# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_jj18_2
_database_code_depnum_ccdc_archive 'CCDC 1402907'
_audit_update_record             
;
2015-05-26 deposited with the CCDC.
2015-08-07 downloaded from the CCDC.
;
_audit_creation_date             2015-05-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C124 H168'
_chemical_formula_sum            'C124 H168'
_chemical_formula_weight         1658.57
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C186 H168'
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'

_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      tetragonal
_space_group_IT_number           85
_space_group_name_H-M_alt        'P 4/n'
_space_group_name_Hall           '-P 4a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-1/2, -z'

_cell_length_a                   19.3824(4)
_cell_length_b                   19.3824(4)
_cell_length_c                   14.8604(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5582.7(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2604
_cell_measurement_temperature    172.9(3)
_cell_measurement_theta_max      51.3186
_cell_measurement_theta_min      2.9712
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.987
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1824
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.1939
_exptl_crystal_size_mid          0.1444
_exptl_crystal_size_min          0.0262
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.587
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5632
_diffrn_reflns_point_group_measured_fraction_full 0.587
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         51.378
_diffrn_reflns_theta_min         2.974
_diffrn_ambient_temperature      172.9(3)
_diffrn_detector_area_resol_mean 10.6144
_diffrn_measured_fraction_theta_full 0.587
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   21.00   53.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.4130   57.0000    0.0000 32

#__ type_ start__ end____ width___ exp.time_
  2 omega  -62.00  -18.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.4130   57.0000    0.0000 44

#__ type_ start__ end____ width___ exp.time_
  3 omega  -31.00   -3.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      -69.9078   30.0000 -150.0000 28

#__ type_ start__ end____ width___ exp.time_
  4 omega -151.00  -43.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      -69.9078  -61.0000  120.0000 108

