# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_ahv240
_database_code_depnum_ccdc_archive 'CCDC 1970883'
loop_
_audit_author_name
_audit_author_address
'Sergey Troyanov' 'Moscow State University'
_audit_update_record             
;
2019-12-09 deposited with the CCDC.	2020-04-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H16'
_chemical_formula_weight         424.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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                   42.920(4)
_cell_length_b                   5.1561(4)
_cell_length_c                   18.3460(6)
_cell_angle_alpha                90
_cell_angle_beta                 108.246(3)
_cell_angle_gamma                90
_cell_volume                     3855.8(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19500
_cell_measurement_theta_min      5
_cell_measurement_theta_max      31

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_F_000             1760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    0.113
_shelx_estimated_absorpt_T_min   0.980
_shelx_estimated_absorpt_T_max   1.000
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.8266
_diffrn_radiation_type           synchrotron
_diffrn_source                   'BL 14.2 PSF, BESSY, Berlin, Germany'
_diffrn_measurement_device_type  Pilatus2M
_diffrn_measurement_method       HPC
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27418
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_limit_h_min       -62
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.324
_diffrn_reflns_theta_max         36.909
_diffrn_reflns_theta_full        29.450
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             5512
_reflns_number_gt                4867
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       XDS
_computing_cell_refinement       XDS
_computing_data_reduction        XDS
_computing_structure_solution    SHELXD
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0700P)²+6.5000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5512
_refine_ls_number_parameters     371
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0518
_refine_ls_wR_factor_ref         0.1370
_refine_ls_wR_factor_gt          0.1342
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.09368(3) -0.1440(2) 0.30287(7) 0.0139(2) Uani 1 1 d . . . . .
C2 C 0.10378(3) 0.0531(2) 0.26166(7) 0.0143(2) Uani 1 1 d . . . . .
C3 C 0.07434(3) 0.1525(3) 0.21236(7) 0.0156(2) Uani 1 1 d . . . . .
C4 C 0.07573(3) 0.3545(3) 0.16833(7) 0.0158(2) Uani 1 1 d . . . . .
C5 C 0.10655(3) 0.4438(3) 0.16852(7) 0.0147(2) Uani 1 1 d . . . . .
C6 C 0.09929(3) 0.6425(2) 0.11268(7) 0.0150(2) Uani 1 1 d . . . . .
C7 C 0.12386(3) 0.7760(3) 0.09575(7) 0.0158(2) Uani 1 1 d . . . . .
C8 C 0.11289(3) 0.9802(3) 0.04173(7) 0.0189(3) Uani 1 1 d . . . . .
H8 H 0.1285(5) 1.088(4) 0.0262(11) 0.027(5) Uiso 1 1 d . . . . .
C9 C 0.07947(3) 1.0263(3) 0.01015(8) 0.0198(3) Uani 1 1 d . . . . .
H9 H 0.0718(5) 1.170(4) -0.0280(11) 0.025(5) Uiso 1 1 d . . . . .
C10 C 0.05479(3) 0.8788(3) 0.02785(7) 0.0178(2) Uani 1 1 d . . . . .
H15 H 0.0314(5) 0.922(4) 0.0029(11) 0.024(5) Uiso 1 1 d . . . . .
C11 C 0.06447(3) 0.6795(2) 0.08018(7) 0.0152(2) Uani 1 1 d . . . . .
C12 C 0.04863(3) 0.4778(3) 0.11720(7) 0.0153(2) Uani 1 1 d . . . . .
C13 C 0.01871(3) 0.3700(3) 0.11800(7) 0.0156(2) Uani 1 1 d . . . . .
H13 H -0.0019(4) 0.440(4) 0.0848(10) 0.020(4) Uiso 1 1 d . . . . .
C14 C 0.01716(3) 0.1536(3) 0.16769(7) 0.0151(2) Uani 1 1 d . . . . .
H14 H -0.0050(4) 0.092(4) 0.1645(10) 0.021(4) Uiso 1 1 d . . . . .
C15 C 0.04550(3) 0.0372(2) 0.21710(7) 0.0144(2) Uani 1 1 d . . . . .
C16 C 0.05849(3) -0.1695(2) 0.27803(7) 0.0141(2) Uani 1 1 d . . . . .
C17 C 0.04639(3) -0.3648(3) 0.31264(7) 0.0161(2) Uani 1 1 d . . . . .
H17 H 0.0219(4) -0.398(4) 0.2984(10) 0.023(4) Uiso 1 1 d . . . . .
C18 C 0.06898(3) -0.5242(3) 0.36765(7) 0.0170(2) Uani 1 1 d . . . . .
H18 H 0.0605(5) -0.666(4) 0.3923(11) 0.027(5) Uiso 1 1 d . . . . .
C19 C 0.10281(3) -0.4902(3) 0.39088(7) 0.0166(2) Uani 1 1 d . . . . .
H19 H 0.1156(5) -0.607(4) 0.4280(11) 0.028(5) Uiso 1 1 d . . . . .
C20 C 0.11621(3) -0.2869(2) 0.35819(7) 0.0143(2) Uani 1 1 d . . . . .
C21 C 0.15017(3) -0.1930(2) 0.37703(7) 0.0147(2) Uani 1 1 d . . . . .
C22 C 0.17400(3) -0.2983(3) 0.44152(7) 0.0177(2) Uani 1 1 d . . . . .
H22 H 0.1682(4) -0.446(4) 0.4691(10) 0.021(4) Uiso 1 1 d . . . . .
C23 C 0.20525(3) -0.1965(3) 0.46929(8) 0.0205(3) Uani 1 1 d . . . . .
