51A H51A 109.5 . . ?
C49A C51A H51B 109.5 . . ?
C49A C51A H51C 109.5 . . ?
H51A C51A H51B 109.5 . . ?
H51A C51A H51C 109.5 . . ?
H51B C51A H51C 109.5 . . ?
C49A C52A H52A 109.5 . . ?
C49A C52A H52B 109.5 . . ?
C49A C52A H52C 109.5 . . ?
H52A C52A H52B 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
C50B C49B C26 116.6(7) . . ?
C51B C49B C26 108.7(7) . . ?
C51B C49B C50B 108.4(8) . . ?
C51B C49B C52B 107.0(11) . . ?
C52B C49B C26 110.4(15) . . ?
C52B C49B C50B 105.3(11) . . ?
C49B C50B H50D 109.5 . . ?
C49B C50B H50E 109.5 . . ?
C49B C50B H50F 109.5 . . ?
H50D C50B H50E 109.5 . . ?
H50D C50B H50F 109.5 . . ?
H50E C50B H50F 109.5 . . ?
C49B C51B H51D 109.5 . . ?
C49B C51B H51E 109.5 . . ?
C49B C51B H51F 109.5 . . ?
H51D C51B H51E 109.5 . . ?
H51D C51B H51F 109.5 . . ?
H51E C51B H51F 109.5 . . ?
C49B C52B H52D 109.5 . . ?
C49B C52B H52E 109.5 . . ?
C49B C52B H52F 109.5 . . ?
H52D C52B H52E 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 0.2(2) . . . . ?
C1 C2 C7 C8 87.60(15) . . . . ?
C1 C2 C7 C12 -93.20(14) . . . . ?
C1 C2 C7 Li1 -10.89(12) . . . . ?
C1 C6 C15 C16 69.03(16) . . . . ?
C1 C6 C15 C20 -111.07(14) . . . . ?
C1 C6 C15 Li2 -20.36(11) . . . . ?
C2 C1 C6 C5 0.80(17) . . . . ?
C2 C1 C6 C15 -176.68(10) . . . . ?
C2 C1 C6 Li2 159.64(14) . . . . ?
C2 C3 C4 C5 0.27(19) . . . . ?
C2 C3 C4 C45 179.02(12) . . . . ?
C2 C7 C8 C9 179.93(11) . . . . ?
C2 C7 C8 C13 2.62(17) . . . . ?
C2 C7 C12 C11 -179.09(12) . . . . ?
C2 C7 C12 C14 -0.63(19) . . . . ?
C3 C2 C7 C8 -96.49(14) . . . . ?
C3 C2 C7 C12 82.71(15) . . . . ?
C3 C2 C7 Li1 165.02(12) . . . . ?
C3 C4 C5 C6 -0.14(19) . . . . ?
C3 C4 C45 C46 -173.76(17) . . . . ?
C3 C4 C45 C47 65.97(17) . . . . ?
C3 C4 C45 C48 -53.49(19) . . . . ?
C4 C5 C6 C1 -0.43(19) . . . . ?
C4 C5 C6 C15 177.05(11) . . . . ?
C4 C5 C6 Li2 -75.4(3) . . . . ?
C5 C4 C45 C46 4.9(2) . . . . ?
C5 C4 C45 C47 -115.38(15) . . . . ?
C5 C4 C45 C48 125.16(16) . . . . ?
C5 C6 C15 C16 -108.58(14) . . . . ?
C5 C6 C15 C20 71.31(16) . . . . ?
C5 C6 C15 Li2 162.02(12) . . . . ?
C6 C1 C2 C3 -0.66(17) . . . . ?
C6 C1 C2 C7 174.97(11) . . . . ?
C6 C1 C2 Li1 161.80(14) . . . . ?
C6 C15 C16 C17 -179.54(12) . . . . ?
C6 C15 C16 C21 2.61(19) . . . . ?
C6 C15 C20 C19 -179.96(14) . . . . ?
C6 C15 C20 C22 -1.0(2) . . . . ?
C7 C2 C3 C4 -175.55(12) . . . . ?
C7 C8 C9 C10 -0.74(19) . . . . ?
C8 C7 C12 C11 0.11(19) . . . . ?
C8 C7 C12 C14 178.58(13) . . . . ?
C8 C9 C10 C11 -0.1(2) . . . . ?
C9 C10 C11 C12 1.0(2) . . . . ?
C10 C11 C12 C7 -1.0(2) . . . . ?
C10 C11 C12 C14 -179.47(15) . . . . ?
C12 C7 C8 C9 0.74(18) . . . . ?
C12 C7 C8 C13 -176.57(12) . . . . ?
C13 C8 C9 C10 176.54(13) . . . . ?
C15 C16 C17 C18 -0.7(2) . . . . ?
C16 C15 C20 C19 -0.1(2) . . . . ?
C16 C15 C20 C22 178.89(15) . . . . ?
C16 C17 C18 C19 0.3(2) . . . . ?
C17 C18 C19 C20 0.3(3) . . . . ?
C18 C19 C20 C15 -0.3(3) . . . . ?
C18 C19 C20 C22 -179.32(17) . . . . ?
C20 C15 C16 C17 0.6(2) . . . . ?
C20 C15 C16 C21 -177.29(13) . . . . ?
C21 C16 C17 C18 177.23(14) . . . . ?
C23 C24 C25 C26 0.21(19) . . . . ?
C23 C24 C29 C30 -75.16(15) . . . . ?
C23 C24 C29 C34 102.77(14) . . . . ?
C23 C24 C29 Li1 -10.43(11) . . . . ?
C23 C28 C37 C38 -97.33(14) . . . . ?
C23 C28 C37 C42 80.45(16) . . . . ?
C23 C28 C37 Li2 -22.76(12) . . . . ?
C24 C23 C28 C27 1.27(18) . . . . ?
C24 C23 C28 C37 -178.54(11) . . . . ?
C24 C23 C28 Li2 155.49(13) . . . . ?
C24 C25 C26 C27 0.80(18) . . . . ?
C24 C25 C26 C49A 177.0(4) . . . . ?
C24 C25 C26 C49B -174.9(5) . . . . ?
C24 C29 C30 C31 177.35(12) . . . . ?
C24 C29 C30 C35 -4.76(19) . . . . ?
C24 C29 C30 Li1 67.12(11) . . . . ?
C24 C29 C34 C33 -177.47(12) . . . . ?
C24 C29 C34 C36 1.32(19) . . . . ?
