# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2016

####################################################################### 
# 
# 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 
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data_Tr-H1
_database_code_depnum_ccdc_archive 'CCDC 1507657'
_audit_update_record             
;
2016-09-30 deposited with the CCDC.
2016-11-08 downloaded from the CCDC.
;

_vrf_CHEMW03_Tr-H1               
;
RESPONSE: Attempts to refine peaks of residual electron density as
disordered or partial-occupancy solvent dichloromethane chlorine or
carbon atoms were unsuccessful.  The data were corrected for disordered
electron density through use of the SQUEEZE procedure as implemented in
PLATON (Spek, A. L. Acta Crystallogr. 2015, C71, 9-18.  PLATON - a
multipurpose crystallographic tool.  Utrecht University, Utrecht, The
Netherlands).  A total solvent-accessible void volume of 494 cubic
Angstroms with a total electron count of 165 (consistent with four
moleculeS of solvent dichloromethane, or one molecule per formula unit
of 3,3,3-tris(3,5-di-t-butyl)prop-1-yne)) was found in the unit cell.
;

_vrf_FORMU01_Tr-H1               
;
RESPONSE: See above response to CHEMW03 alert concerning the use of
PLATON/SQUEEZE for dealing with highly disordered cocrystallized
solvent CH2Cl2.
;

_vrf_CELLZ01_Tr-H1               
;
RESPONSE: See above response to CHEMW03 alert concerning the use of
PLATON/SQUEEZE for dealing with highly disordered cocrystallized
solvent CH2Cl2.
;

_vrf_PLAT041_Tr-H1               
;
RESPONSE: See above response to CHEMW03 alert concerning the use of
PLATON/SQUEEZE for dealing with highly disordered cocrystallized
solvent CH2Cl2.
;

_vrf_PLAT051_Tr-H1               
;
RESPONSE: See above response to CHEMW03 alert concerning the use of
PLATON/SQUEEZE for dealing with highly disordered cocrystallized
solvent CH2Cl2.
;

_vrf_PLAT068_Tr-H1               
;
RESPONSE: See above response to CHEMW03 alert concerning the use of
PLATON/SQUEEZE for dealing with highly disordered cocrystallized
solvent CH2Cl2.
;

_vrf_PLAT605_Tr-H1               
;
RESPONSE: See above response to CHEMW03 alert concerning the use of
PLATON/SQUEEZE for dealing with highly disordered cocrystallized
solvent CH2Cl2.
;

_audit_creation_method           SHELXL-2014/7

_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'3,3,3-tris(3,5-di-t-butyl)prop-1-yne, dichloromethane solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H64, C H2 Cl2'
_chemical_formula_sum            'C46 H66 Cl2'
_chemical_formula_weight         689.88

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/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.4263(9)
_cell_length_b                   10.2668(9)
_cell_length_c                   40.789(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.6212(14)
_cell_angle_gamma                90
_cell_volume                     4366.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    5254
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      25.25