H23 H 0.2205(5) -0.271(4) 0.5151(12) 0.034(5) Uiso 1 1 d . . . . .
C24 C 0.21348(3) 0.0205(3) 0.43381(8) 0.0199(3) Uani 1 1 d . . . . .
H24 H 0.2352(5) 0.105(4) 0.4527(11) 0.029(5) Uiso 1 1 d . . . . .
C25 C 0.19105(3) 0.1264(3) 0.36918(7) 0.0167(2) Uani 1 1 d . . . . .
H25 H 0.1970(4) 0.283(4) 0.3469(10) 0.019(4) Uiso 1 1 d . . . . .
C26 C 0.15935(3) 0.0215(2) 0.33650(7) 0.0137(2) Uani 1 1 d . . . . .
C27 C 0.13516(3) 0.1406(2) 0.26899(7) 0.0135(2) Uani 1 1 d . . . . .
C28 C 0.13681(3) 0.3475(2) 0.21220(7) 0.0140(2) Uani 1 1 d . . . . .
C29 C 0.16356(3) 0.4609(2) 0.18752(7) 0.0147(2) Uani 1 1 d . . . . .
C30 C 0.19538(3) 0.3528(3) 0.20895(8) 0.0179(3) Uani 1 1 d . . . . .
H30 H 0.1997(4) 0.198(3) 0.2388(10) 0.017(4) Uiso 1 1 d . . . . .
C31 C 0.22044(3) 0.4582(3) 0.18601(8) 0.0219(3) Uani 1 1 d . . . . .
H31 H 0.2425(5) 0.377(4) 0.2002(11) 0.025(5) Uiso 1 1 d . . . . .
C32 C 0.21476(3) 0.6787(3) 0.13960(8) 0.0232(3) Uani 1 1 d . . . . .
H32 H 0.2323(5) 0.759(4) 0.1250(11) 0.027(5) Uiso 1 1 d . . . . .
C33 C 0.18351(3) 0.7817(3) 0.11311(8) 0.0200(3) Uani 1 1 d . . . . .
H33 H 0.1795(5) 0.931(4) 0.0788(11) 0.026(5) Uiso 1 1 d . . . . .
C34 C 0.15708(3) 0.6764(3) 0.13365(7) 0.0156(2) 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
C1 C20 1.3762(16) . ?
C1 C2 1.4132(17) . ?
C1 C16 1.4406(16) . ?
C2 C27 1.3864(16) . ?
C2 C3 1.4004(16) . ?
C3 C4 1.3309(18) . ?
C3 C15 1.4004(17) . ?
C4 C12 1.3977(16) . ?
C4 C5 1.4000(16) . ?
C5 C28 1.3870(16) . ?
C5 C6 1.4127(17) . ?
C6 C7 1.3740(17) . ?
C6 C11 1.4378(17) . ?
C7 C8 1.4213(18) . ?
C7 C34 1.4696(17) . ?
C8 C9 1.3889(19) . ?
C9 C10 1.4216(19) . ?
C10 C11 1.3787(18) . ?
C11 C12 1.5144(18) . ?
C12 C13 1.4035(17) . ?
C13 C14 1.4556(18) . ?
C14 C15 1.4039(16) . ?
C15 C16 1.5186(17) . ?
C16 C17 1.3760(18) . ?
C17 C18 1.4216(18) . ?
C18 C19 1.3904(18) . ?
C19 C20 1.4159(18) . ?
C20 C21 1.4706(17) . ?
C21 C22 1.4082(17) . ?
C21 C26 1.4547(18) . ?
C22 C23 1.3808(19) . ?
C23 C24 1.394(2) . ?
C24 C25 1.3846(18) . ?
C25 C26 1.4112(16) . ?
C26 C27 1.4777(16) . ?
C27 C28 1.5083(17) . ?
C28 C29 1.4801(17) . ?
C29 C30 1.4119(17) . ?
C29 C34 1.4548(18) . ?
C30 C31 1.3834(18) . ?
C31 C32 1.395(2) . ?
C32 C33 1.382(2) . ?
C33 C34 1.4112(17) . ?

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
C20 C1 C2 121.15(11) . . ?
C20 C1 C16 127.54(12) . . ?
C2 C1 C16 111.31(10) . . ?
C27 C2 C3 126.60(12) . . ?
C27 C2 C1 129.30(11) . . ?
C3 C2 C1 104.05(10) . . ?
C4 C3 C15 125.33(12) . . ?
C4 C3 C2 118.40(11) . . ?
C15 C3 C2 116.17(11) . . ?
C3 C4 C12 125.28(12) . . ?
C3 C4 C5 118.54(11) . . ?
C12 C4 C5 116.05(12) . . ?
C28 C5 C4 126.65(12) . . ?
C28 C5 C6 129.25(11) . . ?
C4 C5 C6 104.05(10) . . ?
C7 C6 C5 121.10(11) . . ?
C7 C6 C11 127.69(12) . . ?
C5 C6 C11 111.21(11) . . ?
C6 C7 C8 114.77(12) . . ?
C6 C7 C34 114.67(11) . . ?
C8 C7 C34 130.48(12) . . ?
C9 C8 C7 119.38(12) . . ?
C8 C9 C10 124.01(12) . . ?
C11 C10 C9 118.31(12) . . ?
C10 C11 C6 115.79(12) . . ?
C10 C11 C12 138.12(12) . . ?
C6 C11 C12 106.09(10) . . ?
C4 C12 C13 112.61(11) . . ?
C4 C12 C11 102.55(10) . . ?
C13 C12 C11 144.81(11) . . ?
C12 C13 C14 122.12(11) . . ?
C15 C14 C13 122.13(11) . . ?