C25 C24 C29 C30 103.31(14) . . . . ?
C25 C24 C29 C34 -78.76(15) . . . . ?
C25 C24 C29 Li1 168.04(12) . . . . ?
C25 C26 C27 C28 -0.75(18) . . . . ?
C25 C26 C49A C50A -2.6(7) . . . . ?
C25 C26 C49A C51A -121.8(4) . . . . ?
C25 C26 C49A C52A 116.4(7) . . . . ?
C25 C26 C49B C50B 17.6(11) . . . . ?
C25 C26 C49B C51B -105.3(7) . . . . ?
C25 C26 C49B C52B 137.7(10) . . . . ?
C26 C27 C28 C23 -0.3(2) . . . . ?
C26 C27 C28 C37 179.47(12) . . . . ?
C26 C27 C28 Li2 -78.5(3) . . . . ?
C27 C26 C49A C50A 173.6(3) . . . . ?
C27 C26 C49A C51A 54.4(7) . . . . ?
C27 C26 C49A C52A -67.4(7) . . . . ?
C27 C26 C49B C50B -157.7(7) . . . . ?
C27 C26 C49B C51B 79.4(10) . . . . ?
C27 C26 C49B C52B -37.7(12) . . . . ?
C27 C28 C37 C38 82.85(16) . . . . ?
C27 C28 C37 C42 -99.37(14) . . . . ?
C27 C28 C37 Li2 157.43(12) . . . . ?
C28 C23 C24 C25 -1.20(17) . . . . ?
C28 C23 C24 C29 177.18(11) . . . . ?
C28 C37 C38 C39 176.11(13) . . . . ?
C28 C37 C38 C43 -5.4(2) . . . . ?
C28 C37 C38 Li2 72.80(11) . . . . ?
C28 C37 C42 C41 -177.07(12) . . . . ?
C28 C37 C42 C44 2.68(19) . . . . ?
C29 C24 C25 C26 -178.16(11) . . . . ?
C29 C30 C31 C32 0.1(2) . . . . ?
C30 C29 C34 C33 0.5(2) . . . . ?
C30 C29 C34 C36 179.24(13) . . . . ?
C30 C31 C32 C33 0.4(3) . . . . ?
C31 C32 C33 C34 -0.6(3) . . . . ?
C32 C33 C34 C29 0.1(2) . . . . ?
C32 C33 C34 C36 -178.66(15) . . . . ?
C34 C29 C30 C31 -0.6(2) . . . . ?
C34 C29 C30 C35 177.29(13) . . . . ?
C34 C29 C30 Li1 -110.83(12) . . . . ?
C35 C30 C31 C32 -177.78(15) . . . . ?
C37 C38 C39 C40 1.0(2) . . . . ?
C38 C37 C42 C41 0.7(2) . . . . ?
C38 C37 C42 C44 -179.54(13) . . . . ?
C38 C39 C40 C41 0.5(3) . . . . ?
C39 C40 C41 C42 -1.5(3) . . . . ?
C40 C41 C42 C37 0.9(2) . . . . ?
C40 C41 C42 C44 -178.86(15) . . . . ?
C42 C37 C38 C39 -1.7(2) . . . . ?
C42 C37 C38 C43 176.83(13) . . . . ?
C42 C37 C38 Li2 -104.96(13) . . . . ?
C43 C38 C39 C40 -177.46(17) . . . . ?
C45 C4 C5 C6 -178.83(12) . . . . ?
Li1 C1 C2 C3 -162.46(13) . . . . ?
Li1 C1 C2 C7 13.18(14) . . . . ?
Li1 C1 C6 C5 149.78(15) . . . . ?
Li1 C1 C6 C15 -27.7(2) . . . . ?
Li1 C1 C6 Li2 -51.38(16) . . . . ?
Li1 C2 C3 C4 -63.3(4) . . . . ?
Li1 C2 C7 C8 98.49(12) . . . . ?
Li1 C2 C7 C12 -82.31(12) . . . . ?
Li1 C7 C8 C9 -95.47(12) . . . . ?
Li1 C7 C8 C13 87.22(13) . . . . ?
Li1 C7 C12 C11 104.39(14) . . . . ?
Li1 C7 C12 C14 -77.14(15) . . . . ?
Li1 C23 C24 C25 -165.45(12) . . . . ?
Li1 C23 C24 C29 12.94(14) . . . . ?
Li1 C23 C28 C27 155.58(15) . . . . ?
Li1 C23 C28 C37 -24.2(2) . . . . ?
Li1 C23 C28 Li2 -50.20(17) . . . . ?
Li1 C29 C30 C31 110.24(14) . . . . ?
Li1 C29 C30 C35 -71.88(14) . . . . ?
Li1 C29 C34 C33 -85.51(15) . . . . ?
Li1 C29 C34 C36 93.28(14) . . . . ?
Li1 C30 C31 C32 86.27(18) . . . . ?
Li2 C1 C2 C3 141.24(17) . . . . ?
Li2 C1 C2 C7 -43.1(2) . . . . ?
Li2 C1 C2 Li1 -56.30(18) . . . . ?
Li2 C1 C6 C5 -158.84(12) . . . . ?
Li2 C1 C6 C15 23.69(13) . . . . ?
Li2 C6 C15 C16 89.40(12) . . . . ?
Li2 C6 C15 C20 -90.71(13) . . . . ?
Li2 C15 C16 C17 -100.20(13) . . . . ?
Li2 C15 C16 C21 81.95(13) . . . . ?
Li2 C15 C20 C19 99.88(16) . . . . ?
Li2 C15 C20 C22 -81.17(16) . . . . ?
Li2 C23 C24 C25 133.79(16) . . . . ?
Li2 C23 C24 C29 -47.8(2) . . . . ?
Li2 C23 C28 C27 -154.22(13) . . . . ?
Li2 C23 C28 C37 25.97(13) . . . . ?
Li2 C28 C37 C38 -74.57(12) . . . . ?
Li2 C28 C37 C42 103.21(12) . . . . ?
Li2 C37 C38 C39 103.30(15) . . . . ?
Li2 C37 C38 C43 -78.21(15) . . . . ?
Li2 C37 C42 C41 -90.17(14) . . . . ?
Li2 C37 C42 C44 89.58(15) . . . . ?
Li2 C38 C39 C40 75.7(2) . . . . ?
C49A C26 C27 C28 -177.3(4) . . . . ?
C49B C26 C27 C28 174.7(6) . . . . ?