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_F_000             1504
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.590
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    0.176
_shelx_estimated_absorpt_T_min   0.903
_shelx_estimated_absorpt_T_max   0.962
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8924
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31531
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_theta_min         1.997
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8298
_reflns_number_gt                6236
_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. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0598P)²+2.0474P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8298
_refine_ls_number_parameters     455
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0607
_refine_ls_wR_factor_ref         0.1593
_refine_ls_wR_factor_gt          0.1479
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.072
_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 0.2794(2) 0.0908(2) 0.17139(6) 0.0562(6) Uani 1 1 d . . . . .
H1 H 0.3316 0.0416 0.1861 0.067 Uiso 1 1 calc R U . . .
C2 C 0.21429(19) 0.15208(19) 0.15309(5) 0.0390(5) Uani 1 1 d . . . . .
C3 C 0.13150(17) 0.22922(18) 0.13041(4) 0.0328(4) Uani 1 1 d . . . . .
C11 C 0.15437(17) 0.37511(18) 0.13806(4) 0.0330(4) Uani 1 1 d . . . . .
C12 C 0.05406(17) 0.46105(18) 0.14262(4) 0.0329(4) Uani 1 1 d . . . . .
H12 H -0.0317 0.4301 0.1411 0.039 Uiso 1 1 calc R U . . .
C13 C 0.07641(18) 0.59253(18) 0.14943(4) 0.0351(4) Uani 1 1 d . . . . .
C14 C 0.20243(18) 0.63551(19) 0.15116(5) 0.0377(4) Uani 1 1 d . . . . .
H14 H 0.2187 0.7246 0.1559 0.045 Uiso 1 1 calc R U . . .
C15 C 0.30614(18) 0.5522(2) 0.14614(5) 0.0395(5) Uani 1 1 d . . . . .
C16 C 0.27957(18) 0.4220(2) 0.13986(5) 0.0396(5) Uani 1 1 d . . . . .
H16 H 0.3487 0.3632 0.1367 0.047 Uiso 1 1 calc R U . . .
C17 C -0.03886(19) 0.68253(19) 0.15509(5) 0.0436(5) Uani 1 1 d . . . . .
C18 C -0.1076(2) 0.6376(2) 0.18619(6) 0.0600(6) Uani 1 1 d . . . . .
H18A H -0.1333 0.5463 0.1837 0.072 Uiso 1 1 calc R U . . .
H18B H -0.0495 0.6463 0.2051 0.072 Uiso 1 1 calc R U . . .
H18C H -0.1839 0.6915 0.1896 0.072 Uiso 1 1 calc R U . . .
C19 C 0.0001(2) 0.8247(2) 0.15948(7) 0.0631(7) Uani 1 1 d . . . . .
H19A H 0.0595 0.8323 0.1782 0.076 Uiso 1 1 calc R U . . .
H19B H 0.0421 0.8556 0.1396 0.076 Uiso 1 1 calc R U . . .
H19C H -0.0764 0.8775 0.1635 0.076 Uiso 1 1 calc R U . . .
C20 C -0.1314(2) 0.6745(2) 0.12579(7) 0.0596(6) Uani 1 1 d . . . . .
H20A H -0.1578 0.5838 0.1225 0.071 Uiso 1 1 calc R U . . .
H20B H -0.2071 0.7282 0.1301 0.071 Uiso 1 1 calc R U . . .
H20C H -0.0885 0.7063 0.1061 0.071 Uiso 1 1 calc R U . . .
C21 C 0.4456(2) 0.6012(2) 0.14695(6) 0.0544(6) Uani 1 1 d D . . . .
C22A C 0.4974(3) 0.5913(4) 0.11082(9) 0.0732(10) Uani 0.8 1 d . . P A 1
H22A H 0.4455 0.6468 0.0963 0.088 Uiso 0.8 1 calc R U P A 1
H22B H 0.5870 0.6201 0.1104 0.088 Uiso 0.8 1 calc R U P A 1
H22C H 0.4919 0.5008 0.1033 0.088 Uiso 0.8 1 calc R U P A 1
C23A C 0.4581(3) 0.7433(4) 0.15613(11) 0.0821(12) Uani 0.8 1 d . . P A 1
H23A H 0.4026 0.7958 0.1417 0.099 Uiso 0.8 1 calc R U P A 1
H23B H 0.4322 0.7554 0.1790 0.099 Uiso 0.8 1 calc R U P A 1
H23C H 0.5474 0.7710 0.1536 0.099 Uiso 0.8 1 calc R U P A 1
C24A C 0.5278(3) 0.5151(4) 0.16797(12) 0.0859(12) Uani 0.8 1 d . . P A 1
H24A H 0.5166 0.4242 0.1611 0.103 Uiso 0.8 1 calc R U P A 1
H24B H 0.6180 0.5401 0.1656 0.103 Uiso 0.8 1 calc R U P A 1
H24C H 0.5028 0.5244 0.1909 0.103 Uiso 0.8 1 calc R U P A 1
C22B C 0.4634(15) 0.7122(13) 0.1232(3) 0.077(2) Uiso 0.2 1 d D U P A 2
H22D H 0.3979 0.7788 0.1271 0.092 Uiso 0.2 1 calc R U P A 2
H22E H 0.5488 0.7503 0.1265 0.092 Uiso 0.2 1 calc R U P A 2
H22F H 0.4550 0.6797 0.1007 0.092 Uiso 0.2 1 calc R U P A 2
C23B C 0.4643(15) 0.6595(15) 0.1825(3) 0.077(2) Uiso 0.2 1 d D U P A 2
H23D H 0.4535 0.5903 0.1987 0.092 Uiso 0.2 1 calc R U P A 2
H23E H 0.5506 0.6966 0.1846 0.092 Uiso 0.2 1 calc R U P A 2
H23F H 0.4004 0.7278 0.1861 0.092 Uiso 0.2 1 calc R U P A 2
C24B C 0.5454(13) 0.4936(13) 0.1421(4) 0.077(2) Uiso 0.2 1 d D U P A 2
H24D H 0.5307 0.4235 0.1580 0.092 Uiso 0.2 1 calc R U P A 2
H24E H 0.5378 0.4590 0.1198 0.092 Uiso 0.2 1 calc R U P A 2
H24F H 0.6316 0.5296 0.1455 0.092 Uiso 0.2 1 calc R U P A 2
C31 C 0.17064(16) 0.19532(17) 0.09490(4) 0.0316(4) Uani 1 1 d . . . . .
C32 C 0.17712(17) 0.06400(18) 0.08603(5) 0.0338(4) Uani 1 1 d . . . . .
H32 H 0.1606 -0.0008 0.1021 0.041 Uiso 1 1 calc R U . . .
C33 C 0.20689(18) 0.02635(17) 0.05456(4) 0.0340(4) Uani 1 1 d . . . . .