C3 C15 C14 112.49(11) . . ?
C3 C15 C16 102.45(10) . . ?
C14 C15 C16 145.04(11) . . ?
C17 C16 C1 115.52(11) . . ?
C17 C16 C15 138.47(11) . . ?
C1 C16 C15 106.00(10) . . ?
C16 C17 C18 118.59(12) . . ?
C19 C18 C17 124.01(12) . . ?
C18 C19 C20 119.16(12) . . ?
C1 C20 C19 115.09(11) . . ?
C1 C20 C21 114.39(11) . . ?
C19 C20 C21 130.41(11) . . ?
C22 C21 C26 118.74(11) . . ?
C22 C21 C20 118.44(12) . . ?
C26 C21 C20 122.52(11) . . ?
C23 C22 C21 121.98(13) . . ?
C22 C23 C24 119.46(12) . . ?
C25 C24 C23 120.43(12) . . ?
C24 C25 C26 122.14(13) . . ?
C25 C26 C21 116.99(11) . . ?
C25 C26 C27 121.86(11) . . ?
C21 C26 C27 120.83(10) . . ?
C2 C27 C26 110.65(11) . . ?
C2 C27 C28 114.68(10) . . ?
C26 C27 C28 134.43(11) . . ?
C5 C28 C29 110.95(11) . . ?
C5 C28 C27 114.48(10) . . ?
C29 C28 C27 134.38(11) . . ?
C30 C29 C34 116.97(11) . . ?
C30 C29 C28 122.28(12) . . ?
C34 C29 C28 120.51(11) . . ?
C31 C30 C29 122.44(13) . . ?
C30 C31 C32 120.12(13) . . ?
C33 C32 C31 119.54(13) . . ?
C32 C33 C34 122.07(13) . . ?
C33 C34 C29 118.46(12) . . ?
C33 C34 C7 118.75(12) . . ?
C29 C34 C7 122.64(11) . . ?

_refine_diff_density_max         0.562
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.063



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2/n-hexane mixture'
####################################################################### 
# 
# 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_ahv241m
_database_code_depnum_ccdc_archive 'CCDC 1970884'
loop_
_audit_author_name
_audit_author_address
'Sergey Troyanov' 'Moscow State University'
_audit_update_record             
;
2019-12-09 deposited with the CCDC.	2020-04-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H16'
_chemical_formula_weight         424.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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                   26.8060(10)
_cell_length_b                   3.7509(3)
_cell_length_c                   20.5591(7)
_cell_angle_alpha                90
_cell_angle_beta                 115.479(7)
_cell_angle_gamma                90
_cell_volume                     1866.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8400
_cell_measurement_theta_min      5
_cell_measurement_theta_max      30

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_F_000             880
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.117
_shelx_estimated_absorpt_T_min   0.997
_shelx_estimated_absorpt_T_max   0.999
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.8266
_diffrn_radiation_type           synchrotron
_diffrn_source                   'BL 14.2 PSF, BESSY, Berlin, Germany'
_diffrn_measurement_device_type  Pilatus2M
_diffrn_measurement_method       HPC
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12174
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.958
_diffrn_reflns_theta_max         36.959
_diffrn_reflns_theta_full        29.450
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measured_fraction_theta_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_point_group_measured_fraction_full 0.953
_reflns_number_total             2552
_reflns_number_gt                2351
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       XDS
_computing_cell_refinement       XDS
_computing_data_reduction        XDS
_computing_structure_solution    SHELXD
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0900P)²+3.1000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2552
_refine_ls_number_parameters     186
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0624
_refine_ls_wR_factor_ref         0.1674
_refine_ls_wR_factor_gt          0.1657
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.11320(5) 0.0846(4) 0.29114(7) 0.0169(3) Uani 1 1 d . . . . .
C2 C 0.06149(5) -0.0247(4) 0.23633(7) 0.0167(3) Uani 1 1 d . . . . .
C3 C 0.02779(5) -0.1035(4) 0.27049(7) 0.0171(3) Uani 1 1 d . . . . .
C4 C 0.05294(5) -0.0142(4) 0.34543(7) 0.0173(3) Uani 1 1 d . . . . .
C5 C 0.11132(5) 0.0873(4) 0.35944(7) 0.0178(3) Uani 1 1 d . . . . .
C6 C 0.15749(6) 0.2192(5) 0.41657(7) 0.0200(3) Uani 1 1 d . . . . .
C7 C 0.20192(6) 0.3500(5) 0.40303(8) 0.0201(3) Uani 1 1 d . . . . .
C8 C 0.20018(6) 0.3680(4) 0.33450(8) 0.0193(3) Uani 1 1 d . . . . .
C9 C 0.15337(5) 0.2376(4) 0.27464(7) 0.0169(3) Uani 1 1 d . . . . .
C10 C 0.13897(5) 0.2685(4) 0.19722(7) 0.0169(3) Uani 1 1 d . . . . .
C11 C 0.17837(6) 0.3907(4) 0.17414(8) 0.0190(3) Uani 1 1 d . . . . .
C12 C 0.16602(6) 0.4282(5) 0.10176(8) 0.0202(3) Uani 1 1 d . . . . .
C13 C 0.11275(6) 0.3536(5) 0.04955(8) 0.0207(3) Uani 1 1 d . . . . .
C14 C 0.07253(6) 0.2410(4) 0.07033(8) 0.0193(3) Uani 1 1 d . . . . .
C15 C 0.08413(5) 0.1898(4) 0.14315(7) 0.0170(3) Uani 1 1 d . . . . .
C16 C 0.04144(5) 0.0573(4) 0.16406(7) 0.0164(3) Uani 1 1 d . . . . .