_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_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 1.446
_oxdiff_exptl_absorpt_empirical_full_min 0.563
####################################################################### 
# 
# 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_oajvle
_database_code_depnum_ccdc_archive 'CCDC 2045217'
loop_
_audit_author_name
_audit_author_address
'Stephen P. Argent'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2020-11-18 deposited with the CCDC.	2020-12-04 downloaded from the CCDC.
;
_nottingham_internal_coll_name   OAJVLE
_nottingham_internal_coll_number 16535
_nottingham_internal_coll_client AJV/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 2.00, 8.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   10/10/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 11/10/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 11/10/2016
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 28/04/2020
_nottingham_internal_refinement_user pcxav1/pczspa
_nottingham_internal_self_archive_date 12/10/2016
_nottingham_internal_self_validation_date 12/10/2016
_nottingham_internal_self_validation_user pcxav1
_nottingham_internal_validation_date 28/04/2020
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date ?
_refine_special_details          
;
 Conformational disorder is modelled for the fluorine atoms
 of the two CF3 moieties. The occupancies of the pairs of
 disorder components are refined and contrained to sum to
 unit. In both pairs disorder components the minor occupancy
 component fluorine atoms are refined with isotropic
 displacement parameters. Similarity and rigid bond restraints
 (SIMU, RIGU) have been applied to all the atoms of the
 disordered CF3 moieties. The C-F and F...F distances of
 the disordered moieties are restrained to be similar to
 reflect their three-fold symmetry (SADI).
;
_audit_creation_date             2020-06-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C23 H20 F3 I'
_chemical_formula_sum            'C23 H20 F3 I'
_chemical_formula_weight         480.29
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C23 H20 F3 I1'
_chemical_oxdiff_usercomment     
'OAJVLE #16535 GVB-1177 IN FOMBLIN FILM ON MICROMOUNT FOR AJV/DLK'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.51060(10)
_cell_length_b                   35.0225(4)
_cell_length_c                   13.61300(10)
_cell_angle_alpha                90
_cell_angle_beta                 99.1350(10)
_cell_angle_gamma                90
_cell_volume                     4006.06(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    32590
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.5350
_cell_measurement_theta_min      4.1350
_shelx_estimated_absorpt_T_max   0.354
_shelx_estimated_absorpt_T_min   0.067
_exptl_absorpt_coefficient_mu    12.836
_exptl_absorpt_correction_T_max  0.461
_exptl_absorpt_correction_T_min  0.074
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1904
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 6 -7 0.0728
3 6 -8 0.0777
4 -1 4 0.1065
-4 -6 7 0.1125
1 -22 0 0.0426
1 21 -2 0.0415
2 -16 -5 0.0767
2 -7 -8 0.1130
-5 8 5 0.1050
-1 22 2 0.0674
3 -17 3 0.0865
-2 -21 2 0.0579
1 22 2 0.0553
2 6 -8 0.1084
-4 15 4 0.0875
-4 -14 5 0.0684

_exptl_crystal_recrystallization_method 
'Recrystallised from diethyl ether by slow evapouration at room temperature.'
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.102
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.0000 6.0690 -6.9952 0.1670 -0.7590 0.5225
3.0000 6.0725 -7.9945 0.1609 -0.8731 0.5154
3.9965 -0.9618 3.9916 -0.0895 0.5338 0.7492
-3.9992 -6.0823 6.9964 -0.1495 0.7403 -0.7039
0.9925 -22.0055 -0.0144 -0.9790 0.0769 0.0778
1.0058 21.0380 -1.9873 0.8881 -0.2653 0.2660
1.9939 -15.9698 -5.0085 -0.7648 -0.4911 0.2518
1.9968 -6.9518 -8.0010 -0.3897 -0.8573 0.2729
-4.9941 7.9233 5.0075 0.4677 0.4563 -0.8336
-0.9926 21.9986 2.0130 0.9912 0.1514 -0.0636
2.9924 -16.9852 2.9840 -0.7773 0.4434 0.4854
-2.0051 -21.0512 1.9885 -0.8705 0.2466 -0.4474
1.0059 22.0250 2.0105 0.9561 0.1887 0.2992
2.0008 6.0593 -7.9932 0.1784 -0.8918 0.3341
-3.9926 14.9460 4.0111 0.7501 0.3423 -0.6264
-4.0016 -14.0821 4.9931 -0.5113 0.5333 -0.7558

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            61587
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.735
_diffrn_reflns_theta_min         3.522
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -94.00  -2.00   1.00    2.00    --  -38.50 125.00 -60.00   92
  2  ω   -112.00  -7.00   1.00    2.00    --  -38.50 -77.00-150.00  105
  3  ω    -50.00  34.00   1.00    2.00    --  -38.50  38.00 150.00   84
  4  ω     33.00 122.00   1.00    8.00    --  104.50-125.00  30.00   89
  5  ω     33.00 122.00   1.00    8.00    --  104.50-125.00 -30.00   89
  6  ω     23.00 109.00   1.00    8.00    --  104.50 -94.00 120.00   86
  7  ω     59.00 178.00   1.00    8.00    --  104.50  15.00  60.00  119
  8  ω     81.00 178.00   1.00    8.00    --  104.50  30.00 120.00   97
  9  ω     34.00 132.00   1.00    8.00    --  104.50 -61.00 -30.00   98
 10  ω     30.00  91.00   1.00    8.00    --  104.50 -30.00 150.00   61
 11  ω     20.00 115.00   1.00    2.00    --   42.83  38.00 -60.00   95
 12  ω     16.00 113.00   1.00    2.00    --   42.83  57.00 120.00   97