C34 C 0.23311(18) 0.12389(18) 0.03163(5) 0.0362(4) Uani 1 1 d . . . . .
H34 H 0.2548 0.0993 0.0099 0.043 Uiso 1 1 calc R U . . .
C35 C 0.22847(17) 0.25475(18) 0.03948(5) 0.0352(4) Uani 1 1 d . . . . .
C36 C 0.19480(17) 0.28893(18) 0.07144(5) 0.0345(4) Uani 1 1 d . . . . .
H36 H 0.1884 0.3784 0.0771 0.041 Uiso 1 1 calc R U . . .
C37 C 0.2134(2) -0.11707(18) 0.04402(5) 0.0413(5) Uani 1 1 d . . . . .
C38 C 0.1193(3) -0.1393(2) 0.01533(6) 0.0616(6) Uani 1 1 d . . . . .
H38A H 0.1409 -0.0809 -0.0028 0.074 Uiso 1 1 calc R U . . .
H38B H 0.1253 -0.2299 0.0079 0.074 Uiso 1 1 calc R U . . .
H38C H 0.0317 -0.1214 0.0225 0.074 Uiso 1 1 calc R U . . .
C39 C 0.1775(3) -0.2088(2) 0.07160(6) 0.0639(7) Uani 1 1 d . . . . .
H39A H 0.0901 -0.1895 0.0788 0.077 Uiso 1 1 calc R U . . .
H39B H 0.1819 -0.2989 0.0638 0.077 Uiso 1 1 calc R U . . .
H39C H 0.2374 -0.1971 0.0900 0.077 Uiso 1 1 calc R U . . .
C40 C 0.3499(2) -0.1481(2) 0.03309(6) 0.0578(6) Uani 1 1 d . . . . .
H40A H 0.3738 -0.0892 0.0153 0.069 Uiso 1 1 calc R U . . .
H40B H 0.4094 -0.1365 0.0516 0.069 Uiso 1 1 calc R U . . .
H40C H 0.3538 -0.2384 0.0254 0.069 Uiso 1 1 calc R U . . .
C41 C 0.2593(2) 0.36048(19) 0.01417(5) 0.0446(5) Uani 1 1 d D . . . .
C42A C 0.3054(4) 0.3099(3) -0.01750(8) 0.0655(10) Uani 0.75 1 d . . P B 1
H42A H 0.3819 0.2562 -0.0137 0.079 Uiso 0.75 1 calc R U P B 1
H42B H 0.2381 0.2569 -0.0279 0.079 Uiso 0.75 1 calc R U P B 1
H42C H 0.3269 0.3829 -0.0319 0.079 Uiso 0.75 1 calc R U P B 1
C43A C 0.3666(3) 0.4509(3) 0.02959(8) 0.0531(8) Uani 0.75 1 d . . P B 1
H43A H 0.3373 0.4852 0.0506 0.064 Uiso 0.75 1 calc R U P B 1
H43B H 0.4453 0.4002 0.0330 0.064 Uiso 0.75 1 calc R U P B 1
H43C H 0.3840 0.5234 0.0146 0.064 Uiso 0.75 1 calc R U P B 1
C44A C 0.1401(3) 0.4448(3) 0.00960(8) 0.0518(7) Uani 0.75 1 d . . P B 1
H44A H 0.1120 0.4768 0.0310 0.062 Uiso 0.75 1 calc R U P B 1
H44B H 0.1603 0.5189 -0.0046 0.062 Uiso 0.75 1 calc R U P B 1
H44C H 0.0715 0.3929 -0.0005 0.062 Uiso 0.75 1 calc R U P B 1
C42B C 0.1735(11) 0.3339(12) -0.0182(2) 0.0765(18) Uiso 0.25 1 d D U P B 2
H42D H 0.1819 0.2424 -0.0247 0.092 Uiso 0.25 1 calc R U P B 2
H42E H 0.0834 0.3530 -0.0136 0.092 Uiso 0.25 1 calc R U P B 2
H42F H 0.2030 0.3900 -0.0361 0.092 Uiso 0.25 1 calc R U P B 2
C43B C 0.3910(10) 0.3281(12) -0.0006(3) 0.0765(18) Uiso 0.25 1 d D U P B 2
H43D H 0.3961 0.2344 -0.0050 0.092 Uiso 0.25 1 calc R U P B 2
H43E H 0.4014 0.3762 -0.0212 0.092 Uiso 0.25 1 calc R U P B 2
H43F H 0.4591 0.3531 0.0149 0.092 Uiso 0.25 1 calc R U P B 2
C44B C 0.2400(12) 0.4993(9) 0.0218(3) 0.0765(18) Uiso 0.25 1 d D U P B 2
H44D H 0.2646 0.5523 0.0029 0.092 Uiso 0.25 1 calc R U P B 2
H44E H 0.1495 0.5147 0.0268 0.092 Uiso 0.25 1 calc R U P B 2
H44F H 0.2932 0.5233 0.0408 0.092 Uiso 0.25 1 calc R U P B 2
C51 C -0.01003(17) 0.19205(17) 0.13645(4) 0.0312(4) Uani 1 1 d . . . . .
C52 C -0.09702(18) 0.18071(18) 0.11080(4) 0.0342(4) Uani 1 1 d . . . . .
H52 H -0.0681 0.1903 0.0889 0.041 Uiso 1 1 calc R U . . .
C53 C -0.22661(18) 0.15538(19) 0.11640(5) 0.0367(4) Uani 1 1 d . . . . .
C54 C -0.26607(19) 0.14164(19) 0.14844(5) 0.0397(5) Uani 1 1 d . . . . .
H54 H -0.3541 0.1250 0.1525 0.048 Uiso 1 1 calc R U . . .
C55 C -0.18089(19) 0.15146(18) 0.17499(5) 0.0375(4) Uani 1 1 d . . . . .
C56 C -0.05309(18) 0.17706(18) 0.16853(5) 0.0353(4) Uani 1 1 d . . . . .
H56 H 0.0063 0.1846 0.1863 0.042 Uiso 1 1 calc R U . . .
C57 C -0.3188(2) 0.1396(2) 0.08706(5) 0.0486(5) Uani 1 1 d . . . . .
C58 C -0.2843(2) 0.0144(3) 0.06897(6) 0.0610(6) Uani 1 1 d . . . . .
H58A H -0.1944 0.0182 0.0622 0.073 Uiso 1 1 calc R U . . .
H58B H -0.2966 -0.0604 0.0835 0.073 Uiso 1 1 calc R U . . .
H58C H -0.3397 0.0050 0.0495 0.073 Uiso 1 1 calc R U . . .
C59 C -0.3058(2) 0.2563(3) 0.06384(6) 0.0638(7) Uani 1 1 d . . . . .
H59A H -0.3280 0.3365 0.0755 0.077 Uiso 1 1 calc R U . . .
H59B H -0.2172 0.2620 0.0562 0.077 Uiso 1 1 calc R U . . .
H59C H -0.3638 0.2450 0.0450 0.077 Uiso 1 1 calc R U . . .
C60 C -0.4595(2) 0.1311(3) 0.09733(7) 0.0743(8) Uani 1 1 d . . . . .
H60A H -0.4834 0.2108 0.1090 0.089 Uiso 1 1 calc R U . . .
H60B H -0.5142 0.1212 0.0778 0.089 Uiso 1 1 calc R U . . .
H60C H -0.4711 0.0558 0.1118 0.089 Uiso 1 1 calc R U . . .
C61 C -0.2304(2) 0.1367(2) 0.21015(5) 0.0504(5) Uani 1 1 d . . . . .
C62A C -0.2955(10) 0.0054(8) 0.2131(3) 0.113(4) Uani 0.6 1 d . . P C 1
H62A H -0.3610 -0.0034 0.1958 0.135 Uiso 0.6 1 calc R U P C 1
H62B H -0.2317 -0.0640 0.2108 0.135 Uiso 0.6 1 calc R U P C 1
H62C H -0.3361 -0.0015 0.2346 0.135 Uiso 0.6 1 calc R U P C 1
C63A C -0.3334(6) 0.2416(6) 0.21664(13) 0.0703(15) Uani 0.6 1 d . . P C 1