C17 C -0.01829(6) 0.0608(4) 0.12166(7) 0.0180(3) Uani 1 1 d . . . . .
H6 H 0.1581(9) 0.241(6) 0.4652(12) 0.028(5) Uiso 1 1 d . . . . .
H7 H 0.2341(9) 0.456(6) 0.4450(12) 0.025(5) Uiso 1 1 d . . . . .
H8 H 0.2307(9) 0.486(6) 0.3296(11) 0.022(5) Uiso 1 1 d . . . . .
H11 H 0.2170(9) 0.446(6) 0.2121(11) 0.023(5) Uiso 1 1 d . . . . .
H12 H 0.1942(10) 0.508(7) 0.0855(12) 0.036(6) Uiso 1 1 d . . . . .
H13 H 0.1064(10) 0.379(7) 0.0003(13) 0.037(6) Uiso 1 1 d . . . . .
H14 H 0.0348(8) 0.181(6) 0.0328(11) 0.020(5) Uiso 1 1 d . . . . .
H17 H -0.0335(9) 0.164(6) 0.0720(12) 0.026(5) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C9 1.3848(19) . ?
C1 C2 1.4196(18) . ?
C1 C5 1.4268(19) . ?
C2 C16 1.3799(18) . ?
C2 C3 1.3937(19) . ?
C3 C3 1.360(2) 2 ?
C3 C4 1.4307(19) . ?
C4 C17 1.3930(19) 2 ?
C4 C5 1.5129(19) . ?
C5 C6 1.3802(19) . ?
C6 C7 1.422(2) . ?
C7 C8 1.391(2) . ?
C8 C9 1.4141(19) . ?
C9 C10 1.4722(19) . ?
C10 C11 1.4079(19) . ?
C10 C15 1.4415(18) . ?
C11 C12 1.386(2) . ?
C12 C13 1.397(2) . ?
C13 C14 1.3854(19) . ?
C14 C15 1.4052(19) . ?
C15 C16 1.4714(18) . ?
C16 C17 1.4570(18) . ?
C17 C4 1.3929(19) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 C1 C2 121.46(13) . . ?
C9 C1 C5 126.76(13) . . ?
C2 C1 C5 110.32(12) . . ?
C16 C2 C3 123.58(12) . . ?
C16 C2 C1 125.82(13) . . ?
C3 C2 C1 106.54(12) . . ?
C3 C3 C2 117.56(16) 2 . ?
C3 C3 C4 123.39(16) 2 . ?
C2 C3 C4 112.69(12) . . ?
C17 C4 C3 117.81(12) 2 . ?
C17 C4 C5 135.07(14) 2 . ?
C3 C4 C5 103.51(11) . . ?
C6 C5 C1 116.21(13) . . ?
C6 C5 C4 136.69(13) . . ?
C1 C5 C4 106.41(12) . . ?
C5 C6 C7 118.50(13) . . ?
C8 C7 C6 123.30(13) . . ?
C7 C8 C9 119.68(13) . . ?
C1 C9 C8 115.00(13) . . ?
C1 C9 C10 115.31(12) . . ?
C8 C9 C10 129.45(13) . . ?
C11 C10 C15 118.08(12) . . ?
C11 C10 C9 120.28(12) . . ?
C15 C10 C9 121.59(12) . . ?
C12 C11 C10 121.85(13) . . ?
C11 C12 C13 119.87(13) . . ?
C14 C13 C12 119.88(13) . . ?
C13 C14 C15 121.68(13) . . ?
C14 C15 C10 118.59(12) . . ?
C14 C15 C16 120.94(12) . . ?
C10 C15 C16 120.47(12) . . ?
C2 C16 C17 117.71(12) . . ?
C2 C16 C15 113.47(12) . . ?
C17 C16 C15 127.94(13) . . ?
C4 C17 C16 119.89(13) 2 . ?

_refine_diff_density_max         0.666
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.110



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2/n-hexane mixture'
####################################################################### 
# 
# 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_af84f3
_database_code_depnum_ccdc_archive 'CCDC 1970885'
loop_
_audit_author_name
_audit_author_address
'Sergey Troyanov' 'Moscow State University'
_audit_update_record             
;
2019-12-09 deposited with the CCDC.	2020-04-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46.58 H25.16 Cl1.16'
_chemical_formula_weight         626.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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                   12.7460(10)
_cell_length_b                   24.782(2)
_cell_length_c                   9.4020(10)
_cell_angle_alpha                90
_cell_angle_beta                 91.330(10)
_cell_angle_gamma                90
_cell_volume                     2969.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10000
_cell_measurement_theta_min      5
_cell_measurement_theta_max      30

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_F_000             1298
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.264
_shelx_estimated_absorpt_T_min   0.993
_shelx_estimated_absorpt_T_max   0.998
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.8266
_diffrn_radiation_type           synchrotron
_diffrn_source                   'BL 14.2 PSF, BESSY, Berlin, Germany'
_diffrn_measurement_device_type  Pilatus2M
_diffrn_measurement_method       HPC
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28692
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.859
_diffrn_reflns_theta_max         36.780
_diffrn_reflns_theta_full        29.450
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measured_fraction_theta_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_point_group_measured_fraction_full 0.972
_reflns_number_total             8121
_reflns_number_gt                6062
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       XDS
_computing_cell_refinement       XDS
_computing_data_reduction        XDS
_computing_structure_solution    SHELXD
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
A sovent molecule of partially occupied CH2Cl2 is strongly 
disordered over predominantely two orientations.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0800P)²+5.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8121
_refine_ls_number_parameters     470
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0823
_refine_ls_wR_factor_ref         0.2189
_refine_ls_wR_factor_gt          0.2092
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001

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 0.4561(2) 0.09559(10) 0.3056(3) 0.0314(5) Uani 1 1 d . . . . .