 13  ω     11.00 117.00   1.00    2.00    --   42.83  77.00   0.00  106
 14  ω     30.00  91.00   1.00    8.00    --  104.50 -30.00  90.00   61
 15  ω     77.00 175.00   1.00    8.00    --  104.50  61.00-180.00   98
 16  ω     73.00 178.00   1.00    8.00    --  104.50  77.00 -60.00  105
 17  ω     73.00 178.00   1.00    8.00    --  104.50  77.00  30.00  105
 18  ω     80.00 176.00   1.00    8.00    --  104.50  45.00 150.00   96
 19  ω     59.00 178.00   1.00    8.00    --  104.50  15.00 -60.00  119
 20  ω    -94.00  -2.00   1.00    2.00    --  -38.50 125.00 120.00   92
 21  ω     57.00 113.00   1.00    2.00    --   42.83 151.00  18.00   56
 22  ω     11.00 117.00   1.00    2.00    --   42.83  77.00 150.00  106
 23  ω     73.00 178.00   1.00    8.00    --  104.50  77.00  90.00  105
 24  ω     23.00 109.00   1.00    8.00    --  104.50 -94.00-150.00   86
 25  ω     77.00 164.00   1.00    8.00    --  104.50  61.00 -90.00   87
 26  ω     73.00 178.00   1.00    8.00    --  104.50  77.00-150.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0181176000
_diffrn_orient_matrix_UB_12      0.0436686000
_diffrn_orient_matrix_UB_13      0.0062440000
_diffrn_orient_matrix_UB_21      0.0188279000
_diffrn_orient_matrix_UB_22      -0.0027203000
_diffrn_orient_matrix_UB_23      0.1142154000
_diffrn_orient_matrix_UB_31      0.1814425000
_diffrn_orient_matrix_UB_32      0.0046442000
_diffrn_orient_matrix_UB_33      0.0071440000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7747
_reflns_number_total             8027
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.045
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         8027
_refine_ls_number_restraints     636
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0450
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+28.1091P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0905
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F5A-C46 \\sim F5-C46 \\sim F6A-C46 \\sim F6-C46 \\sim F4A-C46 \\sim F4-C46
 with sigma of 0.02
 F4-F6 \\sim F6-F5 \\sim F5-F4 \\sim F4A-F6A \\sim F6A-F5A \\sim F5A-F4A
 with sigma of 0.02
 F1A-C23 \\sim F1-C23 \\sim F3A-C23 \\sim F3-C23 \\sim F2A-C23 \\sim F2-C23
 with sigma of 0.02
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1A-F2A \\sim F2A-F3A \\sim F3A-F1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F6 \\sim F6A \\sim F5 \\sim F5A \\sim F4 \\sim F4A: within 2.5A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2.5A
F1A \\sim F1 \\sim F3A \\sim F3 \\sim F2A \\sim F2: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
F1A \\sim F1 \\sim F2 \\sim F2A \\sim F3 \\sim F3A: within 2.5A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2.5A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F4A)=Sof(F6A)=Sof(F5A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F1A)=Sof(F3A)=Sof(F2A)=1-FVAR(2)
 Sof(F3)=Sof(F1)=Sof(F2)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C3(H3), C26(H26), C32(H32), C33(H33), C42(H42), C9(H9), C5(H5),
 C41(H41), C34(H34), C17(H17), C40(H40), C11(H11), C18(H18), C19(H19), C10(H10)
6.b Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C45(H45a,H45b,H45c), C44(H44a,H44b,H44c), C21(H21a,H21b,
 H21c), C36(H36a,H36b,H36c), C14(H14a,H14b,H14c), C37(H37a,H37b,H37c), C13(H13a,
 H13b,H13c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
I2 I 0.90154(4) 0.74444(2) 0.47936(2) 0.02103(8) Uani 1 1 d . . . . .
I1 I 0.25778(4) 0.51690(2) 0.02430(2) 0.02546(8) Uani 1 1 d . . . . .
F3 F 0.3142(7) 0.59764(17) 0.4946(5) 0.0261(11) Uani 0.801(19) 1 d D U P A 1
F4 F 0.7855(5) 0.54991(13) 0.3964(6) 0.0315(13) Uani 0.88(2) 1 d D U P B 1
F5 F 1.0377(6) 0.54855(16) 0.4406(7) 0.0362(12) Uani 0.88(2) 1 d D U P B 1
F6 F 0.8837(13) 0.54625(10) 0.5514(3) 0.0366(17) Uani 0.88(2) 1 d D U P B 1
F1 F 0.3745(11) 0.53999(11) 0.5404(3) 0.0393(17) Uani 0.801(19) 1 d D U P A 1
F2 F 0.5549(5) 0.5787(3) 0.5087(5) 0.0463(18) Uani 0.801(19) 1 d D U P A 1
C29 C 0.9273(5) 0.66574(13) 0.3881(3) 0.0173(8) Uani 1 1 d . . . . .
C1 C 0.3106(5) 0.53379(13) 0.1741(3) 0.0192(9) Uani 1 1 d . . . . .
C25 C 0.8838(5) 0.66407(13) 0.5622(3) 0.0169(8) Uani 1 1 d . . . . .
C28 C 0.9279(5) 0.62613(13) 0.3879(3) 0.0192(9) Uani 1 1 d . . . . .
H28 H 0.943626 0.612868 0.329358 0.023 Uiso 1 1 calc R U . . .
C3 C 0.3953(6) 0.58149(13) 0.2959(4) 0.0231(9) Uani 1 1 d . . . . .
H3 H 0.431929 0.606563 0.313594 0.028 Uiso 1 1 calc R U . . .
C30 C 0.8589(5) 0.68332(12) 0.6569(3) 0.0171(8) Uani 1 1 d . . . . .
C24 C 0.9046(5) 0.68421(12) 0.4762(3) 0.0164(8) Uani 1 1 d . . . . .
C4 C 0.3748(5) 0.55554(14) 0.3702(3) 0.0216(9) Uani 1 1 d . . . . .
C15 C 0.2324(6) 0.46740(13) 0.2224(3) 0.0205(9) Uani 1 1 d . . . . .
C6 C 0.2906(5) 0.50704(13) 0.2476(3) 0.0188(9) Uani 1 1 d . . . . .
C35 C 0.7033(6) 0.68732(13) 0.6778(3) 0.0205(9) Uani 1 1 d . . . . .
C31 C 0.9908(6) 0.69529(13) 0.7259(3) 0.0206(9) Uani 1 1 d . . . . .
C26 C 0.8846(5) 0.62439(13) 0.5583(3) 0.0194(9) Uani 1 1 d . . . . .
H26 H 0.870466 0.610067 0.615517 0.023 Uiso 1 1 calc R U . . .
C32 C 0.9637(6) 0.71125(13) 0.8150(3) 0.0266(10) Uani 1 1 d . . . . .
H32 H 1.051365 0.719873 0.861848 0.032 Uiso 1 1 calc R U . . .
C38 C 0.9517(6) 0.68621(12) 0.2955(3) 0.0184(8) Uani 1 1 d . . . . .
C12 C 0.2536(6) 0.62046(13) 0.0708(4) 0.0246(10) Uani 1 1 d . . . . .