#__ type_ start__ end____ width___ exp.time_
  5 omega  108.00  161.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       70.2203  125.0000    0.0000 53
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0010815000
_diffrn_orient_matrix_UB_12      0.0186576000
_diffrn_orient_matrix_UB_13      0.1008691000
_diffrn_orient_matrix_UB_21      0.0048120000
_diffrn_orient_matrix_UB_22      0.0769857000
_diffrn_orient_matrix_UB_23      -0.0242755000
_diffrn_orient_matrix_UB_31      -0.0793627000
_diffrn_orient_matrix_UB_32      0.0052485000
_diffrn_orient_matrix_UB_33      -0.0002469000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2509
_reflns_number_total             2972
_reflns_odcompleteness_completeness 98.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_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 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         2972
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0759
_refine_ls_restrained_S_all      1.122
_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)+(0.1105P)²+6.9493P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1974
_refine_ls_wR_factor_ref         0.2091
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C19A-C17 \\sim C20-C17 \\sim C18A-C17 \\sim C19-C17 \\sim C18-C17 \\sim
C17-C20A
 with sigma of 0.02
 C18-C18A \\sim C18A-C19A
 with sigma of 0.02
 C37-C39A \\sim C40-C37 \\sim C38A-C37 \\sim C39-C37 \\sim C40A-C37 \\sim
C38-C37
 with sigma of 0.02
 C21-C23A \\sim C22-C21 \\sim C24A-C21 \\sim C23-C21 \\sim C22A-C21 \\sim
C24-C21
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C19A) = Uanis(C20) = Uanis(C18A) = Uanis(C19) = Uanis(C20A) = Uanis(C18)
Uanis(C38A) = Uanis(C40) = Uanis(C39A) = Uanis(C38) = Uanis(C40A) = Uanis(C39)
Uanis(C23A) = Uanis(C22) = Uanis(C24A) = Uanis(C23) = Uanis(C22A) = Uanis(C24)
4. Others
 Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=1-FVAR(1)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C18)=Sof(H18D)=Sof(H18E)=Sof(H18F)=FVAR(1)
 Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C39A)=Sof(H39D)=
 Sof(H39E)=Sof(H39F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C22A)=
 Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(2)
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=
 FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C16(H16), C32(H32), C34(H34), C36(H36)
5.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C20A(H20D,H20E,H20F), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C38A(H38D,H38E,H38F), C24A(H24D,H24E,H24F), C40A(H40D,
 H40E,H40F), C39A(H39D,H39E,H39F), C19A(H19D,H19E,H19F), C18A(H18A,H18B,H18C),
 C18(H18D,H18E,H18F), C23A(H23D,H23E,H23F), C22A(H22D,H22E,H22F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.42500(16) 0.32394(15) 0.3897(2) 0.0337(8) Uani 1 1 d . . . . .
C2 C 0.36257(17) 0.29709(15) 0.3993(2) 0.0331(9) Uani 1 1 d . . . . .
C3 C 0.30047(16) 0.27081(14) 0.4030(2) 0.0286(8) Uani 1 1 d . . . . .
C11 C 0.44980(15) 0.33645(15) 0.2961(2) 0.0369(9) Uani 1 1 d . . . . .
C12 C 0.40607(17) 0.36714(16) 0.2343(2) 0.0430(9) Uani 1 1 d . . . . .
H12 H 0.3618 0.3795 0.2524 0.052 Uiso 1 1 calc R . . . .
C13 C 0.42603(19) 0.38009(19) 0.1466(3) 0.0535(10) Uani 1 1 d . . . . .
C14 C 0.4928(2) 0.36123(19) 0.1220(3) 0.0593(11) Uani 1 1 d . . . . .
H14 H 0.5074 0.3702 0.0636 0.071 Uiso 1 1 calc R . . . .
C15 C 0.53838(18) 0.32974(17) 0.1807(3) 0.0503(10) Uani 1 1 d . . . . .
C16 C 0.51558(16) 0.31747(16) 0.2680(3) 0.0441(9) Uani 1 1 d . . . . .
H16 H 0.5451 0.2960 0.3087 0.053 Uiso 1 1 calc R . . . .
C17 C 0.3775(2) 0.4129(2) 0.0786(3) 0.0752(14) Uani 1 1 d D . . . .
C19 C 0.3572(4) 0.3544(4) 0.0070(5) 0.0957(15) Uani 0.759(5) 1 d D . P A 1
H19A H 0.3983 0.3370 -0.0211 0.144 Uiso 0.759(5) 1 calc GR . P A 1
H19B H 0.3275 0.3738 -0.0381 0.144 Uiso 0.759(5) 1 calc GR . P A 1
H19C H 0.3337 0.3175 0.0371 0.144 Uiso 0.759(5) 1 calc GR . P A 1
C20 C 0.4102(4) 0.4681(4) 0.0248(5) 0.0957(15) Uani 0.759(5) 1 d D . P A 1
H20A H 0.4229 0.5056 0.0636 0.144 Uiso 0.759(5) 1 calc GR . P A 1
H20B H 0.3783 0.4842 -0.0199 0.144 Uiso 0.759(5) 1 calc GR . P A 1
H20C H 0.4507 0.4502 -0.0042 0.144 Uiso 0.759(5) 1 calc GR . P A 1
C20A C 0.3185(12) 0.4536(12) 0.1230(18) 0.0957(15) Uani 0.241(5) 1 d D . P A 1
H20D H 0.2913 0.4230 0.1595 0.144 Uiso 0.241(5) 1 calc GR . P A 1
H20E H 0.2899 0.4737 0.0773 0.144 Uiso 0.241(5) 1 calc GR . P A 1
H20F H 0.3375 0.4895 0.1601 0.144 Uiso 0.241(5) 1 calc GR . P A 1
C21 C 0.61153(19) 0.3110(2) 0.1525(3) 0.0650(12) Uani 1 1 d D . . . .
C22 C 0.6332(4) 0.2412(4) 0.1857(7) 0.1044(17) Uani 0.754(4) 1 d D . P B 1
H22A H 0.6366 0.2420 0.2502 0.157 Uiso 0.754(4) 1 calc GR . P B 1
H22B H 0.6772 0.2295 0.1604 0.157 Uiso 0.754(4) 1 calc GR . P B 1
H22C H 0.5995 0.2075 0.1679 0.157 Uiso 0.754(4) 1 calc GR . P B 1
C23 C 0.6574(3) 0.3702(4) 0.1761(6) 0.1044(17) Uani 0.754(4) 1 d D . P B 1
H23A H 0.6407 0.4113 0.1473 0.157 Uiso 0.754(4) 1 calc GR . P B 1
H23B H 0.7035 0.3607 0.1559 0.157 Uiso 0.754(4) 1 calc GR . P B 1
H23C H 0.6575 0.3767 0.2401 0.157 Uiso 0.754(4) 1 calc GR . P B 1
C24 C 0.6154(4) 0.3043(5) 0.0471(5) 0.1044(17) Uani 0.754(4) 1 d D . P B 1
H24A H 0.5831 0.2699 0.0272 0.157 Uiso 0.754(4) 1 calc GR . P B 1
H24B H 0.6612 0.2910 0.0297 0.157 Uiso 0.754(4) 1 calc GR . P B 1
H24C H 0.6041 0.3478 0.0200 0.157 Uiso 0.754(4) 1 calc GR . P B 1
C31 C 0.46723(15) 0.34324(15) 0.4687(2) 0.0368(9) Uani 1 1 d . . . . .
C32 C 0.44737(17) 0.32419(17) 0.5553(2) 0.0436(9) Uani 1 1 d . . . . .
H32 H 0.4084 0.2967 0.5627 0.052 Uiso 1 1 calc R . . . .
C33 C 0.48376(19) 0.34481(19) 0.6307(2) 0.0509(10) Uani 1 1 d . . . . .
C34 C 0.54316(19) 0.38452(19) 0.6167(3) 0.0557(11) Uani 1 1 d . . . . .
H34 H 0.5692 0.3978 0.6664 0.067 Uiso 1 1 calc R . . . .
C35 C 0.56473(17) 0.40478(17) 0.5321(3) 0.0470(10) Uani 1 1 d . . . . .
C36 C 0.52561(16) 0.38470(16) 0.4589(2) 0.0407(9) Uani 1 1 d . . . . .
H36 H 0.5385 0.3992 0.4017 0.049 Uiso 1 1 calc R . . . .
C37 C 0.4601(2) 0.3292(2) 0.7258(3) 0.0667(12) Uani 1 1 d D . . . .
C38 C 0.4400(4) 0.4012(3) 0.7686(4) 0.0886(12) Uani 0.754(4) 1 d D . P B 1
H38A H 0.4796 0.4310 0.7684 0.133 Uiso 0.754(4) 1 calc GR . P B 1
H38B H 0.4247 0.3944 0.8294 0.133 Uiso 0.754(4) 1 calc GR . P B 1
H38C H 0.4037 0.4219 0.7339 0.133 Uiso 0.754(4) 1 calc GR . P B 1
C39 C 0.3954(3) 0.2863(4) 0.7282(4) 0.0886(12) Uani 0.754(4) 1 d D . P B 1
H39A H 0.3593 0.3099 0.6963 0.133 Uiso 0.754(4) 1 calc GR . P B 1
H39B H 0.3816 0.2792 0.7896 0.133 Uiso 0.754(4) 1 calc GR . P B 1
H39C H 0.4040 0.2425 0.7002 0.133 Uiso 0.754(4) 1 calc GR . P B 1
C40 C 0.5168(4) 0.2962(4) 0.7772(5) 0.0886(12) Uani 0.754(4) 1 d D . P B 1
H40A H 0.5303 0.2542 0.7479 0.133 Uiso 0.754(4) 1 calc GR . P B 1
H40B H 0.5013 0.2862 0.8372 0.133 Uiso 0.754(4) 1 calc GR . P B 1
H40C H 0.5556 0.3270 0.7798 0.133 Uiso 0.754(4) 1 calc GR . P B 1
C41 C 0.63160(18) 0.44647(19) 0.5200(3) 0.0571(11) Uani 1 1 d . . . . .
C42 C 0.6445(2) 0.4936(2) 0.6009(3) 0.0782(14) Uani 1 1 d . . . . .
H42A H 0.6048 0.5224 0.6105 0.117 Uiso 1 1 calc GR . . . .
H42B H 0.6841 0.5220 0.5894 0.117 Uiso 1 1 calc GR . . . .
H42C H 0.6526 0.4660 0.6535 0.117 Uiso 1 1 calc GR . . . .
C43 C 0.6908(2) 0.3955(2) 0.5098(4) 0.0898(17) Uani 1 1 d . . . . .
H43A H 0.6935 0.3670 0.5625 0.135 Uiso 1 1 calc GR . . . .
H43B H 0.7333 0.4203 0.5025 0.135 Uiso 1 1 calc GR . . . .
H43C H 0.6829 0.3671 0.4579 0.135 Uiso 1 1 calc GR . . . .
C44 C 0.6270(2) 0.4925(2) 0.4371(3) 0.0772(14) Uani 1 1 d . . . . .
H44A H 0.6249 0.4643 0.3841 0.116 Uiso 1 1 calc GR . . . .
H44B H 0.6670 0.5217 0.4343 0.116 Uiso 1 1 calc GR . . . .
H44C H 0.5862 0.5205 0.4408 0.116 Uiso 1 1 calc GR . . . .
C38A C 0.4530(12) 0.2462(7) 0.7359(13) 0.0886(12) Uani 0.246(4) 1 d D . P B 2
H38D H 0.4207 0.2293 0.6921 0.133 Uiso 0.246(4) 1 calc GR . P B 2
H38E H 0.4368 0.2352 0.7952 0.133 Uiso 0.246(4) 1 calc GR . P B 2
H38F H 0.4971 0.2251 0.7262 0.133 Uiso 0.246(4) 1 calc GR . P B 2
C24A C 0.6631(8) 0.3293(14) 0.2316(14) 0.1044(17) Uani 0.246(4) 1 d D . P B 2
H24D H 0.6494 0.3721 0.2589 0.157 Uiso 0.246(4) 1 calc GR . P B 2
H24E H 0.7090 0.3337 0.2080 0.157 Uiso 0.246(4) 1 calc GR . P B 2
H24F H 0.6621 0.2933 0.2759 0.157 Uiso 0.246(4) 1 calc GR . P B 2
C40A C 0.3897(8) 0.3531(12) 0.7546(13) 0.0886(12) Uani 0.246(4) 1 d D . P B 2
H40D H 0.3883 0.4026 0.7546 0.133 Uiso 0.246(4) 1 calc GR . P B 2
H40E H 0.3801 0.3363 0.8141 0.133 Uiso 0.246(4) 1 calc GR . P B 2
H40F H 0.3557 0.3356 0.7135 0.133 Uiso 0.246(4) 1 calc GR . P B 2
C39A C 0.5127(10) 0.3338(13) 0.8047(12) 0.0886(12) Uani 0.246(4) 1 d D . P B 2
H39D H 0.5575 0.3201 0.7838 0.133 Uiso 0.246(4) 1 calc GR . P B 2
H39E H 0.4984 0.3037 0.8525 0.133 Uiso 0.246(4) 1 calc GR . P B 2
H39F H 0.5146 0.3804 0.8265 0.133 Uiso 0.246(4) 1 calc GR . P B 2
C19A C 0.3885(12) 0.4944(7) 0.1077(13) 0.0957(15) Uani 0.241(5) 1 d D . P A 2
H19D H 0.3741 0.5008 0.1690 0.144 Uiso 0.241(5) 1 calc GR . P A 2
H19E H 0.3614 0.5234 0.0691 0.144 Uiso 0.241(5) 1 calc GR . P A 2
H19F H 0.4363 0.5064 0.1019 0.144 Uiso 0.241(5) 1 calc GR . P A 2
C18A C 0.3976(11) 0.4036(12) -0.0186(9) 0.0957(15) Uani 0.241(5) 1 d D . P A 2
H18A H 0.4391 0.4292 -0.0306 0.144 Uiso 0.241(5) 1 calc GR . P A 2
H18B H 0.3612 0.4203 -0.0566 0.144 Uiso 0.241(5) 1 calc GR . P A 2
H18C H 0.4055 0.3556 -0.0305 0.144 Uiso 0.241(5) 1 calc GR . P A 2
C18 C 0.3059(4) 0.4236(4) 0.1133(6) 0.0957(15) Uani 0.759(5) 1 d D . P A 2
H18D H 0.2848 0.3796 0.1244 0.144 Uiso 0.759(5) 1 calc GR . P A 2
H18E H 0.2794 0.4485 0.0696 0.144 Uiso 0.759(5) 1 calc GR . P A 2
H18F H 0.3077 0.4494 0.1684 0.144 Uiso 0.759(5) 1 calc GR . P A 2
C23A C 0.6143(12) 0.2299(8) 0.157(2) 0.1044(17) Uani 0.246(4) 1 d D . P B 2
H23D H 0.5966 0.2148 0.2146 0.157 Uiso 0.246(4) 1 calc GR . P B 2
H23E H 0.6611 0.2147 0.1509 0.157 Uiso 0.246(4) 1 calc GR . P B 2
H23F H 0.5867 0.2107 0.1100 0.157 Uiso 0.246(4) 1 calc GR . P B 2
C22A C 0.6379(11) 0.3291(14) 0.0596(12) 0.1044(17) Uani 0.246(4) 1 d D . P B 2
H22D H 0.6009 0.3255 0.0169 0.157 Uiso 0.246(4) 1 calc GR . P B 2
H22E H 0.6742 0.2979 0.0432 0.157 Uiso 0.246(4) 1 calc GR . P B 2
H22F H 0.6554 0.3755 0.0597 0.157 Uiso 0.246(4) 1 calc GR . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.325(5) . ?
C1 C11 1.492(5) . ?
C1 C31 1.479(5) . ?
C2 C3 1.308(4) . ?
C3 C3 1.497(4) 2 ?
C3 C3 1.496(4) 4 ?
C11 C12 1.384(5) . ?
C11 C16 1.391(4) . ?
C12 C13 1.383(5) . ?
C13 C14 1.394(5) . ?
C13 C17 1.520(6) . ?
C14 C15 1.383(6) . ?
C15 C16 1.391(5) . ?
C15 C21 1.522(5) . ?
C17 C19 1.604(8) . ?
C17 C20 1.479(7) . ?
C17 C20A 1.537(14) . ?
C17 C19A 1.651(13) . ?
C17 C18A 1.508(13) . ?
C17 C18 1.493(7) . ?
C21 C22 1.500(8) . ?
C21 C23 1.493(7) . ?
C21 C24 1.575(8) . ?
C21 C24A 1.583(14) . ?
C21 C23A 1.575(15) . ?
C21 C22A 1.514(14) . ?
C31 C32 1.393(5) . ?
C31 C36 1.395(5) . ?
C32 C33 1.383(5) . ?
C33 C34 1.401(5) . ?
C33 C37 1.517(6) . ?
C34 C35 1.381(5) . ?
C35 C36 1.382(5) . ?
C35 C41 1.538(5) . ?
C37 C38 1.583(7) . ?
C37 C39 1.506(7) . ?
C37 C40 1.482(7) . ?
C37 C38A 1.620(13) . ?
C37 C40A 1.505(13) . ?
C37 C39A 1.555(13) . ?
C41 C42 1.531(6) . ?
C41 C43 1.521(6) . ?
C41 C44 1.523(6) . ?