H63A H -0.4016 0.2349 0.2000 0.084 Uiso 0.6 1 calc R U P C 1
H63B H -0.3697 0.2281 0.2384 0.084 Uiso 0.6 1 calc R U P C 1
H63C H -0.2941 0.3282 0.2156 0.084 Uiso 0.6 1 calc R U P C 1
C64A C -0.1288(9) 0.1528(12) 0.23659(18) 0.133(5) Uani 0.6 1 d . . P C 1
H64A H -0.0877 0.2381 0.2343 0.160 Uiso 0.6 1 calc R U P C 1
H64B H -0.1686 0.1466 0.2582 0.160 Uiso 0.6 1 calc R U P C 1
H64C H -0.0642 0.0841 0.2344 0.160 Uiso 0.6 1 calc R U P C 1
C62B C -0.3478(13) 0.0550(16) 0.2124(3) 0.124(7) Uani 0.4 1 d . . P C 2
H62D H -0.3307 -0.0313 0.2031 0.148 Uiso 0.4 1 calc R U P C 2
H62E H -0.3722 0.0460 0.2354 0.148 Uiso 0.4 1 calc R U P C 2
H62F H -0.4179 0.0964 0.2000 0.148 Uiso 0.4 1 calc R U P C 2
C63B C -0.2459(11) 0.2716(9) 0.2237(2) 0.087(3) Uani 0.4 1 d . . P C 2
H63D H -0.1652 0.3196 0.2214 0.105 Uiso 0.4 1 calc R U P C 2
H63E H -0.3142 0.3170 0.2115 0.105 Uiso 0.4 1 calc R U P C 2
H63F H -0.2685 0.2665 0.2469 0.105 Uiso 0.4 1 calc R U P C 2
C64B C -0.1249(14) 0.0699(11) 0.2309(3) 0.083(3) Uani 0.4 1 d . . P C 2
H64D H -0.0459 0.1215 0.2300 0.100 Uiso 0.4 1 calc R U P C 2
H64E H -0.1529 0.0633 0.2537 0.100 Uiso 0.4 1 calc R U P C 2
H64F H -0.1087 -0.0175 0.2222 0.100 Uiso 0.4 1 calc R U P C 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.185(3) . ?
C2 C3 1.487(3) . ?
C3 C51 1.546(2) . ?
C3 C11 1.548(3) . ?
C3 C31 1.549(2) . ?
C11 C12 1.382(3) . ?
C11 C16 1.392(3) . ?
C12 C13 1.397(3) . ?
C13 C14 1.387(3) . ?
C13 C17 1.535(3) . ?
C14 C15 1.396(3) . ?
C15 C16 1.388(3) . ?
C15 C21 1.539(3) . ?
C17 C19 1.525(3) . ?
C17 C20 1.530(3) . ?
C17 C18 1.535(3) . ?
C21 C24A 1.495(4) . ?
C21 C22B 1.507(10) . ?
C21 C23A 1.512(4) . ?
C21 C24B 1.532(10) . ?
C21 C23B 1.577(10) . ?
C21 C22A 1.578(4) . ?
C31 C36 1.381(3) . ?
C31 C32 1.398(3) . ?
C32 C33 1.379(3) . ?
C33 C34 1.399(3) . ?
C33 C37 1.536(3) . ?
C34 C35 1.382(3) . ?
C35 C36 1.399(3) . ?
C35 C41 1.534(3) . ?
C37 C39 1.517(3) . ?
C37 C40 1.529(3) . ?
C37 C38 1.536(3) . ?
C41 C44B 1.473(9) . ?
C41 C42A 1.478(4) . ?
C41 C44A 1.524(4) . ?
C41 C43B 1.542(9) . ?
C41 C43A 1.579(4) . ?
C41 C42B 1.611(9) . ?
C51 C52 1.382(3) . ?
C51 C56 1.397(3) . ?
C52 C53 1.397(3) . ?
C53 C54 1.382(3) . ?
C53 C57 1.535(3) . ?
C54 C55 1.397(3) . ?
C55 C56 1.386(3) . ?
C55 C61 1.537(3) . ?
C57 C58 1.528(3) . ?
C57 C60 1.533(3) . ?
C57 C59 1.534(3) . ?
C61 C62B 1.488(12) . ?
C61 C63B 1.500(9) . ?
C61 C64A 1.513(9) . ?
C61 C62A 1.515(9) . ?
C61 C64B 1.542(14) . ?
C61 C63A 1.545(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
C1 C2 C3 179.3(2) . . ?
C2 C3 C51 108.55(15) . . ?
C2 C3 C11 107.64(15) . . ?
C51 C3 C11 110.60(14) . . ?
C2 C3 C31 107.76(15) . . ?
C51 C3 C31 110.78(14) . . ?
C11 C3 C31 111.36(15) . . ?
C12 C11 C16 118.84(17) . . ?
C12 C11 C3 121.98(16) . . ?
C16 C11 C3 119.17(16) . . ?
C11 C12 C13 121.24(17) . . ?
C14 C13 C12 118.24(17) . . ?
C14 C13 C17 122.92(17) . . ?
C12 C13 C17 118.83(17) . . ?
C13 C14 C15 122.17(18) . . ?
C16 C15 C14 117.64(17) . . ?
C16 C15 C21 120.38(18) . . ?
C14 C15 C21 121.98(18) . . ?
C15 C16 C11 121.84(18) . . ?
C19 C17 C20 108.0(2) . . ?
C19 C17 C18 108.46(19) . . ?
C20 C17 C18 109.46(19) . . ?
C19 C17 C13 112.70(17) . . ?
C20 C17 C13 109.77(17) . . ?
C18 C17 C13 108.46(17) . . ?
C24A C21 C23A 112.5(3) . . ?
C22B C21 C24B 112.0(9) . . ?
C24A C21 C15 110.7(2) . . ?
C22B C21 C15 110.8(6) . . ?
C23A C21 C15 113.6(2) . . ?
C24B C21 C15 113.9(6) . . ?
C22B C21 C23B 106.7(9) . . ?
C24B C21 C23B 108.3(9) . . ?
C15 C21 C23B 104.5(6) . . ?
C24A C21 C22A 107.3(3) . . ?
C23A C21 C22A 105.3(3) . . ?
C15 C21 C22A 106.94(19) . . ?
C36 C31 C32 118.83(16) . . ?
C36 C31 C3 122.91(16) . . ?
C32 C31 C3 118.22(16) . . ?
C33 C32 C31 121.56(17) . . ?
C32 C33 C34 117.97(17) . . ?
C32 C33 C37 122.73(17) . . ?
C34 C33 C37 119.30(16) . . ?
C35 C34 C33 122.22(17) . . ?
C34 C35 C36 118.01(17) . . ?
C34 C35 C41 121.58(17) . . ?
C36 C35 C41 120.41(17) . . ?
C31 C36 C35 121.37(17) . . ?
C39 C37 C40 108.93(19) . . ?
C39 C37 C33 112.05(16) . . ?
C40 C37 C33 108.98(17) . . ?
C39 C37 C38 108.19(19) . . ?
C40 C37 C38 109.62(19) . . ?
C33 C37 C38 109.04(17) . . ?
C42A C41 C44A 111.4(2) . . ?
C44B C41 C35 120.8(5) . . ?
C42A C41 C35 114.32(19) . . ?
C44A C41 C35 107.93(18) . . ?
C44B C41 C43B 114.5(7) . . ?
C35 C41 C43B 107.7(5) . . ?
C42A C41 C43A 108.6(2) . . ?
C44A C41 C43A 106.7(2) . . ?
C35 C41 C43A 107.49(19) . . ?
C44B C41 C42B 105.2(7) . . ?
C35 C41 C42B 108.3(5) . . ?
C43B C41 C42B 97.5(7) . . ?
C52 C51 C56 119.01(17) . . ?
C52 C51 C3 121.32(16) . . ?
C56 C51 C3 119.56(16) . . ?
C51 C52 C53 121.33(17) . . ?
C54 C53 C52 118.16(17) . . ?