C2 C 0.4374(2) 0.08667(10) 0.1606(3) 0.0325(5) Uani 1 1 d . . . . .
H2 H 0.3736 0.0989 0.1176 0.039 Uiso 1 1 calc R U . . .
C3 C 0.5100(2) 0.06043(11) 0.0783(3) 0.0379(6) Uani 1 1 d . . . . .
H3 H 0.4967 0.0554 -0.0206 0.045 Uiso 1 1 calc R U . . .
C4 C 0.6019(2) 0.04163(11) 0.1411(3) 0.0381(6) Uani 1 1 d . . . . .
H4 H 0.6517 0.0231 0.0855 0.046 Uiso 1 1 calc R U . . .
C5 C 0.6217(2) 0.04968(10) 0.2848(3) 0.0349(5) Uani 1 1 d . . . . .
H5 H 0.6851 0.0366 0.3271 0.042 Uiso 1 1 calc R U . . .
C6 C 0.5494(2) 0.07684(10) 0.3689(3) 0.0309(5) Uani 1 1 d . . . . .
C7 C 0.57519(19) 0.08502(11) 0.5209(3) 0.0313(5) Uani 1 1 d . . . . .
C8 C 0.6152(2) 0.04129(11) 0.5969(3) 0.0351(5) Uani 1 1 d . . . . .
H8 H 0.6120 0.0062 0.5561 0.042 Uiso 1 1 calc R U . . .
C9 C 0.6600(2) 0.04819(12) 0.7326(3) 0.0390(6) Uani 1 1 d . . . . .
H9 H 0.6804 0.0178 0.7883 0.047 Uiso 1 1 calc R U . . .
C10 C 0.6742(2) 0.09941(12) 0.7842(3) 0.0369(6) Uani 1 1 d . . . . .
H10 H 0.7107 0.1044 0.8725 0.044 Uiso 1 1 calc R U . . .
C11 C 0.63602(19) 0.14486(11) 0.7096(3) 0.0315(5) Uani 1 1 d . . . . .
C12 C 0.66326(19) 0.19955(11) 0.7566(3) 0.0314(5) Uani 1 1 d . . . . .
C13 C 0.7393(2) 0.20900(12) 0.8642(3) 0.0356(6) Uani 1 1 d . . . . .
H13 H 0.7698 0.1793 0.9138 0.043 Uiso 1 1 calc R U . . .
C14 C 0.7704(2) 0.26060(12) 0.8990(3) 0.0361(6) Uani 1 1 d . . . . .
H14 H 0.8218 0.2663 0.9723 0.043 Uiso 1 1 calc R U . . .
C15 C 0.7264(2) 0.30448(12) 0.8265(3) 0.0353(6) Uani 1 1 d . . . . .
H15 H 0.7489 0.3401 0.8490 0.042 Uiso 1 1 calc R U . . .
C16 C 0.6506(2) 0.29628(11) 0.7228(3) 0.0334(5) Uani 1 1 d . . . . .
H16 H 0.6203 0.3264 0.6749 0.040 Uiso 1 1 calc R U . . .
C17 C 0.61709(18) 0.24378(11) 0.6861(3) 0.0301(5) Uani 1 1 d . . . . .
C18 C 0.53109(18) 0.23435(10) 0.5847(3) 0.0294(5) Uani 1 1 d . . . . .
C19 C 0.46609(19) 0.27750(10) 0.5391(3) 0.0303(5) Uani 1 1 d . . . . .
H19 H 0.4915 0.3134 0.5489 0.036 Uiso 1 1 calc R U . . .
C20 C 0.36868(19) 0.26946(10) 0.4819(3) 0.0298(5) Uani 1 1 d . . . . .
C21 C 0.3136(2) 0.31587(10) 0.4153(3) 0.0308(5) Uani 1 1 d . . . . .
C22 C 0.3722(2) 0.35081(11) 0.3316(3) 0.0330(5) Uani 1 1 d . . . . .
H22 H 0.4450 0.3442 0.3210 0.040 Uiso 1 1 calc R U . . .
C23 C 0.3268(2) 0.39455(11) 0.2640(3) 0.0379(6) Uani 1 1 d . . . . .
H23 H 0.3682 0.4184 0.2098 0.046 Uiso 1 1 calc R U . . .
C24 C 0.2203(2) 0.40331(12) 0.2759(3) 0.0409(6) Uani 1 1 d . . . . .
H24 H 0.1877 0.4327 0.2274 0.049 Uiso 1 1 calc R U . . .
C25 C 0.1614(2) 0.36925(12) 0.3583(3) 0.0387(6) Uani 1 1 d . . . . .
H25 H 0.0884 0.3757 0.3663 0.046 Uiso 1 1 calc R U . . .
C26 C 0.2070(2) 0.32534(11) 0.4304(3) 0.0325(5) Uani 1 1 d . . . . .
C27 C 0.14071(19) 0.29200(12) 0.5234(3) 0.0331(5) Uani 1 1 d . . . . .
C28 C 0.0708(2) 0.31965(13) 0.6084(3) 0.0395(6) Uani 1 1 d . . . . .
H28 H 0.0748 0.3579 0.6142 0.047 Uiso 1 1 calc R U . . .
C29 C -0.0047(2) 0.29264(14) 0.6847(3) 0.0434(7) Uani 1 1 d . . . . .
H29 H -0.0474 0.3116 0.7493 0.052 Uiso 1 1 calc R U . . .