C33 C 0.8113(7) 0.71477(14) 0.8367(4) 0.0289(10) Uani 1 1 d . . . . .
H33 H 0.795153 0.725251 0.898681 0.035 Uiso 1 1 calc R U . . .
C43 C 1.1074(6) 0.69311(13) 0.2785(3) 0.0210(9) Uani 1 1 d . . . . .
C23 C 0.4063(6) 0.56830(13) 0.4760(4) 0.0275(10) Uani 1 1 d D . . . .
C42 C 1.1295(6) 0.70988(14) 0.1885(4) 0.0260(10) Uani 1 1 d . . . . .
H42 H 1.234183 0.714868 0.175885 0.031 Uiso 1 1 calc R U . . .
C27 C 0.9056(5) 0.60552(13) 0.4720(3) 0.0196(9) Uani 1 1 d . . . . .
C39 C 0.8201(6) 0.69613(13) 0.2244(3) 0.0222(9) Uani 1 1 d . . . . .
C9 C 0.5555(7) 0.63092(15) 0.0183(4) 0.0309(11) Uani 1 1 d . . . . .
H9 H 0.658028 0.634886 0.000913 0.037 Uiso 1 1 calc R U . . .
C46 C 0.9051(5) 0.56284(13) 0.4665(3) 0.0234(9) Uani 1 1 d D . . . .
C20 C 0.3406(6) 0.43828(14) 0.2105(3) 0.0247(10) Uani 1 1 d . . . . .
C2 C 0.3629(5) 0.57115(13) 0.1962(3) 0.0208(9) Uani 1 1 d . . . . .
C22 C 0.5163(6) 0.44586(16) 0.2184(4) 0.0325(11) Uani 1 1 d . . . . .
H22A H 0.540034 0.454449 0.153802 0.049 Uiso 1 1 calc R U . . .
H22B H 0.575550 0.422362 0.238104 0.049 Uiso 1 1 calc R U . . .
H22C H 0.547788 0.465704 0.268409 0.049 Uiso 1 1 calc R U . . .
C5 C 0.3244(5) 0.51878(13) 0.3466(3) 0.0210(9) Uani 1 1 d . . . . .
H5 H 0.312665 0.501275 0.398233 0.025 Uiso 1 1 calc R U . . .
C45 C 1.2476(6) 0.68350(15) 0.3566(4) 0.0301(11) Uani 1 1 d . . . . .
H45A H 1.242876 0.698732 0.416492 0.045 Uiso 1 1 calc R U . . .
H45B H 1.346479 0.689231 0.331207 0.045 Uiso 1 1 calc R U . . .
H45C H 1.244800 0.656297 0.373095 0.045 Uiso 1 1 calc R U . . .
C41 C 1.0003(7) 0.71927(14) 0.1176(4) 0.0296(11) Uani 1 1 d . . . . .
H41 H 1.016814 0.730200 0.056186 0.036 Uiso 1 1 calc R U . . .
C44 C 0.6523(6) 0.68980(15) 0.2437(4) 0.0287(11) Uani 1 1 d . . . . .
H44A H 0.637138 0.662712 0.257670 0.043 Uiso 1 1 calc R U . . .
H44B H 0.576832 0.697432 0.184936 0.043 Uiso 1 1 calc R U . . .
H44C H 0.633855 0.705131 0.301000 0.043 Uiso 1 1 calc R U . . .
C7 C 0.3841(6) 0.59949(13) 0.1171(3) 0.0218(9) Uani 1 1 d . . . . .
C8 C 0.5362(6) 0.60439(14) 0.0917(4) 0.0251(10) Uani 1 1 d . . . . .
C16 C 0.0681(6) 0.46013(14) 0.2112(3) 0.0231(9) Uani 1 1 d . . . . .
C34 C 0.6823(6) 0.70314(14) 0.7687(4) 0.0255(10) Uani 1 1 d . . . . .
H34 H 0.577912 0.705963 0.784146 0.031 Uiso 1 1 calc R U . . .
C17 C 0.0141(7) 0.42332(14) 0.1860(4) 0.0283(10) Uani 1 1 d . . . . .
H17 H -0.096783 0.418058 0.176439 0.034 Uiso 1 1 calc R U . . .
C21 C -0.0471(6) 0.49148(15) 0.2254(4) 0.0290(11) Uani 1 1 d . . . . .
H21A H -0.021372 0.501650 0.293140 0.044 Uiso 1 1 calc R U . . .
H21B H -0.155646 0.481249 0.215036 0.044 Uiso 1 1 calc R U . . .
H21C H -0.039278 0.511947 0.177361 0.044 Uiso 1 1 calc R U . . .
C40 C 0.8472(6) 0.71284(14) 0.1357(4) 0.0280(10) Uani 1 1 d . . . . .
H40 H 0.759294 0.719889 0.086977 0.034 Uiso 1 1 calc R U . . .
C11 C 0.2766(7) 0.64661(14) -0.0032(4) 0.0319(11) Uani 1 1 d . . . . .
H11 H 0.189243 0.661092 -0.035770 0.038 Uiso 1 1 calc R U . . .
C36 C 1.1579(6) 0.69035(16) 0.7051(4) 0.0304(11) Uani 1 1 d . . . . .
H36A H 1.183767 0.663091 0.704541 0.046 Uiso 1 1 calc R U . . .
H36B H 1.232304 0.703222 0.756929 0.046 Uiso 1 1 calc R U . . .
H36C H 1.166662 0.701525 0.640143 0.046 Uiso 1 1 calc R U . . .
C14 C 0.0890(6) 0.61443(15) 0.0959(4) 0.0312(11) Uani 1 1 d . . . . .
H14A H 0.047712 0.589716 0.069688 0.047 Uiso 1 1 calc R U . . .
H14B H 0.018471 0.634868 0.066014 0.047 Uiso 1 1 calc R U . . .
H14C H 0.093884 0.614803 0.168306 0.047 Uiso 1 1 calc R U . . .
C18 C 0.1201(7) 0.39437(14) 0.1746(4) 0.0317(11) Uani 1 1 d . . . . .
H18 H 0.081822 0.369381 0.157417 0.038 Uiso 1 1 calc R U . . .
C19 C 0.2814(7) 0.40171(14) 0.1881(4) 0.0298(11) Uani 1 1 d . . . . .
H19 H 0.353365 0.381430 0.182060 0.036 Uiso 1 1 calc R U . . .
C37 C 0.5619(6) 0.67490(16) 0.6043(4) 0.0317(11) Uani 1 1 d . . . . .