C54 C53 C57 122.41(17) . . ?
C52 C53 C57 119.39(17) . . ?
C53 C54 C55 122.19(18) . . ?
C56 C55 C54 118.08(17) . . ?
C56 C55 C61 121.97(18) . . ?
C54 C55 C61 119.94(18) . . ?
C55 C56 C51 121.23(18) . . ?
C58 C57 C60 108.4(2) . . ?
C58 C57 C59 109.65(19) . . ?
C60 C57 C59 107.8(2) . . ?
C58 C57 C53 108.44(18) . . ?
C60 C57 C53 112.73(18) . . ?
C59 C57 C53 109.86(18) . . ?
C62B C61 C63B 114.0(7) . . ?
C64A C61 C62A 110.6(6) . . ?
C62B C61 C55 113.4(4) . . ?
C63B C61 C55 106.9(3) . . ?
C64A C61 C55 114.5(4) . . ?
C62A C61 C55 108.5(4) . . ?
C62B C61 C64B 107.4(8) . . ?
C63B C61 C64B 106.7(6) . . ?
C55 C61 C64B 108.1(4) . . ?
C64A C61 C63A 106.5(4) . . ?
C62A C61 C63A 107.1(4) . . ?
C55 C61 C63A 109.4(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C3 C11 C12 -131.05(18) . . . . ?
C51 C3 C11 C12 -12.6(2) . . . . ?
C31 C3 C11 C12 111.04(19) . . . . ?
C2 C3 C11 C16 50.1(2) . . . . ?
C51 C3 C11 C16 168.53(16) . . . . ?
C31 C3 C11 C16 -67.8(2) . . . . ?
C16 C11 C12 C13 -1.0(3) . . . . ?
C3 C11 C12 C13 -179.86(17) . . . . ?
C11 C12 C13 C14 0.7(3) . . . . ?
C11 C12 C13 C17 -178.51(17) . . . . ?
C12 C13 C14 C15 0.4(3) . . . . ?
C17 C13 C14 C15 179.62(18) . . . . ?
C13 C14 C15 C16 -1.2(3) . . . . ?
C13 C14 C15 C21 177.94(19) . . . . ?
C14 C15 C16 C11 1.0(3) . . . . ?
C21 C15 C16 C11 -178.22(19) . . . . ?
C12 C11 C16 C15 0.1(3) . . . . ?
C3 C11 C16 C15 179.02(18) . . . . ?
C14 C13 C17 C19 5.4(3) . . . . ?
C12 C13 C17 C19 -175.35(19) . . . . ?
C14 C13 C17 C20 125.8(2) . . . . ?
C12 C13 C17 C20 -55.0(2) . . . . ?
C14 C13 C17 C18 -114.6(2) . . . . ?
C12 C13 C17 C18 64.6(2) . . . . ?
C16 C15 C21 C24A -48.8(3) . . . . ?
C14 C15 C21 C24A 132.0(3) . . . . ?
C16 C15 C21 C22B 124.3(7) . . . . ?
C14 C15 C21 C22B -54.8(7) . . . . ?
C16 C15 C21 C23A -176.5(3) . . . . ?
C14 C15 C21 C23A 4.4(3) . . . . ?
C16 C15 C21 C24B -3.0(8) . . . . ?
C14 C15 C21 C24B 177.9(7) . . . . ?
C16 C15 C21 C23B -121.0(6) . . . . ?
C14 C15 C21 C23B 59.8(7) . . . . ?
C16 C15 C21 C22A 67.8(3) . . . . ?
C14 C15 C21 C22A -111.4(2) . . . . ?
C2 C3 C31 C36 -131.22(18) . . . . ?
C51 C3 C31 C36 110.17(19) . . . . ?
C11 C3 C31 C36 -13.4(2) . . . . ?
C2 C3 C31 C32 51.1(2) . . . . ?
C51 C3 C31 C32 -67.5(2) . . . . ?
C11 C3 C31 C32 168.99(16) . . . . ?
C36 C31 C32 C33 0.0(3) . . . . ?
C3 C31 C32 C33 177.71(17) . . . . ?
C31 C32 C33 C34 1.2(3) . . . . ?
C31 C32 C33 C37 -179.36(18) . . . . ?
C32 C33 C34 C35 -0.8(3) . . . . ?
C37 C33 C34 C35 179.74(18) . . . . ?
C33 C34 C35 C36 -0.8(3) . . . . ?
C33 C34 C35 C41 179.15(18) . . . . ?
C32 C31 C36 C35 -1.6(3) . . . . ?
C3 C31 C36 C35 -179.23(17) . . . . ?
C34 C35 C36 C31 2.0(3) . . . . ?
C41 C35 C36 C31 -177.93(17) . . . . ?
C32 C33 C37 C39 2.7(3) . . . . ?
C34 C33 C37 C39 -177.9(2) . . . . ?
C32 C33 C37 C40 -118.0(2) . . . . ?
C34 C33 C37 C40 61.5(2) . . . . ?
C32 C33 C37 C38 122.4(2) . . . . ?
C34 C33 C37 C38 -58.2(2) . . . . ?
C34 C35 C41 C44B 173.1(6) . . . . ?
C36 C35 C41 C44B -7.0(6) . . . . ?
C34 C35 C41 C42A -5.6(3) . . . . ?
C36 C35 C41 C42A 174.3(2) . . . . ?
C34 C35 C41 C44A 119.0(2) . . . . ?
C36 C35 C41 C44A -61.1(3) . . . . ?
C34 C35 C41 C43B -52.6(6) . . . . ?
C36 C35 C41 C43B 127.3(6) . . . . ?
C34 C35 C41 C43A -126.2(2) . . . . ?
C36 C35 C41 C43A 53.7(2) . . . . ?
C34 C35 C41 C42B 52.0(5) . . . . ?
C36 C35 C41 C42B -128.1(5) . . . . ?
C2 C3 C51 C52 -141.35(17) . . . . ?
C11 C3 C51 C52 100.77(19) . . . . ?
C31 C3 C51 C52 -23.2(2) . . . . ?
C2 C3 C51 C56 42.5(2) . . . . ?
C11 C3 C51 C56 -75.4(2) . . . . ?
C31 C3 C51 C56 160.63(16) . . . . ?
C56 C51 C52 C53 0.4(3) . . . . ?
C3 C51 C52 C53 -175.83(17) . . . . ?
C51 C52 C53 C54 -0.1(3) . . . . ?
C51 C52 C53 C57 -178.21(18) . . . . ?
C52 C53 C54 C55 -0.4(3) . . . . ?
C57 C53 C54 C55 177.65(19) . . . . ?
C53 C54 C55 C56 0.6(3) . . . . ?
C53 C54 C55 C61 179.36(19) . . . . ?
C54 C55 C56 C51 -0.3(3) . . . . ?
C61 C55 C56 C51 -179.06(18) . . . . ?
C52 C51 C56 C55 -0.1(3) . . . . ?
C3 C51 C56 C55 176.11(17) . . . . ?
C54 C53 C57 C58 -110.1(2) . . . . ?
C52 C53 C57 C58 67.9(3) . . . . ?
C54 C53 C57 C60 9.9(3) . . . . ?
C52 C53 C57 C60 -172.1(2) . . . . ?
C54 C53 C57 C59 130.0(2) . . . . ?
C52 C53 C57 C59 -51.9(2) . . . . ?
C56 C55 C61 C62B -154.3(8) . . . . ?
C54 C55 C61 C62B 27.0(8) . . . . ?
C56 C55 C61 C63B 79.2(5) . . . . ?
C54 C55 C61 C63B -99.5(5) . . . . ?
C56 C55 C61 C64A 0.1(6) . . . . ?
C54 C55 C61 C64A -178.6(5) . . . . ?
C56 C55 C61 C62A -123.9(5) . . . . ?
C54 C55 C61 C62A 57.4(5) . . . . ?
C56 C55 C61 C64B -35.3(6) . . . . ?
C54 C55 C61 C64B 145.9(5) . . . . ?
C56 C55 C61 C63A 119.6(3) . . . . ?
C54 C55 C61 C63A -59.1(4) . . . . ?