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 C11 117.3(3) . . ?
C2 C1 C31 121.3(3) . . ?
C31 C1 C11 121.4(3) . . ?
C3 C2 C1 176.3(3) . . ?
C2 C3 C3 135.5(3) . 4 ?
C2 C3 C3 134.4(3) . 2 ?
C3 C3 C3 90.0 4 2 ?
C12 C11 C1 119.4(3) . . ?
C12 C11 C16 118.4(3) . . ?
C16 C11 C1 122.1(3) . . ?
C13 C12 C11 122.2(3) . . ?
C12 C13 C14 117.3(4) . . ?
C12 C13 C17 121.9(3) . . ?
C14 C13 C17 120.8(3) . . ?
C15 C14 C13 123.0(4) . . ?
C14 C15 C16 117.4(3) . . ?
C14 C15 C21 121.8(4) . . ?
C16 C15 C21 120.8(4) . . ?
C15 C16 C11 121.7(3) . . ?
C13 C17 C19 107.3(4) . . ?
C13 C17 C20A 113.0(11) . . ?
C13 C17 C19A 98.4(8) . . ?
C20 C17 C13 113.3(4) . . ?
C20 C17 C19 104.9(5) . . ?
C20 C17 C20A 100.4(10) . . ?
C20A C17 C19 117.7(12) . . ?
C18A C17 C13 115.2(8) . . ?
C18A C17 C19A 109.3(10) . . ?
C18 C17 C13 113.8(4) . . ?
C18 C17 C19A 84.1(9) . . ?
C18 C17 C18A 126.0(9) . . ?
C15 C21 C24 109.7(4) . . ?
C15 C21 C24A 109.3(7) . . ?
C15 C21 C23A 104.8(9) . . ?
C22 C21 C15 112.6(4) . . ?
C22 C21 C24 103.8(5) . . ?
C23 C21 C15 107.9(4) . . ?
C23 C21 C22 116.7(5) . . ?
C23 C21 C24 105.6(5) . . ?
C23A C21 C24A 99.7(14) . . ?
C22A C21 C15 120.7(10) . . ?
C22A C21 C24A 114.3(12) . . ?
C22A C21 C23A 105.2(15) . . ?
C32 C31 C1 120.9(3) . . ?
C32 C31 C36 118.2(3) . . ?
C36 C31 C1 120.8(3) . . ?
C33 C32 C31 122.1(3) . . ?
C32 C33 C34 117.2(4) . . ?
C32 C33 C37 122.9(3) . . ?
C34 C33 C37 119.8(3) . . ?
C35 C34 C33 122.7(3) . . ?
C34 C35 C36 118.0(3) . . ?
C34 C35 C41 120.7(3) . . ?
C36 C35 C41 121.2(4) . . ?
C35 C36 C31 121.7(3) . . ?
C33 C37 C38 105.8(4) . . ?
C33 C37 C38A 108.1(7) . . ?
C33 C37 C39A 119.5(9) . . ?
C39 C37 C33 112.6(4) . . ?
C39 C37 C38 105.8(4) . . ?
C40 C37 C33 110.0(4) . . ?
C40 C37 C38 110.8(5) . . ?
C40 C37 C39 111.6(5) . . ?
C40A C37 C33 118.5(8) . . ?
C40A C37 C38A 101.6(12) . . ?
C40A C37 C39A 111.3(12) . . ?
C39A C37 C38A 92.5(12) . . ?
C42 C41 C35 111.0(3) . . ?
C43 C41 C35 107.8(3) . . ?
C43 C41 C42 110.1(3) . . ?
C43 C41 C44 110.1(4) . . ?
C44 C41 C35 110.7(3) . . ?
C44 C41 C42 107.1(3) . . ?