H37A H 0.573890 0.683885 0.537738 0.048 Uiso 1 1 calc R U . . .
H37B H 0.464804 0.685740 0.623158 0.048 Uiso 1 1 calc R U . . .
H37C H 0.554864 0.646971 0.604138 0.048 Uiso 1 1 calc R U . . .
C10 C 0.4273(7) 0.65155(15) -0.0295(4) 0.0345(12) Uani 1 1 d . . . . .
H10 H 0.441737 0.669136 -0.080480 0.041 Uiso 1 1 calc R U . . .
C13 C 0.6759(6) 0.58099(17) 0.1400(4) 0.0366(12) Uani 1 1 d . . . . .
H13A H 0.768573 0.586494 0.107841 0.055 Uiso 1 1 calc R U . . .
H13B H 0.649629 0.553784 0.132750 0.055 Uiso 1 1 calc R U . . .
H13C H 0.700419 0.587454 0.210823 0.055 Uiso 1 1 calc R U . . .
F4A F 0.774(2) 0.5446(11) 0.429(3) 0.036(5) Uiso 0.12(2) 1 d D U P B 2
F6A F 0.955(5) 0.5481(10) 0.5580(12) 0.036(5) Uiso 0.12(2) 1 d D U P B 2
F5A F 1.018(3) 0.5521(12) 0.412(2) 0.029(5) Uiso 0.12(2) 1 d D U P B 2
F1A F 0.450(3) 0.5420(4) 0.5409(13) 0.032(4) Uiso 0.199(19) 1 d D U P A 2
F3A F 0.295(2) 0.5905(6) 0.505(2) 0.032(5) Uiso 0.199(19) 1 d D U P A 2
F2A F 0.537(2) 0.5934(5) 0.4823(16) 0.028(4) Uiso 0.199(19) 1 d D U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I2 C24 2.110(4) . ?
I1 C1 2.103(4) . ?
F3 C23 1.341(6) . ?
F4 C46 1.357(6) . ?
F5 C46 1.332(6) . ?
F6 C46 1.332(5) . ?
F1 C23 1.378(7) . ?
F2 C23 1.323(6) . ?
C29 C28 1.387(6) . ?
C29 C24 1.403(6) . ?
C29 C38 1.494(6) . ?
C1 C6 1.400(6) . ?
C1 C2 1.399(6) . ?
C25 C30 1.499(6) . ?
C25 C24 1.402(6) . ?
C25 C26 1.391(6) . ?
C28 H28 0.9500 . ?
C28 C27 1.391(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.391(7) . ?
C3 C2 1.389(6) . ?
C30 C35 1.406(6) . ?
C30 C31 1.408(6) . ?
C4 C23 1.492(6) . ?
C4 C5 1.379(7) . ?
C15 C6 1.495(6) . ?
C15 C20 1.401(7) . ?
C15 C16 1.405(7) . ?
C6 C5 1.395(6) . ?
C35 C34 1.393(6) . ?
C35 C37 1.502(7) . ?
C31 C32 1.389(6) . ?
C31 C36 1.504(7) . ?
C26 H26 0.9500 . ?
C26 C27 1.385(6) . ?
C32 H32 0.9500 . ?
C32 C33 1.381(8) . ?
C38 C43 1.402(7) . ?
C38 C39 1.403(6) . ?
C12 C7 1.395(7) . ?
C12 C11 1.398(7) . ?
C12 C14 1.509(7) . ?
C33 H33 0.9500 . ?
C33 C34 1.380(7) . ?
C43 C42 1.398(6) . ?
C43 C45 1.505(7) . ?
C23 F1A 1.289(11) . ?
C23 F3A 1.334(13) . ?
C23 F2A 1.408(11) . ?
C42 H42 0.9500 . ?
C42 C41 1.382(7) . ?
C27 C46 1.497(6) . ?
C39 C44 1.509(7) . ?
C39 C40 1.394(7) . ?
C9 H9 0.9500 . ?
C9 C8 1.393(7) . ?
C9 C10 1.383(8) . ?
C46 F4A 1.320(14) . ?
C46 F6A 1.354(13) . ?
C46 F5A 1.351(14) . ?
C20 C22 1.506(7) . ?
C20 C19 1.392(7) . ?
C2 C7 1.497(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C5 H5 0.9500 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C41 H41 0.9500 . ?
C41 C40 1.382(8) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C7 C8 1.403(7) . ?
C8 C13 1.506(7) . ?
C16 C17 1.394(7) . ?
C16 C21 1.505(7) . ?
C34 H34 0.9500 . ?
C17 H17 0.9500 . ?
C17 C18 1.382(8) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C40 H40 0.9500 . ?
C11 H11 0.9500 . ?
C11 C10 1.396(8) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C18 H18 0.9500 . ?
C18 C19 1.380(8) . ?
C19 H19 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C10 H10 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C28 C29 C24 117.6(4) . . ?
C28 C29 C38 118.5(4) . . ?
C24 C29 C38 123.9(4) . . ?
C6 C1 I1 118.2(3) . . ?
C2 C1 I1 118.9(3) . . ?
C2 C1 C6 122.9(4) . . ?
C24 C25 C30 123.0(4) . . ?
C26 C25 C30 119.0(4) . . ?
C26 C25 C24 118.0(4) . . ?
C29 C28 H28 119.5 . . ?
C29 C28 C27 121.1(4) . . ?
C27 C28 H28 119.5 . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C2 C3 C4 120.7(4) . . ?
C35 C30 C25 119.0(4) . . ?
C35 C30 C31 120.8(4) . . ?
C31 C30 C25 120.1(4) . . ?
C29 C24 I2 118.8(3) . . ?
C25 C24 I2 118.9(3) . . ?
C25 C24 C29 122.3(4) . . ?
C3 C4 C23 118.8(4) . . ?
C5 C4 C3 120.7(4) . . ?
C5 C4 C23 120.4(4) . . ?
C20 C15 C6 120.2(4) . . ?
C20 C15 C16 121.1(4) . . ?
C16 C15 C6 118.7(4) . . ?
C1 C6 C15 122.1(4) . . ?
C5 C6 C1 117.6(4) . . ?
C5 C6 C15 120.3(4) . . ?
C30 C35 C37 121.2(4) . . ?
C34 C35 C30 118.5(4) . . ?
C34 C35 C37 120.3(4) . . ?
C30 C31 C36 121.2(4) . . ?