_refine_diff_density_max         0.431
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.035



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2'
####################################################################### 
# 
# 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_Tr-H2
_database_code_depnum_ccdc_archive 'CCDC 1507658'
_audit_update_record             
;
2016-09-30 deposited with the CCDC.
2016-11-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7

_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
5,5,5-tris(3,5-di-t-butylphenyl)penta-1,3-diyne
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C47 H64'
_chemical_formula_sum            'C47 H64'
_chemical_formula_weight         628.98

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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   10.3367(13)
_cell_length_b                   10.4631(13)
_cell_length_c                   19.275(2)
_cell_angle_alpha                88.5549(18)
_cell_angle_beta                 78.0127(18)
_cell_angle_gamma                88.5903(19)
_cell_volume                     2038.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    4128
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      27.43

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_F_000             692
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.620
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.260
_exptl_absorpt_coefficient_mu    0.057
_shelx_estimated_absorpt_T_min   0.966
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.9105
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17675
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.947
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_full        26.400
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             9200
_reflns_number_gt                7037
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0725P)²+0.5109P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9200
_refine_ls_number_parameters     451
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1467
_refine_ls_wR_factor_gt          0.1344
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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 0.3405(2) 0.35690(19) 0.46134(10) 0.0589(5) Uani 1 1 d . . . . .
H1 H 0.3732 0.3934 0.4957 0.071 Uiso 1 1 calc R U . . .
C2 C 0.29767(16) 0.30902(15) 0.41636(8) 0.0417(3) Uani 1 1 d . . . . .
C3 C 0.24643(14) 0.24957(13) 0.36535(7) 0.0348(3) Uani 1 1 d . . . . .
C4 C 0.20225(13) 0.19284(13) 0.32244(7) 0.0312(3) Uani 1 1 d . . . . .
C5 C 0.14564(12) 0.11594(12) 0.27300(7) 0.0284(3) Uani 1 1 d . . . . .
C11 C 0.17579(12) -0.02617(12) 0.28863(7) 0.0278(3) Uani 1 1 d . . . . .
C12 C 0.21578(13) -0.11269(13) 0.23500(7) 0.0311(3) Uani 1 1 d . . . . .
H12 H 0.2273 -0.0841 0.1870 0.037 Uiso 1 1 calc R U . . .
C13 C 0.23960(13) -0.24176(13) 0.25016(7) 0.0322(3) Uani 1 1 d . . . . .
C14 C 0.22332(14) -0.28041(13) 0.32073(7) 0.0330(3) Uani 1 1 d . . . . .
H14 H 0.2406 -0.3674 0.3317 0.040 Uiso 1 1 calc R U . . .
C15 C 0.18234(13) -0.19561(12) 0.37645(7) 0.0294(3) Uani 1 1 d . . . . .
C16 C 0.15865(13) -0.06912(12) 0.35922(7) 0.0293(3) Uani 1 1 d . . . . .
H16 H 0.1301 -0.0101 0.3962 0.035 Uiso 1 1 calc R U . . .
C17 C 0.28647(16) -0.33417(14) 0.18900(8) 0.0410(3) Uani 1 1 d . . . . .
C18 C 0.42805(17) -0.29898(18) 0.15214(9) 0.0520(4) Uani 1 1 d . . . . .
H18A H 0.4861 -0.3065 0.1864 0.062 Uiso 1 1 calc R U . . .
H18B H 0.4600 -0.3571 0.1129 0.062 Uiso 1 1 calc R U . . .
H18C H 0.4284 -0.2109 0.1336 0.062 Uiso 1 1 calc R U . . .
C19 C 0.1944(2) -0.32292(19) 0.13624(9) 0.0560(5) Uani 1 1 d . . . . .
H19A H 0.2249 -0.3821 0.0974 0.067 Uiso 1 1 calc R U . . .
H19B H 0.1043 -0.3442 0.1605 0.067 Uiso 1 1 calc R U . . .
H19C H 0.1952 -0.2352 0.1171 0.067 Uiso 1 1 calc R U . . .
C20 C 0.2886(2) -0.47409(16) 0.21474(10) 0.0626(5) Uani 1 1 d . . . . .
H20A H 0.3470 -0.4836 0.2487 0.075 Uiso 1 1 calc R U . . .
H20B H 0.1989 -0.4989 0.2378 0.075 Uiso 1 1 calc R U . . .
H20C H 0.3212 -0.5291 0.1741 0.075 Uiso 1 1 calc R U . . .
C21 C 0.16785(14) -0.24480(13) 0.45350(7) 0.0349(3) Uani 1 1 d . . . . .
C22 C 0.07834(18) -0.36069(17) 0.46591(9) 0.0498(4) Uani 1 1 d . . . . .
H22A H 0.1152 -0.4271 0.4321 0.060 Uiso 1 1 calc R U . . .
H22B H 0.0726 -0.3941 0.5144 0.060 Uiso 1 1 calc R U . . .
H22C H -0.0102 -0.3352 0.4593 0.060 Uiso 1 1 calc R U . . .
C23 C 0.30516(18) -0.28354(19) 0.46658(10) 0.0548(4) Uani 1 1 d . . . . .
H23A H 0.3456 -0.3480 0.4323 0.066 Uiso 1 1 calc R U . . .
H23B H 0.3612 -0.2082 0.4610 0.066 Uiso 1 1 calc R U . . .
H23C H 0.2963 -0.3191 0.5148 0.066 Uiso 1 1 calc R U . . .
C24 C 0.1067(2) -0.14482(18) 0.50712(8) 0.0586(5) Uani 1 1 d . . . . .
H24A H 0.1620 -0.0689 0.5005 0.070 Uiso 1 1 calc R U . . .
H24B H 0.0179 -0.1211 0.5001 0.070 Uiso 1 1 calc R U . . .
H24C H 0.1007 -0.1800 0.5553 0.070 Uiso 1 1 calc R U . . .
C31 C -0.00529(12) 0.14489(12) 0.28876(6) 0.0279(3) Uani 1 1 d . . . . .
C32 C -0.09797(13) 0.04932(12) 0.30301(7) 0.0299(3) Uani 1 1 d . . . . .
H32 H -0.0690 -0.0376 0.3019 0.036 Uiso 1 1 calc R U . . .
C33 C -0.23367(13) 0.07858(13) 0.31897(7) 0.0315(3) Uani 1 1 d . . . . .