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
-9 9 -1 0.0788 -8.6443 9.0684 -0.6977 0.0895 0.6735 0.7338
-7 -10 1 0.0655 -7.2068 -10.2896 0.8899 -0.1100 -0.8484 0.5177
7 -10 1 0.0797 6.9176 -10.4372 0.8206 -0.1045 -0.7901 -0.6040
9 9 -1 0.0662 8.9312 8.8488 -0.7811 0.0960 0.7432 -0.6622
0 0 10 0.0066 0.0852 0.0118 9.6382 0.9725 -0.2327 -0.0091
13 -1 0 0.1001 12.5359 -0.8031 0.3959 0.0385 -0.0111 -0.9992
0 0 -10 0.0197 -0.0852 -0.0118 -9.6382 -0.9725 0.2327 0.0091

_olex2_date_sample_data_collection 07.08.2012
_olex2_date_sample_submission    23.07.2012
_olex2_exptl_crystal_mounting_method 'mounted on a loop'
_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_dw06
_database_code_depnum_ccdc_archive 'CCDC 1402908'
_audit_update_record             
;
2015-05-29 deposited with the CCDC.
2015-08-07 downloaded from the CCDC.
;
_audit_creation_date             2015-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C76 H56'
_chemical_formula_sum            'C76 H56'
_chemical_formula_weight         969.20
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C38 H28'
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'

_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                   16.2177(3)
_cell_length_b                   9.01016(14)
_cell_length_c                   21.3998(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.2323(18)
_cell_angle_gamma                90
_cell_volume                     3094.81(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4167
_cell_measurement_temperature    172.9(3)
_cell_measurement_theta_max      63.5230
_cell_measurement_theta_min      5.3340
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.956
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic brownish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.040
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.1367
_exptl_crystal_size_mid          0.0871
_exptl_crystal_size_min          0.0167
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.784
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7901
_diffrn_reflns_point_group_measured_fraction_full 0.784
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         58.916
_diffrn_reflns_theta_min         5.335
_diffrn_reflns_v_R_equivalents   ?
_diffrn_ambient_temperature      172.9(3)
_diffrn_detector_area_resol_mean 10.6144
_diffrn_measured_fraction_theta_full 0.784
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -86.00  -35.00   1.0000   27.9500
omega____ theta____ kappa____ phi______ frames
    -       -1.3659 -178.0000   30.0000 51

#__ type_ start__ end____ width___ exp.time_
  2 omega  -20.00   41.00   1.0000   27.9500
omega____ theta____ kappa____ phi______ frames
    -        1.3659   77.0000 -120.0000 61

#__ type_ start__ end____ width___ exp.time_
  3 omega   60.00  152.00   1.0000  111.8000
omega____ theta____ kappa____ phi______ frames
    -       85.9553   45.0000 -150.0000 92

#__ type_ start__ end____ width___ exp.time_
  4 omega   15.00   91.00   1.0000  111.8000
omega____ theta____ kappa____ phi______ frames
    -       85.9553  -30.0000 -150.0000 76

#__ type_ start__ end____ width___ exp.time_
  5 omega   59.00  158.00   1.0000  111.8000
omega____ theta____ kappa____ phi______ frames
    -       85.9553   30.0000  120.0000 99