C32 C31 C30 118.5(4) . . ?
C32 C31 C36 120.3(4) . . ?
C25 C26 H26 119.6 . . ?
C27 C26 C25 120.8(4) . . ?
C27 C26 H26 119.6 . . ?
C31 C32 H32 119.5 . . ?
C33 C32 C31 121.0(5) . . ?
C33 C32 H32 119.5 . . ?
C43 C38 C29 118.9(4) . . ?
C43 C38 C39 121.1(4) . . ?
C39 C38 C29 119.9(4) . . ?
C7 C12 C11 118.5(5) . . ?
C7 C12 C14 121.7(4) . . ?
C11 C12 C14 119.8(5) . . ?
C32 C33 H33 119.8 . . ?
C34 C33 C32 120.3(5) . . ?
C34 C33 H33 119.8 . . ?
C38 C43 C45 120.6(4) . . ?
C42 C43 C38 118.6(4) . . ?
C42 C43 C45 120.8(4) . . ?
F3 C23 F1 104.6(5) . . ?
F3 C23 C4 113.0(4) . . ?
F1 C23 C4 112.0(4) . . ?
F2 C23 F3 106.4(5) . . ?
F2 C23 F1 104.9(5) . . ?
F2 C23 C4 115.0(4) . . ?
F1A C23 C4 115.9(9) . . ?
F1A C23 F3A 110.9(12) . . ?
F1A C23 F2A 105.4(9) . . ?
F3A C23 C4 115.5(15) . . ?
F3A C23 F2A 102.1(10) . . ?
F2A C23 C4 105.3(9) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 C43 120.6(5) . . ?
C41 C42 H42 119.7 . . ?
C28 C27 C46 118.5(4) . . ?
C26 C27 C28 120.2(4) . . ?
C26 C27 C46 121.3(4) . . ?
C38 C39 C44 121.2(4) . . ?
C40 C39 C38 118.5(5) . . ?
C40 C39 C44 120.3(4) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C10 C9 C8 120.8(5) . . ?
F4 C46 C27 111.4(4) . . ?
F5 C46 F4 105.2(4) . . ?
F5 C46 F6 107.7(4) . . ?
F5 C46 C27 113.1(4) . . ?
F6 C46 F4 105.9(4) . . ?
F6 C46 C27 113.1(4) . . ?
F4A C46 C27 120.0(18) . . ?
F4A C46 F6A 107.1(13) . . ?
F4A C46 F5A 106.6(14) . . ?
F6A C46 C27 109.7(15) . . ?
F5A C46 C27 108.0(18) . . ?
F5A C46 F6A 104.4(13) . . ?
C15 C20 C22 121.8(4) . . ?
C19 C20 C15 118.3(5) . . ?
C19 C20 C22 119.9(5) . . ?
C1 C2 C7 122.4(4) . . ?
C3 C2 C1 117.4(4) . . ?
C3 C2 C7 120.2(4) . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C4 C5 C6 120.6(4) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C41 H41 119.8 . . ?
C42 C41 C40 120.3(5) . . ?
C40 C41 H41 119.8 . . ?
C39 C44 H44A 109.5 . . ?
C39 C44 H44B 109.5 . . ?
C39 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C12 C7 C2 119.7(4) . . ?
C12 C7 C8 121.6(5) . . ?
C8 C7 C2 118.6(4) . . ?
C9 C8 C7 118.4(5) . . ?
C9 C8 C13 120.1(5) . . ?
C7 C8 C13 121.5(5) . . ?
C15 C16 C21 120.7(4) . . ?
C17 C16 C15 118.5(5) . . ?
C17 C16 C21 120.7(5) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 C35 120.8(5) . . ?
C33 C34 H34 119.6 . . ?
C16 C17 H17 119.6 . . ?
C18 C17 C16 120.7(5) . . ?
C18 C17 H17 119.6 . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C39 C40 H40 119.6 . . ?
C41 C40 C39 120.9(5) . . ?
C41 C40 H40 119.6 . . ?
C12 C11 H11 119.8 . . ?
C10 C11 C12 120.4(5) . . ?
C10 C11 H11 119.8 . . ?
C31 C36 H36A 109.5 . . ?
C31 C36 H36B 109.5 . . ?
C31 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C17 C18 H18 119.9 . . ?
C19 C18 C17 120.1(5) . . ?
C19 C18 H18 119.9 . . ?
C20 C19 H19 119.4 . . ?
C18 C19 C20 121.2(5) . . ?
C18 C19 H19 119.4 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C9 C10 C11 120.2(5) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
I1 C1 C6 C15 -0.4(6) . . . . ?
I1 C1 C6 C5 -179.3(3) . . . . ?
I1 C1 C2 C3 179.4(3) . . . . ?
I1 C1 C2 C7 -0.6(6) . . . . ?
C29 C28 C27 C26 -0.8(7) . . . . ?
C29 C28 C27 C46 179.1(4) . . . . ?
C29 C38 C43 C42 175.6(4) . . . . ?
C29 C38 C43 C45 -5.9(6) . . . . ?
C29 C38 C39 C44 5.7(7) . . . . ?
C29 C38 C39 C40 -175.6(4) . . . . ?
C1 C6 C5 C4 0.4(7) . . . . ?
C1 C2 C7 C12 84.2(6) . . . . ?
C1 C2 C7 C8 -96.1(6) . . . . ?
C25 C30 C35 C34 176.1(4) . . . . ?
C25 C30 C35 C37 -3.8(6) . . . . ?
C25 C30 C31 C32 -176.7(4) . . . . ?
C25 C30 C31 C36 2.1(7) . . . . ?
C25 C26 C27 C28 0.6(7) . . . . ?
C25 C26 C27 C46 -179.4(4) . . . . ?
C28 C29 C24 I2 -179.6(3) . . . . ?
C28 C29 C24 C25 0.3(7) . . . . ?
C28 C29 C38 C43 -85.4(5) . . . . ?
C28 C29 C38 C39 90.8(5) . . . . ?
C28 C27 C46 F4 -61.3(6) . . . . ?
C28 C27 C46 F5 56.9(7) . . . . ?
C28 C27 C46 F6 179.7(6) . . . . ?
C28 C27 C46 F4A -84(2) . . . . ?
C28 C27 C46 F6A 152(2) . . . . ?
C28 C27 C46 F5A 38.8(18) . . . . ?
C3 C4 C23 F3 59.7(7) . . . . ?