C34 C -0.27317(13) 0.20650(13) 0.31912(7) 0.0312(3) Uani 1 1 d . . . . .
H34 H -0.3650 0.2276 0.3305 0.037 Uiso 1 1 calc R U . . .
C35 C -0.18237(13) 0.30527(12) 0.30311(7) 0.0304(3) Uani 1 1 d . . . . .
C36 C -0.04850(13) 0.27195(13) 0.28869(7) 0.0317(3) Uani 1 1 d . . . . .
H36 H 0.0150 0.3375 0.2785 0.038 Uiso 1 1 calc R U . . .
C37 C -0.33214(14) -0.03117(14) 0.33701(9) 0.0418(4) Uani 1 1 d . . . . .
C38 C -0.31047(18) -0.10265(18) 0.40388(11) 0.0577(5) Uani 1 1 d . . . . .
H38A H -0.2184 -0.1332 0.3969 0.069 Uiso 1 1 calc R U . . .
H38B H -0.3296 -0.0449 0.4441 0.069 Uiso 1 1 calc R U . . .
H38C H -0.3695 -0.1757 0.4135 0.069 Uiso 1 1 calc R U . . .
C39 C -0.3077(2) -0.12588(17) 0.27528(12) 0.0607(5) Uani 1 1 d . . . . .
H39A H -0.2158 -0.1573 0.2668 0.073 Uiso 1 1 calc R U . . .
H39B H -0.3674 -0.1981 0.2875 0.073 Uiso 1 1 calc R U . . .
H39C H -0.3246 -0.0824 0.2323 0.073 Uiso 1 1 calc R U . . .
C40 C -0.47582(16) 0.01572(18) 0.34874(12) 0.0598(5) Uani 1 1 d . . . . .
H40A H -0.4907 0.0617 0.3061 0.072 Uiso 1 1 calc R U . . .
H40B H -0.5345 -0.0576 0.3585 0.072 Uiso 1 1 calc R U . . .
H40C H -0.4946 0.0732 0.3891 0.072 Uiso 1 1 calc R U . . .
C41 C -0.22426(14) 0.44678(13) 0.29942(8) 0.0361(3) Uani 1 1 d . . . . .
C42 C -0.1885(2) 0.49383(16) 0.22202(9) 0.0547(4) Uani 1 1 d . . . . .
H42A H -0.0934 0.4807 0.2038 0.066 Uiso 1 1 calc R U . . .
H42B H -0.2381 0.4458 0.1935 0.066 Uiso 1 1 calc R U . . .
H42C H -0.2110 0.5851 0.2193 0.066 Uiso 1 1 calc R U . . .
C43 C -0.1515(2) 0.52681(16) 0.34399(10) 0.0547(4) Uani 1 1 d . . . . .
H43A H -0.0559 0.5149 0.3274 0.066 Uiso 1 1 calc R U . . .
H43B H -0.1755 0.6173 0.3392 0.066 Uiso 1 1 calc R U . . .
H43C H -0.1766 0.4995 0.3939 0.066 Uiso 1 1 calc R U . . .
C44 C -0.37265(18) 0.46809(17) 0.32691(13) 0.0649(6) Uani 1 1 d . . . . .
H44A H -0.4217 0.4177 0.2992 0.078 Uiso 1 1 calc R U . . .
H44B H -0.3962 0.4412 0.3769 0.078 Uiso 1 1 calc R U . . .
H44C H -0.3951 0.5590 0.3222 0.078 Uiso 1 1 calc R U . . .
C51 C 0.21183(13) 0.15633(12) 0.19610(7) 0.0290(3) Uani 1 1 d . . . . .
C52 C 0.34919(13) 0.16594(13) 0.17917(7) 0.0310(3) Uani 1 1 d . . . . .
H52 H 0.3986 0.1489 0.2149 0.037 Uiso 1 1 calc R U . . .
C53 C 0.41499(13) 0.19990(13) 0.11127(7) 0.0309(3) Uani 1 1 d . . . . .
C54 C 0.33910(13) 0.22593(13) 0.06012(7) 0.0319(3) Uani 1 1 d . . . . .
H54 H 0.3829 0.2504 0.0135 0.038 Uiso 1 1 calc R U . . .
C55 C 0.20262(13) 0.21740(13) 0.07475(7) 0.0304(3) Uani 1 1 d . . . . .
C56 C 0.13977(13) 0.18056(12) 0.14398(7) 0.0302(3) Uani 1 1 d . . . . .
H56 H 0.0464 0.1722 0.1552 0.036 Uiso 1 1 calc R U . . .
C57 C 0.56580(13) 0.21209(15) 0.09071(7) 0.0365(3) Uani 1 1 d . . . . .
C58 C 0.62036(16) 0.12065(18) 0.03036(10) 0.0513(4) Uani 1 1 d . . . . .
H58A H 0.5789 0.1408 -0.0100 0.062 Uiso 1 1 calc R U . . .
H58B H 0.7163 0.1302 0.0158 0.062 Uiso 1 1 calc R U . . .
H58C H 0.6008 0.0324 0.0467 0.062 Uiso 1 1 calc R U . . .
C59 C 0.63192(16) 0.1787(2) 0.15291(10) 0.0616(5) Uani 1 1 d . . . . .
H59A H 0.6110 0.0907 0.1693 0.074 Uiso 1 1 calc R U . . .
H59B H 0.7280 0.1865 0.1376 0.074 Uiso 1 1 calc R U . . .
H59C H 0.5992 0.2373 0.1918 0.074 Uiso 1 1 calc R U . . .
C60 C 0.60009(16) 0.34955(17) 0.06646(10) 0.0487(4) Uani 1 1 d . . . . .
H60A H 0.5585 0.3728 0.0265 0.058 Uiso 1 1 calc R U . . .
H60B H 0.5675 0.4074 0.1057 0.058 Uiso 1 1 calc R U . . .
H60C H 0.6963 0.3566 0.0516 0.058 Uiso 1 1 calc R U . . .
C61 C 0.12323(15) 0.25025(15) 0.01747(8) 0.0403(3) Uani 1 1 d . . . . .
C62A C 0.1771(3) 0.1737(4) -0.05097(17) 0.0571(9) Uani 0.55 1 d . . P A 1
H62A H 0.2737 0.1796 -0.0635 0.068 Uiso 0.55 1 calc R U P A 1
H62B H 0.1527 0.0839 -0.0426 0.068 Uiso 0.55 1 calc R U P A 1
H62C H 0.1390 0.2095 -0.0899 0.068 Uiso 0.55 1 calc R U P A 1
C63A C -0.0183(3) 0.2456(4) 0.03882(17) 0.0506(8) Uani 0.55 1 d . . P A 1
H63A H -0.0583 0.2681 -0.0018 0.061 Uiso 0.55 1 calc R U P A 1
H63B H -0.0440 0.1590 0.0560 0.061 Uiso 0.55 1 calc R U P A 1
H63C H -0.0490 0.3064 0.0769 0.061 Uiso 0.55 1 calc R U P A 1
C64A C 0.1611(4) 0.3959(3) -0.0089(2) 0.0571(8) Uani 0.55 1 d . . P A 1
H64A H 0.2574 0.4020 -0.0238 0.069 Uiso 0.55 1 calc R U P A 1
H64B H 0.1197 0.4192 -0.0489 0.069 Uiso 0.55 1 calc R U P A 1
H64C H 0.1291 0.4544 0.0302 0.069 Uiso 0.55 1 calc R U P A 1
C62B C 0.0446(4) 0.1216(4) 0.0103(2) 0.0539(9) Uani 0.45 1 d . . P A 2
H62D H -0.0051 0.0947 0.0571 0.065 Uiso 0.45 1 calc R U P A 2
H62E H -0.0167 0.1382 -0.0216 0.065 Uiso 0.45 1 calc R U P A 2
H62F H 0.1080 0.0538 -0.0091 0.065 Uiso 0.45 1 calc R U P A 2
C63B C 0.0112(4) 0.3468(4) 0.0490(2) 0.0509(9) Uani 0.45 1 d . . P A 2
H63D H -0.0366 0.3143 0.0951 0.061 Uiso 0.45 1 calc R U P A 2
H63E H 0.0497 0.4294 0.0552 0.061 Uiso 0.45 1 calc R U P A 2
H63F H -0.0502 0.3577 0.0167 0.061 Uiso 0.45 1 calc R U P A 2
C64B C 0.1965(4) 0.2919(6) -0.0496(2) 0.0640(13) Uani 0.45 1 d . . P A 2
H64D H 0.1360 0.3100 -0.0817 0.077 Uiso 0.45 1 calc R U P A 2
H64E H 0.2438 0.3697 -0.0438 0.077 Uiso 0.45 1 calc R U P A 2
H64F H 0.2603 0.2248 -0.0695 0.077 Uiso 0.45 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.180(2) . ?
C2 C3 1.377(2) . ?
C3 C4 1.200(2) . ?
C4 C5 1.480(2) . ?
C5 C11 1.5467(17) . ?
C5 C31 1.5500(17) . ?