#__ type_ start__ end____ width___ exp.time_
  6 omega   21.00   89.00   1.0000  111.8000
omega____ theta____ kappa____ phi______ frames
    -       85.9553  -94.0000 -120.0000 68
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0751563000
_diffrn_orient_matrix_UB_12      0.0179214000
_diffrn_orient_matrix_UB_13      -0.0524012000
_diffrn_orient_matrix_UB_21      -0.0559274000
_diffrn_orient_matrix_UB_22      -0.0801809000
_diffrn_orient_matrix_UB_23      0.0416367000
_diffrn_orient_matrix_UB_31      -0.0210462000
_diffrn_orient_matrix_UB_32      0.1499042000
_diffrn_orient_matrix_UB_33      0.0284968000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3760
_reflns_number_total             4392
_reflns_odcompleteness_completeness 98.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_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 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4392
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0617
_refine_ls_restrained_S_all      1.086
_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)+(0.1291P)²+0.6424P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.1947
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C37-C36 \\sim C37A-C32
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C37A) = Uanis(C37)
4. Others
 Sof(H36)=Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(1)
 Sof(H32)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C22(H22), C23(H23), C24(H24),
 C25(H25), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43),
  C44(H44), C45(H45)
5.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C37A(H37D,H37E,
 H37F), C47(H47A,H47B,H47C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.75053(11) 0.0580(2) 0.52918(9) 0.0324(5) Uani 1 1 d . . . . .
C2 C 0.80798(12) 0.1452(2) 0.51220(9) 0.0351(5) Uani 1 1 d . . . . .
C3 C 0.86147(11) 0.24073(19) 0.49391(9) 0.0332(5) Uani 1 1 d . . . . .
C4 C 0.92901(12) 0.3013(2) 0.53636(9) 0.0343(5) Uani 1 1 d . . . . .
C5 C 0.98620(12) 0.3743(2) 0.56186(9) 0.0339(5) Uani 1 1 d . . . . .
C6 C 0.74020(13) 0.1919(2) 0.33706(9) 0.0395(5) Uani 1 1 d . . . . .
C7 C 0.79764(12) 0.2420(2) 0.38134(10) 0.0367(5) Uani 1 1 d . . . . .
C8 C 0.85218(12) 0.2983(2) 0.42675(9) 0.0340(5) Uani 1 1 d . . . . .
C9 C 0.90413(12) 0.4214(2) 0.41642(9) 0.0355(5) Uani 1 1 d . . . . .
C10 C 0.95285(12) 0.5229(2) 0.42086(9) 0.0345(5) Uani 1 1 d . . . . .
C11 C 0.67366(11) 0.1309(2) 0.54617(9) 0.0343(5) Uani 1 1 d . . . . .
C12 C 0.62661(13) 0.2201(2) 0.50135(11) 0.0434(5) Uani 1 1 d . . . . .
H12 H 0.6433 0.2325 0.4619 0.052 Uiso 1 1 calc R . . . .
C13 C 0.55573(15) 0.2903(3) 0.51463(12) 0.0552(6) Uani 1 1 d . . . . .
H13 H 0.5248 0.3496 0.4843 0.066 Uiso 1 1 calc R . . . .
C14 C 0.53105(16) 0.2722(3) 0.57287(13) 0.0618(7) Uani 1 1 d . . . . .
H14 H 0.4830 0.3185 0.5821 0.074 Uiso 1 1 calc R . . . .
C15 C 0.57767(15) 0.1851(3) 0.61768(12) 0.0599(7) Uani 1 1 d . . . . .
H15 H 0.5608 0.1752 0.6572 0.072 Uiso 1 1 calc R . . . .
C16 C 0.64891(13) 0.1117(2) 0.60559(10) 0.0445(5) Uani 1 1 d . . . . .
C17 C 0.69772(18) 0.0166(3) 0.65529(12) 0.0660(7) Uani 1 1 d . . . . .
H17A H 0.6908 -0.0859 0.6435 0.099 Uiso 1 1 calc GR . . . .
H17B H 0.6779 0.0324 0.6950 0.099 Uiso 1 1 calc GR . . . .
H17C H 0.7556 0.0426 0.6592 0.099 Uiso 1 1 calc GR . . . .
C21 C 0.75636(12) -0.1066(2) 0.52837(9) 0.0345(5) Uani 1 1 d . . . . .
C22 C 0.68238(13) -0.1864(2) 0.51356(11) 0.0432(5) Uani 1 1 d . . . . .
H22 H 0.6320 -0.1358 0.5060 0.052 Uiso 1 1 calc R . . . .
C23 C 0.68295(15) -0.3393(2) 0.50991(12) 0.0536(6) Uani 1 1 d . . . . .
H23 H 0.6332 -0.3912 0.4999 0.064 Uiso 1 1 calc R . . . .
C24 C 0.75724(15) -0.4144(2) 0.52117(12) 0.0540(6) Uani 1 1 d . . . . .
H24 H 0.7580 -0.5174 0.5184 0.065 Uiso 1 1 calc R . . . .
C25 C 0.83056(15) -0.3371(2) 0.53662(11) 0.0498(6) Uani 1 1 d . . . . .
H25 H 0.8803 -0.3896 0.5446 0.060 Uiso 1 1 calc R . . . .
C26 C 0.83255(13) -0.1836(2) 0.54067(10) 0.0397(5) Uani 1 1 d . . . . .
C27 C 0.91482(14) -0.1076(3) 0.55844(13) 0.0576(6) Uani 1 1 d . . . . .
H27A H 0.9333 -0.0677 0.5212 0.086 Uiso 1 1 calc GR . . . .
H27B H 0.9550 -0.1779 0.5779 0.086 Uiso 1 1 calc GR . . . .
H27C H 0.9088 -0.0286 0.5875 0.086 Uiso 1 1 calc GR . . . .
C31 C 0.65610(14) 0.2621(3) 0.32917(10) 0.0483(6) Uani 1 1 d . . . . .
C32 C 0.58613(16) 0.1699(4) 0.32672(14) 0.0762(9) Uani 1 1 d D . . . .
H32 H 0.5930 0.0675 0.3295 0.091 Uiso 0.706(5) 1 calc R . P A 1
C33 C 0.5076(2) 0.2294(7) 0.3202(2) 0.1107(14) Uani 1 1 d . . . . .
H33 H 0.4616 0.1670 0.3188 0.133 Uiso 1 1 calc R . . . .
C34 C 0.4963(3) 0.3758(9) 0.31590(19) 0.1215(18) Uani 1 1 d . . . . .
H34 H 0.4425 0.4140 0.3118 0.146 Uiso 1 1 calc R . . . .
C35 C 0.5633(3) 0.4723(5) 0.31746(14) 0.1001(13) Uani 1 1 d . . . . .
H35 H 0.5542 0.5740 0.3134 0.120 Uiso 1 1 calc R . . . .
C36 C 0.64540(18) 0.4152(3) 0.32529(11) 0.0632(7) Uani 1 1 d D . . . .
H36 H 0.6911 0.4785 0.3278 0.076 Uiso 0.294(5) 1 calc R . P A 2
C37 C 0.7104(3) 0.5260(5) 0.3313(2) 0.0743(11) Uani 0.706(5) 1 d D . P A 1
H37A H 0.7296 0.5436 0.3753 0.111 Uiso 0.706(5) 1 calc GR . P A 1
H37B H 0.6888 0.6166 0.3118 0.111 Uiso 0.706(5) 1 calc GR . P A 1
H37C H 0.7558 0.4914 0.3111 0.111 Uiso 0.706(5) 1 calc GR . P A 1
C37A C 0.5917(7) 0.0142(10) 0.3470(5) 0.0743(11) Uani 0.294(5) 1 d D . P A 2
H37D H 0.6015 -0.0474 0.3122 0.111 Uiso 0.294(5) 1 calc GR . P A 2
H37E H 0.5405 -0.0148 0.3611 0.111 Uiso 0.294(5) 1 calc GR . P A 2
H37F H 0.6369 0.0029 0.3809 0.111 Uiso 0.294(5) 1 calc GR . P A 2
C41 C 0.75590(14) 0.0728(2) 0.29226(11) 0.0489(6) Uani 1 1 d . . . . .
C42 C 0.72318(17) 0.0966(3) 0.22801(12) 0.0665(7) Uani 1 1 d . . . . .
H42 H 0.6924 0.1819 0.2166 0.080 Uiso 1 1 calc R . . . .
C43 C 0.7362(2) -0.0042(4) 0.18236(15) 0.0847(9) Uani 1 1 d . . . . .
H43 H 0.7151 0.0130 0.1403 0.102 Uiso 1 1 calc R . . . .
C44 C 0.7804(2) -0.1296(4) 0.19951(16) 0.0872(10) Uani 1 1 d . . . . .
H44 H 0.7896 -0.1984 0.1688 0.105 Uiso 1 1 calc R . . . .
C45 C 0.8118(3) -0.1556(3) 0.26164(17) 0.0885(10) Uani 1 1 d . . . . .
H45 H 0.8405 -0.2435 0.2722 0.106 Uiso 1 1 calc R . . . .
C46 C 0.80186(19) -0.0542(3) 0.30952(13) 0.0653(7) Uani 1 1 d . . . . .
C47 C 0.8389(3) -0.0856(3) 0.37658(15) 0.0939(11) Uani 1 1 d . . . . .
H47A H 0.8846 -0.0191 0.3889 0.141 Uiso 1 1 calc GR . . . .
H47B H 0.8586 -0.1862 0.3800 0.141 Uiso 1 1 calc GR . . . .
H47C H 0.7973 -0.0717 0.4037 0.141 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.309(3) . ?
C1 C11 1.499(3) . ?
C1 C21 1.487(3) . ?
C2 C3 1.320(3) . ?
C3 C4 1.428(3) . ?
C3 C8 1.515(3) . ?
C4 C5 1.202(3) . ?
C5 C10 1.366(3) 3_766 ?
C6 C7 1.310(3) . ?
C6 C31 1.491(3) . ?
C6 C41 1.485(3) . ?
C7 C8 1.318(3) . ?
C8 C9 1.429(3) . ?
C9 C10 1.204(3) . ?
C10 C5 1.366(3) 3_766 ?
C11 C12 1.393(3) . ?
C11 C16 1.398(3) . ?
C12 C13 1.377(3) . ?
C13 C14 1.372(4) . ?
C14 C15 1.378(4) . ?
C15 C16 1.387(3) . ?
C16 C17 1.500(3) . ?
C21 C22 1.396(3) . ?
C21 C26 1.408(3) . ?
C22 C23 1.380(3) . ?
C23 C24 1.373(3) . ?
C24 C25 1.377(3) . ?
C25 C26 1.386(3) . ?
C26 C27 1.499(3) . ?
C31 C32 1.401(4) . ?
C31 C36 1.392(4) . ?
C32 C33 1.371(5) . ?
C32 C37A 1.467(9) . ?
C33 C34 1.333(7) . ?
C34 C35 1.389(7) . ?
C35 C36 1.415(5) . ?
C36 C37 1.443(5) . ?
C41 C42 1.417(4) . ?
C41 C46 1.387(4) . ?
C42 C43 1.372(4) . ?
C43 C44 1.360(5) . ?
C44 C45 1.374(5) . ?
C45 C46 1.399(4) . ?
C46 C47 1.501(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C11 117.00(16) . . ?
C2 C1 C21 123.13(17) . . ?
C21 C1 C11 119.76(16) . . ?
C1 C2 C3 175.66(19) . . ?
C2 C3 C4 122.51(18) . . ?
C2 C3 C8 121.60(17) . . ?
C4 C3 C8 115.82(16) . . ?
C5 C4 C3 165.87(19) . . ?
C4 C5 C10 167.11(19) . 3_766 ?
C7 C6 C31 118.67(19) . . ?
C7 C6 C41 123.10(19) . . ?
C41 C6 C31 118.17(18) . . ?
C6 C7 C8 176.6(2) . . ?
C7 C8 C3 122.17(17) . . ?
C7 C8 C9 122.21(18) . . ?
C9 C8 C3 115.58(16) . . ?
C10 C9 C8 166.6(2) . . ?
C9 C10 C5 167.9(2) . 3_766 ?
C12 C11 C1 118.59(18) . . ?
C12 C11 C16 119.85(18) . . ?
C16 C11 C1 121.57(17) . . ?
C13 C12 C11 120.9(2) . . ?
C14 C13 C12 119.6(2) . . ?
C13 C14 C15 119.8(2) . . ?
C14 C15 C16 122.0(2) . . ?
C11 C16 C17 121.63(19) . . ?
C15 C16 C11 117.8(2) . . ?
C15 C16 C17 120.6(2) . . ?
C22 C21 C1 117.55(17) . . ?
C22 C21 C26 119.45(18) . . ?
C26 C21 C1 122.98(17) . . ?
C23 C22 C21 121.0(2) . . ?
C24 C23 C22 119.7(2) . . ?
C23 C24 C25 119.9(2) . . ?
C24 C25 C26 122.1(2) . . ?
C21 C26 C27 123.24(19) . . ?
C25 C26 C21 117.87(19) . . ?
C25 C26 C27 118.88(19) . . ?
C32 C31 C6 118.4(2) . . ?
C36 C31 C6 122.1(2) . . ?
C36 C31 C32 119.5(2) . . ?
C31 C32 C37A 122.7(5) . . ?
C33 C32 C31 120.5(4) . . ?
C33 C32 C37A 114.9(5) . . ?
C34 C33 C32 120.7(4) . . ?
C33 C34 C35 121.3(4) . . ?
C34 C35 C36 119.7(4) . . ?
C31 C36 C35 118.3(3) . . ?
C31 C36 C37 126.7(3) . . ?
C35 C36 C37 114.9(3) . . ?
C42 C41 C6 116.2(2) . . ?
C46 C41 C6 124.0(2) . . ?
C46 C41 C42 119.7(2) . . ?
C43 C42 C41 121.1(3) . . ?
C44 C43 C42 119.1(3) . . ?
C43 C44 C45 120.7(3) . . ?
C44 C45 C46 122.1(3) . . ?
C41 C46 C45 117.2(3) . . ?
C41 C46 C47 122.4(2) . . ?
C45 C46 C47 120.3(3) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.444 0.250 224.1 8.7 ?
2 0.000 -0.601 0.750 224.1 8.7 ?