C3 C4 C23 F1 177.5(6) . . . . ?
C3 C4 C23 F2 -62.8(8) . . . . ?
C3 C4 C23 F1A -152.4(13) . . . . ?
C3 C4 C23 F3A 75.5(13) . . . . ?
C3 C4 C23 F2A -36.4(11) . . . . ?
C3 C4 C5 C6 -1.0(7) . . . . ?
C3 C2 C7 C12 -95.7(5) . . . . ?
C3 C2 C7 C8 83.9(6) . . . . ?
C30 C25 C24 I2 0.1(6) . . . . ?
C30 C25 C24 C29 -179.8(4) . . . . ?
C30 C25 C26 C27 179.4(4) . . . . ?
C30 C35 C34 C33 0.2(7) . . . . ?
C30 C31 C32 C33 1.1(7) . . . . ?
C24 C29 C28 C27 0.4(7) . . . . ?
C24 C29 C38 C43 94.3(5) . . . . ?
C24 C29 C38 C39 -89.6(6) . . . . ?
C24 C25 C30 C35 98.1(5) . . . . ?
C24 C25 C30 C31 -85.3(5) . . . . ?
C24 C25 C26 C27 0.1(7) . . . . ?
C4 C3 C2 C1 -0.5(7) . . . . ?
C4 C3 C2 C7 179.4(4) . . . . ?
C15 C6 C5 C4 -178.5(4) . . . . ?
C15 C20 C19 C18 2.2(7) . . . . ?
C15 C16 C17 C18 1.6(7) . . . . ?
C6 C1 C2 C3 -0.1(7) . . . . ?
C6 C1 C2 C7 179.9(4) . . . . ?
C6 C15 C20 C22 -2.3(7) . . . . ?
C6 C15 C20 C19 179.3(4) . . . . ?
C6 C15 C16 C17 178.8(4) . . . . ?
C6 C15 C16 C21 -0.7(6) . . . . ?
C35 C30 C31 C32 -0.2(7) . . . . ?
C35 C30 C31 C36 178.7(4) . . . . ?
C31 C30 C35 C34 -0.5(7) . . . . ?
C31 C30 C35 C37 179.5(4) . . . . ?
C31 C32 C33 C34 -1.4(7) . . . . ?
C26 C25 C30 C35 -81.2(5) . . . . ?
C26 C25 C30 C31 95.5(5) . . . . ?
C26 C25 C24 I2 179.4(3) . . . . ?
C26 C25 C24 C29 -0.6(7) . . . . ?
C26 C27 C46 F4 118.7(6) . . . . ?
C26 C27 C46 F5 -123.1(6) . . . . ?
C26 C27 C46 F6 -0.3(8) . . . . ?
C26 C27 C46 F4A 96(2) . . . . ?
C26 C27 C46 F6A -28(2) . . . . ?
C26 C27 C46 F5A -141.2(18) . . . . ?
C32 C33 C34 C35 0.7(7) . . . . ?
C38 C29 C28 C27 -180.0(4) . . . . ?
C38 C29 C24 I2 0.7(6) . . . . ?
C38 C29 C24 C25 -179.3(4) . . . . ?
C38 C43 C42 C41 -0.3(7) . . . . ?
C38 C39 C40 C41 0.5(7) . . . . ?
C12 C7 C8 C9 -0.1(7) . . . . ?
C12 C7 C8 C13 -178.4(5) . . . . ?
C12 C11 C10 C9 -0.8(8) . . . . ?
C43 C38 C39 C44 -178.2(4) . . . . ?
C43 C38 C39 C40 0.5(7) . . . . ?
C43 C42 C41 C40 1.2(8) . . . . ?
C23 C4 C5 C6 178.2(4) . . . . ?
C42 C41 C40 C39 -1.3(8) . . . . ?
C39 C38 C43 C42 -0.5(7) . . . . ?
C39 C38 C43 C45 178.0(4) . . . . ?
C20 C15 C6 C1 88.5(6) . . . . ?
C20 C15 C6 C5 -92.7(5) . . . . ?
C20 C15 C16 C17 -1.2(7) . . . . ?
C20 C15 C16 C21 179.3(4) . . . . ?
C2 C1 C6 C15 179.1(4) . . . . ?
C2 C1 C6 C5 0.2(7) . . . . ?
C2 C3 C4 C23 -178.2(4) . . . . ?
C2 C3 C4 C5 1.1(7) . . . . ?
C2 C7 C8 C9 -179.7(4) . . . . ?
C2 C7 C8 C13 1.9(7) . . . . ?
C22 C20 C19 C18 -176.1(4) . . . . ?
C5 C4 C23 F3 -119.6(6) . . . . ?
C5 C4 C23 F1 -1.8(7) . . . . ?
C5 C4 C23 F2 117.9(7) . . . . ?
C5 C4 C23 F1A 28.3(14) . . . . ?
C5 C4 C23 F3A -103.8(12) . . . . ?
C5 C4 C23 F2A 144.3(10) . . . . ?
C45 C43 C42 C41 -178.9(5) . . . . ?
C44 C39 C40 C41 179.1(5) . . . . ?
C7 C12 C11 C10 -0.2(7) . . . . ?
C8 C9 C10 C11 1.4(8) . . . . ?
C16 C15 C6 C1 -91.5(5) . . . . ?
C16 C15 C6 C5 87.3(5) . . . . ?
C16 C15 C20 C22 177.7(4) . . . . ?
C16 C15 C20 C19 -0.7(7) . . . . ?
C16 C17 C18 C19 -0.1(7) . . . . ?
C17 C18 C19 C20 -1.9(7) . . . . ?
C21 C16 C17 C18 -178.9(4) . . . . ?
C11 C12 C7 C2 -179.7(4) . . . . ?
C11 C12 C7 C8 0.7(7) . . . . ?
C36 C31 C32 C33 -177.8(5) . . . . ?
C14 C12 C7 C2 -2.1(7) . . . . ?
C14 C12 C7 C8 178.2(4) . . . . ?
C14 C12 C11 C10 -177.8(5) . . . . ?
C37 C35 C34 C33 -179.8(5) . . . . ?
C10 C9 C8 C7 -0.9(7) . . . . ?
C10 C9 C8 C13 177.4(5) . . . . ?

_olex2_date_sample_data_collection 2016-10-11
_olex2_date_sample_submission    2016-10-10
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_original_sample_id OAJVLE
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.430
_oxdiff_exptl_absorpt_empirical_full_min 0.624