C30 C -0.0165(2) 0.23861(14) 0.6657(3) 0.0408(7) Uani 1 1 d . . . . .
H30 H -0.0707 0.2203 0.7137 0.049 Uiso 1 1 calc R U . . .
C31 C 0.0497(2) 0.20920(12) 0.5766(3) 0.0350(6) Uani 1 1 d . . . . .
C32 C 0.0230(2) 0.15429(12) 0.5346(3) 0.0364(6) Uani 1 1 d . . . . .
C33 C -0.0738(2) 0.13039(13) 0.5687(3) 0.0430(7) Uani 1 1 d . . . . .
H33 H -0.1188 0.1483 0.6326 0.052 Uiso 1 1 calc R U . . .
C34 C -0.1043(2) 0.08160(14) 0.5113(4) 0.0497(8) Uani 1 1 d . . . . .
H34 H -0.1699 0.0663 0.5352 0.060 Uiso 1 1 calc R U . . .
C35 C -0.0390(3) 0.05473(14) 0.4182(4) 0.0498(8) Uani 1 1 d . . . . .
H35 H -0.0610 0.0217 0.3759 0.060 Uiso 1 1 calc R U . . .
C36 C 0.0571(2) 0.07604(13) 0.3879(3) 0.0438(7) Uani 1 1 d . . . . .
H36 H 0.1020 0.0569 0.3264 0.053 Uiso 1 1 calc R U . . .
C37 C 0.0908(2) 0.12576(12) 0.4460(3) 0.0361(6) Uani 1 1 d . . . . .
C38 C 0.1948(2) 0.14729(11) 0.4226(3) 0.0323(5) Uani 1 1 d . . . . .
C39 C 0.2743(2) 0.11415(11) 0.3681(3) 0.0330(5) Uani 1 1 d . . . . .
H39 H 0.2548 0.0824 0.3175 0.040 Uiso 1 1 calc R U . . .
C40 C 0.37843(19) 0.12623(10) 0.3855(3) 0.0303(5) Uani 1 1 d . . . . .
C41 C 0.40822(18) 0.17453(10) 0.4609(3) 0.0290(5) Uani 1 1 d . . . . .
C42 C 0.50796(18) 0.18260(10) 0.5330(3) 0.0286(5) Uani 1 1 d . . . . .
C43 C 0.57349(18) 0.13731(10) 0.5844(3) 0.0294(5) Uani 1 1 d . . . . .
C44 C 0.32978(19) 0.21539(10) 0.4654(3) 0.0291(5) Uani 1 1 d . . . . .
C45 C 0.22002(19) 0.20074(11) 0.4589(3) 0.0305(5) Uani 1 1 d . . . . .
C46 C 0.13785(19) 0.23520(11) 0.5171(3) 0.0320(5) Uani 1 1 d . . . . .
Cl01 Cl 0.0783(4) 0.53706(17) 0.6141(5) 0.0552(10) Uani 0.291(2) 1 d . . P . .
Cl02 Cl 0.1129(4) 0.5868(2) 0.4661(7) 0.1062(18) Uani 0.291(2) 1 d . . P . .
Cl03 Cl 0.1540(3) 0.47920(17) 0.5503(4) 0.0741(11) Uani 0.291(2) 1 d . . P . .
Cl04 Cl 0.0767(6) 0.5219(3) 0.5537(10) 0.102(3) Uani 0.291(2) 1 d . . P . .
C01 C 0.0951(9) 0.5423(5) 0.4762(19) 0.048(3) Uani 0.291(2) 1 d . . P . .
C02 C 0.0390(18) 0.5085(8) 0.4581(17) 0.091(6) Uani 0.291(2) 1 d . . P . .


_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 1.396(4) . ?
C1 C6 1.397(4) . ?
C1 C40 1.468(4) . ?
C2 C3 1.382(4) . ?
C3 C4 1.381(4) . ?
C4 C5 1.383(4) . ?
C5 C6 1.399(4) . ?
C6 C7 1.473(4) . ?
C7 C8 1.388(4) . ?
C7 C43 1.427(4) . ?
C8 C9 1.397(4) . ?
C9 C10 1.369(4) . ?
C10 C11 1.408(4) . ?
C11 C43 1.419(4) . ?
C11 C12 1.465(4) . ?
C12 C17 1.403(4) . ?
C12 C13 1.404(4) . ?
C13 C14 1.376(4) . ?
C14 C15 1.394(4) . ?
C15 C16 1.372(4) . ?
C16 C17 1.410(4) . ?
C17 C18 1.455(3) . ?
C18 C42 1.400(4) . ?
C18 C19 1.413(4) . ?
C19 C20 1.356(4) . ?
C20 C44 1.436(4) . ?
C20 C21 1.479(4) . ?
C21 C26 1.389(4) . ?
C21 C22 1.398(4) . ?
C22 C23 1.377(4) . ?
C23 C24 1.381(4) . ?
C24 C25 1.380(4) . ?
C25 C26 1.401(4) . ?
C26 C27 1.482(4) . ?
C27 C28 1.391(4) . ?
C27 C46 1.409(4) . ?
C28 C29 1.385(4) . ?
C29 C30 1.359(5) . ?
C30 C31 1.406(4) . ?
C31 C46 1.421(3) . ?
C31 C32 1.455(4) . ?
C32 C37 1.405(4) . ?
C32 C33 1.413(4) . ?
C33 C34 1.376(5) . ?
C34 C35 1.391(5) . ?
C35 C36 1.369(4) . ?
C36 C37 1.411(4) . ?
C37 C38 1.450(3) . ?
C38 C45 1.403(4) . ?
C38 C39 1.410(4) . ?