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
-2 6 0 0.0653 -2.3484 5.6997 0.1519 0.2707 -0.3193 0.9082
10 0 2 0.0084 10.0000 -0.0002 2.0010 -0.8564 -0.4759 -0.1535
-10 0 -2 0.0084 -10.0000 0.0002 -2.0010 0.8564 0.4759 0.1535
-3 0 14 0.0506 -2.8335 -0.1548 13.7752 -0.5117 0.7444 0.4290
0 -5 6 0.0607 0.4312 -5.2078 6.1473 -0.4479 0.6494 -0.6146
3 1 -14 0.0368 2.6918 0.5606 -13.7378 0.5276 -0.7675 -0.3641
-10 0 -1 0.0248 -10.2729 -0.3202 -0.9404 0.8156 0.5611 0.1414
-10 -1 -2 0.0016 -9.9866 -1.0087 -1.7418 0.8237 0.5669 0.0093
2 0 -14 0.0411 1.7698 0.2825 -13.8726 0.5990 -0.6992 -0.3902
1 -5 6 0.0574 1.2150 -5.0887 6.3523 -0.5154 0.6046 -0.6074
-2 0 14 0.0484 -1.7892 -0.2364 13.8768 -0.5969 0.6968 0.3977
-2 6 0 0.0653 -1.8878 5.7513 -0.0480 0.2475 -0.3576 0.9005

_olex2_date_sample_data_collection 2013-03-19
_olex2_date_sample_submission    1363561200
_olex2_exptl_crystal_mounting_method 'mounted on a loop'
_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_dw07
_database_code_depnum_ccdc_archive 'CCDC 1402909'
_audit_update_record             
;
2015-05-26 deposited with the CCDC.
2015-08-07 downloaded from the CCDC.
;
_audit_creation_date             2013-04-12
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C72 H56, 2(C H2 Cl2)'
_chemical_formula_sum            'C74 H60 Cl4'
_chemical_formula_weight         1091.02
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C36 H28'
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'

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

_cell_length_a                   9.7822(5)
_cell_length_b                   12.5174(6)
_cell_length_c                   12.6361(8)
_cell_angle_alpha                104.011(5)
_cell_angle_beta                 90.739(4)
_cell_angle_gamma                104.207(4)
_cell_volume                     1451.00(14)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4130
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      61.8770
_cell_measurement_theta_min      3.7550
_exptl_absorpt_coefficient_mu    2.181
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.2648
_exptl_crystal_size_mid          0.1574
_exptl_crystal_size_min          0.1046
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6450
_diffrn_reflns_theta_full        61.96
_diffrn_reflns_theta_max         61.96
_diffrn_reflns_theta_min         3.77
_diffrn_ambient_temperature      173.000(10)
_diffrn_detector_area_resol_mean 10.6144
_diffrn_measured_fraction_theta_full 0.9837
_diffrn_measured_fraction_theta_max 0.9527
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -86.00  -34.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -30.0000 52

#__ type_ start__ end____ width___ exp.time_
  2 omega  -26.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -150.0000 98

#__ type_ start__ end____ width___ exp.time_
  3 omega    7.00   42.00   1.0000    2.7900
omega____ theta____ kappa____ phi______ frames
    -       82.7293  -30.0000 -150.0000 35

#__ type_ start__ end____ width___ exp.time_
  4 omega   23.00  122.00   1.0000    2.7900
omega____ theta____ kappa____ phi______ frames
    -       82.7293 -125.0000  -30.0000 99

#__ type_ start__ end____ width___ exp.time_
  5 omega   57.00  155.00   1.0000    2.7900
omega____ theta____ kappa____ phi______ frames
    -       82.7293   30.0000 -150.0000 98

#__ type_ start__ end____ width___ exp.time_
  6 omega   54.00  149.00   1.0000    2.7900
omega____ theta____ kappa____ phi______ frames
    -       82.7293   30.0000  120.0000 95

#__ type_ start__ end____ width___ exp.time_
  7 omega   10.00   99.00   1.0000    2.7900
omega____ theta____ kappa____ phi______ frames
    -       82.7293  -45.0000  -60.0000 89

#__ type_ start__ end____ width___ exp.time_
  8 omega   56.00   98.00   1.0000    2.7900
omega____ theta____ kappa____ phi______ frames
    -       82.7293 -125.0000  120.0000 42

#__ type_ start__ end____ width___ exp.time_
  9 omega   19.00  115.00   1.0000    2.7900
omega____ theta____ kappa____ phi______ frames
    -       82.7293  -77.0000  120.0000 96
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0620895000
_diffrn_orient_matrix_UB_12      -0.1021834000
_diffrn_orient_matrix_UB_13      -0.0460138000
_diffrn_orient_matrix_UB_21      -0.0545971000
_diffrn_orient_matrix_UB_22      -0.0052352000
_diffrn_orient_matrix_UB_23      -0.1165242000
_diffrn_orient_matrix_UB_31      0.1404025000
_diffrn_orient_matrix_UB_32      0.0821681000
_diffrn_orient_matrix_UB_33      -0.0137175000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3828
_reflns_number_total             4350
_reflns_odcompleteness_completeness 98.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4350
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0529
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0812P)²+0.6294P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1474
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0570(2) 0.42432(18) 0.31266(17) 0.0249(5) Uani 1 1 d . . .
C2 C 0.1830(2) 0.44300(18) 0.36168(17) 0.0260(5) Uani 1 1 d . . .
C3 C 0.3075(2) 0.45270(17) 0.40994(17) 0.0240(5) Uani 1 1 d . . .
C4 C 0.3662(2) 0.53069(18) 0.51220(17) 0.0251(5) Uani 1 1 d . . .
C5 C 0.4561(2) 0.58266(18) 0.58501(17) 0.0253(5) Uani 1 1 d . . .
C6 C 0.5940(2) 0.61989(17) 0.64109(17) 0.0244(5) Uani 1 1 d . . .
C7 C 0.6394(2) 0.71017(18) 0.72335(18) 0.0270(5) Uani 1 1 d . . .
C8 C 0.6966(2) 0.80406(17) 0.79822(17) 0.0242(5) Uani 1 1 d . . .
C11 C -0.0586(2) 0.33297(18) 0.33793(18) 0.0280(5) Uani 1 1 d . . .
C12 C -0.0798(3) 0.3334(2) 0.4476(2) 0.0376(6) Uani 1 1 d . . .
H12 H -0.0229 0.3928 0.5041 0.045 Uiso 1 1 calc R . .
C13 C -0.1816(3) 0.2490(3) 0.4746(3) 0.0507(7) Uani 1 1 d . . .
H13 H -0.1971 0.2512 0.5491 0.061 Uiso 1 1 calc R . .
C14 C -0.2608(3) 0.1614(2) 0.3924(3) 0.0549(8) Uani 1 1 d . . .
H14 H -0.3303 0.1022 0.4105 0.066 Uiso 1 1 calc R . .
C15 C -0.2403(3) 0.1585(2) 0.2841(3) 0.0495(7) Uani 1 1 d . . .
H15 H -0.2960 0.0971 0.2288 0.059 Uiso 1 1 calc R . .
C16 C -0.1388(2) 0.2444(2) 0.2538(2) 0.0362(6) Uani 1 1 d . . .
C17 C -0.1137(3) 0.2355(2) 0.1362(2) 0.0468(7) Uani 1 1 d . . .
H17A H -0.1557 0.2888 0.1102 0.070 Uiso 1 1 calc R . .
H17B H -0.1572 0.1576 0.0932 0.070 Uiso 1 1 calc R . .
H17C H -0.0118 0.2542 0.1280 0.070 Uiso 1 1 calc R . .
C21 C 0.0242(2) 0.49529(17) 0.24144(17) 0.0262(5) Uani 1 1 d . . .
C22 C -0.1066(2) 0.5209(2) 0.24778(19) 0.0328(5) Uani 1 1 d . . .
H22 H -0.1715 0.4913 0.2953 0.039 Uiso 1 1 calc R . .
C23 C -0.1443(3) 0.5887(2) 0.1861(2) 0.0392(6) Uani 1 1 d . . .
H23 H -0.2339 0.6057 0.1914 0.047 Uiso 1 1 calc R . .
C24 C -0.0494(3) 0.6312(2) 0.1167(2) 0.0426(6) Uani 1 1 d . . .
H24 H -0.0730 0.6786 0.0748 0.051 Uiso 1 1 calc R . .
C25 C 0.0793(3) 0.6047(2) 0.1086(2) 0.0397(6) Uani 1 1 d . . .
H25 H 0.1422 0.6331 0.0594 0.048 Uiso 1 1 calc R . .
C26 C 0.1204(2) 0.53741(19) 0.17008(19) 0.0310(5) Uani 1 1 d . . .
C27 C 0.2611(3) 0.5100(2) 0.1552(2) 0.0432(6) Uani 1 1 d . . .
H27A H 0.3291 0.5589 0.2155 0.065 Uiso 1 1 calc R . .
H27B H 0.2951 0.5231 0.0857 0.065 Uiso 1 1 calc R . .
H27C H 0.2508 0.4299 0.1546 0.065 Uiso 1 1 calc R . .
C31 C 0.7021(2) 0.81266(17) 0.91790(17) 0.0253(5) Uani 1 1 d . . .
C32 C 0.8212(2) 0.88630(19) 0.98174(18) 0.0311(5) Uani 1 1 d . . .
H32 H 0.8929 0.9297 0.9479 0.037 Uiso 1 1 calc R . .
C33 C 0.8372(3) 0.8976(2) 1.09295(19) 0.0362(6) Uani 1 1 d . . .
H33 H 0.9195 0.9477 1.1350 0.043 Uiso 1 1 calc R . .
C34 C 0.7325(3) 0.8354(2) 1.14239(19) 0.0380(6) Uani 1 1 d . . .
H34 H 0.7424 0.8424 1.2188 0.046 Uiso 1 1 calc R . .
C35 C 0.6138(3) 0.7630(2) 1.08067(19) 0.0366(6) Uani 1 1 d . . .
H35 H 0.5425 0.7208 1.1158 0.044 Uiso 1 1 calc R . .
C36 C 0.5950(2) 0.74976(19) 0.96806(18) 0.0295(5) Uani 1 1 d . . .
C37 C 0.4610(3) 0.6703(2) 0.9058(2) 0.0472(7) Uani 1 1 d . . .
H37A H 0.4257 0.7061 0.8541 0.071 Uiso 1 1 calc R . .
H37B H 0.3894 0.6542 0.9573 0.071 Uiso 1 1 calc R . .
H37C H 0.4808 0.5989 0.8658 0.071 Uiso 1 1 calc R . .
C39 C 0.4025(3) 0.1710(3) 0.5229(2) 0.0564(8) Uani 1 1 d . . .
H39A H 0.4648 0.2115 0.4761 0.068 Uiso 1 1 calc R . .
H39B H 0.3440 0.0988 0.4753 0.068 Uiso 1 1 calc R . .
C41 C 0.7686(2) 0.90655(18) 0.75804(17) 0.0258(5) Uani 1 1 d . . .
C42 C 0.8738(2) 0.8956(2) 0.68596(18) 0.0322(5) Uani 1 1 d . . .
H42 H 0.8976 0.8248 0.6637 0.039 Uiso 1 1 calc R . .
C43 C 0.9443(3) 0.9867(2) 0.6461(2) 0.0435(6) Uani 1 1 d . . .
H43 H 1.0166 0.9784 0.5976 0.052 Uiso 1 1 calc R . .
C44 C 0.9088(3) 1.0885(2) 0.6773(2) 0.0490(7) Uani 1 1 d . . .
H44 H 0.9569 1.1514 0.6509 0.059 Uiso 1 1 calc R . .
C45 C 0.8028(3) 1.0996(2) 0.7474(2) 0.0475(7) Uani 1 1 d . . .
H45 H 0.7784 1.1703 0.7673 0.057 Uiso 1 1 calc R . .
C46 C 0.7302(2) 1.00972(19) 0.7899(2) 0.0352(6) Uani 1 1 d . . .
C47 C 0.6146(3) 1.0248(2) 0.8649(2) 0.0491(7) Uani 1 1 d . . .
H47A H 0.5392 0.9539 0.8496 0.074 Uiso 1 1 calc R . .
H47B H 0.5761 1.0865 0.8528 0.074 Uiso 1 1 calc R . .
H47C H 0.6530 1.0437 0.9410 0.074 Uiso 1 1 calc R . .
Cl1 Cl 0.50774(8) 0.13977(7) 0.61945(6) 0.0579(2) Uani 1 1 d . . .
Cl2 Cl 0.29193(10) 0.25467(7) 0.58386(6) 0.0657(3) Uani 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.313(3) . ?
C1 C11 1.497(3) . ?
C1 C21 1.491(3) . ?
C2 C3 1.320(3) . ?
C3 C4 1.431(3) . ?
C3 C6 1.527(3) 2_666 ?
C4 C5 1.204(3) . ?
C5 C6 1.431(3) . ?
C6 C3 1.527(3) 2_666 ?
C6 C7 1.314(3) . ?
C7 C8 1.310(3) . ?
C8 C31 1.489(3) . ?
C8 C41 1.510(3) . ?
C11 C12 1.403(3) . ?
C11 C16 1.398(3) . ?
C12 C13 1.375(4) . ?
C13 C14 1.375(4) . ?
C14 C15 1.379(5) . ?
C15 C16 1.405(4) . ?
C16 C17 1.491(4) . ?
C21 C22 1.392(3) . ?
C21 C26 1.409(3) . ?
C22 C23 1.391(3) . ?
C23 C24 1.385(4) . ?
C24 C25 1.378(4) . ?
C25 C26 1.396(3) . ?
C26 C27 1.502(4) . ?
C31 C32 1.395(3) . ?
C31 C36 1.405(3) . ?
C32 C33 1.381(3) . ?
C33 C34 1.381(4) . ?
C34 C35 1.377(4) . ?
C35 C36 1.396(3) . ?
C36 C37 1.511(3) . ?
C39 Cl1 1.760(3) . ?
C39 Cl2 1.745(3) . ?
C41 C42 1.393(3) . ?
C41 C46 1.401(3) . ?
C42 C43 1.389(3) . ?
C43 C44 1.371(4) . ?
C44 C45 1.383(4) . ?
C45 C46 1.403(4) . ?
C46 C47 1.502(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C11 117.1(2) . . ?
C2 C1 C21 122.80(19) . . ?
C21 C1 C11 119.93(18) . . ?
C1 C2 C3 175.3(2) . . ?
C2 C3 C4 125.3(2) . . ?
C2 C3 C6 122.01(19) . 2_666 ?
C4 C3 C6 112.70(17) . 2_666 ?
C5 C4 C3 156.8(2) . . ?
C4 C5 C6 156.9(2) . . ?
C5 C6 C3 112.66(17) . 2_666 ?
C7 C6 C3 121.28(19) . 2_666 ?
C7 C6 C5 125.9(2) . . ?
C8 C7 C6 173.2(2) . . ?
C7 C8 C31 124.0(2) . . ?
C7 C8 C41 116.69(19) . . ?
C31 C8 C41 119.20(17) . . ?
C12 C11 C1 119.0(2) . . ?
C16 C11 C1 120.6(2) . . ?
C16 C11 C12 120.2(2) . . ?
C13 C12 C11 121.0(3) . . ?
C14 C13 C12 119.2(3) . . ?
C13 C14 C15 120.7(3) . . ?
C14 C15 C16 121.5(3) . . ?
C11 C16 C15 117.3(2) . . ?
C11 C16 C17 122.4(2) . . ?
C15 C16 C17 120.2(2) . . ?
C22 C21 C1 117.72(19) . . ?
C22 C21 C26 119.7(2) . . ?
C26 C21 C1 122.56(19) . . ?
C23 C22 C21 121.4(2) . . ?
C24 C23 C22 119.0(2) . . ?
C25 C24 C23 119.9(2) . . ?
C24 C25 C26 122.3(2) . . ?
C21 C26 C27 123.0(2) . . ?
C25 C26 C21 117.6(2) . . ?
C25 C26 C27 119.4(2) . . ?
C32 C31 C8 117.43(19) . . ?
C32 C31 C36 119.3(2) . . ?
C36 C31 C8 123.27(19) . . ?
C33 C32 C31 121.5(2) . . ?
C32 C33 C34 119.3(2) . . ?
C35 C34 C33 119.9(2) . . ?
C34 C35 C36 122.0(2) . . ?
C31 C36 C37 122.9(2) . . ?
C35 C36 C31 118.0(2) . . ?
C35 C36 C37 119.1(2) . . ?
Cl2 C39 Cl1 112.60(16) . . ?
C42 C41 C8 118.15(19) . . ?
C42 C41 C46 120.2(2) . . ?
C46 C41 C8 121.7(2) . . ?
C43 C42 C41 121.0(2) . . ?
C44 C43 C42 119.5(3) . . ?
C43 C44 C45 119.9(2) . . ?
C44 C45 C46 122.2(3) . . ?
C41 C46 C45 117.2(2) . . ?
C41 C46 C47 122.2(2) . . ?
C45 C46 C47 120.6(2) . . ?