C39 C40 1.367(3) . ?
C40 C41 1.438(4) . ?
C41 C44 1.424(4) . ?
C41 C42 1.441(3) . ?
C42 C43 1.474(4) . ?
C44 C45 1.445(3) . ?
C45 C46 1.467(4) . ?
Cl01 Cl04 0.681(7) . ?
Cl01 C01 1.32(2) . ?
Cl01 C02 1.693(17) . ?
Cl01 Cl03 1.837(6) . ?
Cl01 Cl02 1.917(8) . ?
Cl01 C02 1.98(2) 3_566 ?
Cl02 C01 1.131(13) . ?
Cl02 Cl04 1.869(10) . ?
Cl02 C02 2.16(2) . ?
Cl03 Cl04 1.447(9) . ?
Cl03 C02 1.84(2) . ?
Cl03 C01 1.861(13) . ?
Cl04 C01 0.921(16) . ?
Cl04 C02 1.062(18) . ?
Cl04 C02 1.66(2) 3_566 ?
Cl04 Cl04 2.435(12) 3_566 ?
C01 C02 1.11(3) . ?
C02 C02 1.35(4) 3_566 ?
C02 Cl04 1.66(2) 3_566 ?
C02 Cl01 1.98(2) 3_566 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 119.1(2) . . ?
C2 C1 C40 118.7(2) . . ?
C6 C1 C40 122.1(2) . . ?
C3 C2 C1 121.3(3) . . ?
C4 C3 C2 119.5(3) . . ?
C3 C4 C5 120.2(3) . . ?
C4 C5 C6 120.9(3) . . ?
C1 C6 C5 119.0(2) . . ?
C1 C6 C7 122.4(2) . . ?
C5 C6 C7 118.6(2) . . ?
C8 C7 C43 120.2(2) . . ?
C8 C7 C6 117.6(2) . . ?
C43 C7 C6 121.7(2) . . ?
C7 C8 C9 120.8(3) . . ?
C10 C9 C8 119.0(3) . . ?
C9 C10 C11 121.6(3) . . ?
C10 C11 C43 119.3(2) . . ?
C10 C11 C12 120.9(2) . . ?
C43 C11 C12 119.8(2) . . ?
C17 C12 C13 119.0(2) . . ?
C17 C12 C11 119.1(2) . . ?
C13 C12 C11 121.8(3) . . ?
C14 C13 C12 121.1(3) . . ?
C13 C14 C15 119.9(3) . . ?
C16 C15 C14 120.1(3) . . ?
C15 C16 C17 121.0(3) . . ?
C12 C17 C16 118.9(2) . . ?
C12 C17 C18 119.1(2) . . ?
C16 C17 C18 121.9(2) . . ?
C42 C18 C19 118.1(2) . . ?
C42 C18 C17 121.6(2) . . ?
C19 C18 C17 120.3(2) . . ?
C20 C19 C18 122.3(2) . . ?
C19 C20 C44 119.4(2) . . ?
C19 C20 C21 118.4(2) . . ?
C44 C20 C21 121.4(2) . . ?
C26 C21 C22 119.3(2) . . ?
C26 C21 C20 122.9(2) . . ?
C22 C21 C20 117.7(2) . . ?
C23 C22 C21 121.5(3) . . ?
C22 C23 C24 119.3(3) . . ?
C25 C24 C23 119.8(3) . . ?
C24 C25 C26 121.5(3) . . ?
C21 C26 C25 118.5(2) . . ?
C21 C26 C27 122.6(2) . . ?
C25 C26 C27 118.9(2) . . ?
C28 C27 C46 120.0(3) . . ?
C28 C27 C26 116.5(3) . . ?
C46 C27 C26 123.1(2) . . ?
C29 C28 C27 121.4(3) . . ?
C30 C29 C28 119.0(3) . . ?
C29 C30 C31 121.5(3) . . ?
C30 C31 C46 119.4(3) . . ?
C30 C31 C32 120.4(2) . . ?
C46 C31 C32 119.9(2) . . ?
C37 C32 C33 118.5(3) . . ?
C37 C32 C31 119.2(2) . . ?
C33 C32 C31 122.0(3) . . ?
C34 C33 C32 121.3(3) . . ?
C33 C34 C35 120.0(3) . . ?
C36 C35 C34 119.8(3) . . ?
C35 C36 C37 121.5(3) . . ?
C32 C37 C36 118.8(2) . . ?
C32 C37 C38 118.8(3) . . ?
C36 C37 C38 122.3(3) . . ?
C45 C38 C39 118.4(2) . . ?
C45 C38 C37 121.0(2) . . ?
C39 C38 C37 120.5(2) . . ?
C40 C39 C38 122.2(2) . . ?
C39 C40 C41 119.1(2) . . ?
C39 C40 C1 119.3(2) . . ?
C41 C40 C1 120.6(2) . . ?
C44 C41 C40 115.4(2) . . ?
C44 C41 C42 120.0(2) . . ?
C40 C41 C42 124.6(2) . . ?
C18 C42 C41 117.8(2) . . ?
C18 C42 C43 118.1(2) . . ?
C41 C42 C43 122.4(2) . . ?
C11 C43 C7 116.9(2) . . ?
C11 C43 C42 118.3(2) . . ?
C7 C43 C42 124.6(2) . . ?
C41 C44 C20 115.2(2) . . ?
C41 C44 C45 120.0(2) . . ?
C20 C44 C45 124.8(2) . . ?
C38 C45 C44 117.6(2) . . ?
C38 C45 C46 118.6(2) . . ?
C44 C45 C46 122.5(2) . . ?
C27 C46 C31 117.1(2) . . ?