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
6 -1 1 0.1085 6.2258 -0.8876 0.7445 0.4430 -0.4220 0.7910
0 7 -5 0.0649 0.2490 7.3235 -4.6501 -0.5189 0.4899 0.7005
-6 1 -1 0.1288 -6.2447 1.4286 -1.0892 -0.4836 0.4604 -0.7444
0 -7 5 0.0860 0.2561 -7.4418 4.7399 0.5582 -0.5273 -0.6405
2 0 7 0.0529 2.3195 0.4805 6.9281 -0.2239 -0.9364 0.2701
0 -1 8 0.0569 0.1083 -1.3831 8.1699 -0.2279 -0.9507 -0.2105
-1 1 -8 0.0476 -0.9061 0.7511 -7.9472 0.2327 0.9716 0.0435
6 -2 -3 0.1058 6.0366 -1.5803 -2.6239 0.6570 -0.0156 0.7537
0 -8 0 0.0738 0.2766 -7.7897 0.4033 0.7946 -0.0213 -0.6068
-6 1 3 0.1178 -6.0175 0.7930 2.6687 -0.5774 0.0134 -0.8163
1 7 -1 0.0615 0.9179 7.4248 -0.9190 -0.6594 0.0181 0.7516
1 0 -8 0.0608 0.8763 0.0243 -7.9465 0.4176 0.8780 0.2340
-1 -1 -7 0.0577 -0.7742 -1.3775 -7.2645 0.4270 0.8960 -0.1222
-5 -4 3 0.1235 -4.5753 -3.7703 3.1083 -0.0418 -0.0927 -0.9948
0 1 8 0.0575 -0.0125 0.7211 7.7130 -0.4294 -0.9018 -0.0483

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