C27 C46 C45 125.4(2) . . ?
C31 C46 C45 117.4(2) . . ?
Cl04 Cl01 C01 40.5(10) . . ?
Cl04 Cl01 C02 17.2(10) . . ?
C01 Cl01 C02 41.0(9) . . ?
Cl04 Cl01 Cl03 45.8(8) . . ?
C01 Cl01 Cl03 70.0(5) . . ?
C02 Cl01 Cl03 62.5(7) . . ?
Cl04 Cl01 Cl02 75.6(10) . . ?
C01 Cl01 Cl02 35.2(5) . . ?
C02 Cl01 Cl02 73.0(8) . . ?
Cl03 Cl01 Cl02 97.7(3) . . ?
Cl04 Cl01 C02 52.5(10) . 3_566 ?
C01 Cl01 C02 81.8(7) . 3_566 ?
C02 Cl01 C02 42.2(11) . 3_566 ?
Cl03 Cl01 C02 80.9(6) . 3_566 ?
Cl02 Cl01 C02 107.6(6) . 3_566 ?
C01 Cl02 Cl04 21.8(9) . . ?
C01 Cl02 Cl01 42.4(9) . . ?
Cl04 Cl02 Cl01 20.7(2) . . ?
C01 Cl02 C02 15.7(8) . . ?
Cl04 Cl02 C02 29.5(5) . . ?
Cl01 Cl02 C02 48.7(5) . . ?
Cl04 Cl03 C02 35.3(5) . . ?
Cl04 Cl03 Cl01 19.7(3) . . ?
C02 Cl03 Cl01 54.9(5) . . ?
Cl04 Cl03 C01 29.0(5) . . ?
C02 Cl03 C01 35.0(8) . . ?
Cl01 Cl03 C01 42.0(6) . . ?
Cl01 Cl04 C01 110.7(16) . . ?
Cl01 Cl04 C02 151.9(17) . . ?
C01 Cl04 C02 67.7(15) . . ?
Cl01 Cl04 Cl03 114.5(9) . . ?
C01 Cl04 Cl03 101.3(11) . . ?
C02 Cl04 Cl03 92.7(12) . . ?
Cl01 Cl04 C02 108.5(13) . 3_566 ?
C01 Cl04 C02 116.1(11) . 3_566 ?
C02 Cl04 C02 54.3(15) . 3_566 ?
Cl03 Cl04 C02 105.7(8) . 3_566 ?
Cl01 Cl04 Cl02 83.7(10) . . ?
C01 Cl04 Cl02 27.2(9) . . ?
C02 Cl04 Cl02 90.4(14) . . ?
Cl03 Cl04 Cl02 116.4(6) . . ?
C02 Cl04 Cl02 126.2(8) 3_566 . ?
Cl01 Cl04 Cl04 126.9(13) . 3_566 ?
C01 Cl04 Cl04 97.7(9) . 3_566 ?
C02 Cl04 Cl04 33.6(12) . 3_566 ?
Cl03 Cl04 Cl04 101.9(6) . 3_566 ?
C02 Cl04 Cl04 20.8(5) 3_566 3_566 ?
Cl02 Cl04 Cl04 113.9(5) . 3_566 ?
Cl04 C01 C02 62.2(13) . . ?
Cl04 C01 Cl02 131.0(18) . . ?
C02 C01 Cl02 148.3(16) . . ?
Cl04 C01 Cl01 28.7(8) . . ?
C02 C01 Cl01 87.6(16) . . ?
Cl02 C01 Cl01 102.4(10) . . ?
Cl04 C01 Cl03 49.6(8) . . ?
C02 C01 Cl03 71.2(13) . . ?
Cl02 C01 Cl03 140.4(8) . . ?
Cl01 C01 Cl03 68.0(7) . . ?
Cl04 C02 C01 50.1(13) . . ?
Cl04 C02 C02 85.9(15) . 3_566 ?
C01 C02 C02 129(2) . 3_566 ?
Cl04 C02 Cl04 125.7(15) . 3_566 ?
C01 C02 Cl04 157.1(17) . 3_566 ?
C02 C02 Cl04 39.7(13) 3_566 3_566 ?
Cl04 C02 Cl01 10.9(7) . . ?
C01 C02 Cl01 51.4(13) . . ?
C02 C02 Cl01 80.4(13) 3_566 . ?
Cl04 C02 Cl01 119.5(11) 3_566 . ?
Cl04 C02 Cl03 51.9(11) . . ?
C01 C02 Cl03 73.8(13) . . ?
C02 C02 Cl03 101.1(19) 3_566 . ?
Cl04 C02 Cl03 123.4(12) 3_566 . ?
Cl01 C02 Cl03 62.6(7) . . ?
Cl04 C02 Cl01 142.3(17) . 3_566 ?
C01 C02 Cl01 163.7(19) . 3_566 ?
C02 C02 Cl01 57.4(16) 3_566 3_566 ?
Cl04 C02 Cl01 19.0(5) 3_566 3_566 ?
Cl01 C02 Cl01 137.8(11) . 3_566 ?
Cl03 C02 Cl01 121.6(11) . 3_566 ?
Cl04 C02 Cl02 60.1(12) . . ?
C01 C02 Cl02 16.0(8) . . ?
C02 C02 Cl02 126.0(17) 3_566 . ?
Cl04 C02 Cl02 143.0(12) 3_566 . ?
Cl01 C02 Cl02 58.3(7) . . ?
Cl03 C02 Cl02 89.8(10) . . ?
Cl01 C02 Cl02 148.2(11) 3_566 . ?

_refine_diff_density_max         0.591
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.073



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2/n-hexane mixture'