C5 C51 1.5508(17) . ?
C11 C12 1.3821(19) . ?
C11 C16 1.3992(18) . ?
C12 C13 1.4012(19) . ?
C13 C14 1.3867(19) . ?
C13 C17 1.5350(19) . ?
C14 C15 1.4003(19) . ?
C15 C16 1.3848(18) . ?
C15 C21 1.5380(18) . ?
C17 C19 1.531(2) . ?
C17 C20 1.535(2) . ?
C17 C18 1.537(2) . ?
C21 C24 1.521(2) . ?
C21 C22 1.527(2) . ?
C21 C23 1.535(2) . ?
C31 C32 1.3845(18) . ?
C31 C36 1.3920(18) . ?
C32 C33 1.4001(18) . ?
C33 C34 1.3896(19) . ?
C33 C37 1.5382(19) . ?
C34 C35 1.3984(19) . ?
C35 C36 1.3911(18) . ?
C35 C41 1.5364(18) . ?
C37 C40 1.526(2) . ?
C37 C38 1.528(2) . ?
C37 C39 1.544(3) . ?
C41 C44 1.528(2) . ?
C41 C43 1.530(2) . ?
C41 C42 1.532(2) . ?
C51 C56 1.3846(19) . ?
C51 C52 1.3949(18) . ?
C52 C53 1.3858(18) . ?
C53 C54 1.3997(19) . ?
C53 C57 1.5343(18) . ?
C54 C55 1.3847(18) . ?
C55 C56 1.4062(18) . ?
C55 C61 1.5343(19) . ?
C57 C59 1.528(2) . ?
C57 C60 1.528(2) . ?
C57 C58 1.531(2) . ?
C61 C64B 1.419(4) . ?
C61 C63A 1.437(3) . ?
C61 C63B 1.553(4) . ?
C61 C62A 1.555(4) . ?
C61 C62B 1.613(4) . ?
C61 C64A 1.625(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
C1 C2 C3 178.05(18) . . ?
C4 C3 C2 177.16(15) . . ?
C3 C4 C5 176.23(14) . . ?
C4 C5 C11 107.10(10) . . ?
C4 C5 C31 106.83(10) . . ?
C11 C5 C31 111.35(10) . . ?
C4 C5 C51 108.20(10) . . ?
C11 C5 C51 111.47(10) . . ?
C31 C5 C51 111.62(10) . . ?
C12 C11 C16 119.02(12) . . ?
C12 C11 C5 121.98(11) . . ?
C16 C11 C5 118.98(11) . . ?
C11 C12 C13 121.22(12) . . ?
C14 C13 C12 118.11(12) . . ?
C14 C13 C17 122.32(12) . . ?
C12 C13 C17 119.55(12) . . ?
C13 C14 C15 122.25(12) . . ?
C16 C15 C14 117.83(12) . . ?
C16 C15 C21 122.70(12) . . ?
C14 C15 C21 119.46(11) . . ?
C15 C16 C11 121.56(12) . . ?
C19 C17 C13 109.90(13) . . ?
C19 C17 C20 108.01(15) . . ?
C13 C17 C20 112.44(12) . . ?
C19 C17 C18 110.16(13) . . ?
C13 C17 C18 108.19(13) . . ?
C20 C17 C18 108.12(14) . . ?
C24 C21 C22 107.44(14) . . ?
C24 C21 C23 108.74(14) . . ?
C22 C21 C23 109.50(13) . . ?
C24 C21 C15 112.47(12) . . ?
C22 C21 C15 109.73(12) . . ?
C23 C21 C15 108.92(12) . . ?
C32 C31 C36 119.13(12) . . ?
C32 C31 C5 122.45(11) . . ?
C36 C31 C5 118.43(11) . . ?
C31 C32 C33 121.14(12) . . ?
C34 C33 C32 118.14(12) . . ?
C34 C33 C37 122.90(12) . . ?
C32 C33 C37 118.95(12) . . ?
C33 C34 C35 122.22(12) . . ?
C36 C35 C34 117.69(12) . . ?
C36 C35 C41 119.32(12) . . ?
C34 C35 C41 122.98(12) . . ?
C35 C36 C31 121.65(12) . . ?
C40 C37 C38 108.86(14) . . ?
C40 C37 C33 112.53(12) . . ?
C38 C37 C33 109.67(13) . . ?
C40 C37 C39 108.11(15) . . ?
C38 C37 C39 108.38(14) . . ?
C33 C37 C39 109.19(13) . . ?
C44 C41 C43 107.77(15) . . ?
C44 C41 C42 108.69(14) . . ?
C43 C41 C42 108.99(14) . . ?
C44 C41 C35 112.35(12) . . ?
C43 C41 C35 110.26(12) . . ?
C42 C41 C35 108.71(12) . . ?
C56 C51 C52 119.39(12) . . ?
C56 C51 C5 122.37(11) . . ?
C52 C51 C5 118.23(11) . . ?
C53 C52 C51 121.30(12) . . ?
C52 C53 C54 117.90(12) . . ?
C52 C53 C57 122.82(12) . . ?
C54 C53 C57 119.27(11) . . ?
C55 C54 C53 122.58(12) . . ?
C54 C55 C56 117.78(12) . . ?
C54 C55 C61 120.73(12) . . ?
C56 C55 C61 121.47(12) . . ?
C51 C56 C55 121.04(12) . . ?
C59 C57 C60 108.24(14) . . ?
C59 C57 C58 108.41(14) . . ?
C60 C57 C58 109.79(13) . . ?
C59 C57 C53 111.88(12) . . ?
C60 C57 C53 109.46(12) . . ?
C58 C57 C53 109.03(12) . . ?
C64B C61 C55 116.63(19) . . ?
C63A C61 C55 116.62(17) . . ?
C64B C61 C63B 112.3(3) . . ?
C55 C61 C63B 107.95(18) . . ?
C63A C61 C62A 112.3(2) . . ?
C55 C61 C62A 110.95(16) . . ?
C64B C61 C62B 110.9(3) . . ?
C55 C61 C62B 104.62(17) . . ?
C63B C61 C62B 103.4(2) . . ?
C63A C61 C64A 107.6(2) . . ?
C55 C61 C64A 105.96(16) . . ?
C62A C61 C64A 102.0(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 C5 C11 C12 -138.60(12) . . . . ?
C31 C5 C11 C12 104.94(14) . . . . ?
C51 C5 C11 C12 -20.42(17) . . . . ?
C4 C5 C11 C16 43.14(15) . . . . ?
C31 C5 C11 C16 -73.32(15) . . . . ?
C51 C5 C11 C16 161.32(11) . . . . ?
C16 C11 C12 C13 -0.2(2) . . . . ?
C5 C11 C12 C13 -178.44(12) . . . . ?
C11 C12 C13 C14 -0.7(2) . . . . ?
C11 C12 C13 C17 -178.83(13) . . . . ?
C12 C13 C14 C15 1.0(2) . . . . ?
C17 C13 C14 C15 179.08(13) . . . . ?
C13 C14 C15 C16 -0.4(2) . . . . ?
C13 C14 C15 C21 -179.32(13) . . . . ?
C14 C15 C16 C11 -0.50(19) . . . . ?
C21 C15 C16 C11 178.36(12) . . . . ?
C12 C11 C16 C15 0.8(2) . . . . ?
C5 C11 C16 C15 179.10(12) . . . . ?
C14 C13 C17 C19 130.45(15) . . . . ?
C12 C13 C17 C19 -51.49(18) . . . . ?
C14 C13 C17 C20 10.1(2) . . . . ?
C12 C13 C17 C20 -171.85(15) . . . . ?
C14 C13 C17 C18 -109.23(16) . . . . ?
C12 C13 C17 C18 68.82(17) . . . . ?
C16 C15 C21 C24 8.2(2) . . . . ?
C14 C15 C21 C24 -172.96(14) . . . . ?
C16 C15 C21 C22 127.73(15) . . . . ?
C14 C15 C21 C22 -53.43(17) . . . . ?
C16 C15 C21 C23 -112.42(15) . . . . ?
C14 C15 C21 C23 66.42(17) . . . . ?
C4 C5 C31 C32 -126.85(13) . . . . ?
C11 C5 C31 C32 -10.23(17) . . . . ?
C51 C5 C31 C32 115.05(13) . . . . ?
C4 C5 C31 C36 52.97(15) . . . . ?
C11 C5 C31 C36 169.59(11) . . . . ?
C51 C5 C31 C36 -65.13(15) . . . . ?
C36 C31 C32 C33 -1.58(19) . . . . ?
C5 C31 C32 C33 178.24(12) . . . . ?
C31 C32 C33 C34 0.9(2) . . . . ?
C31 C32 C33 C37 -177.82(13) . . . . ?
C32 C33 C34 C35 0.8(2) . . . . ?
C37 C33 C34 C35 179.52(13) . . . . ?
C33 C34 C35 C36 -1.8(2) . . . . ?
C33 C34 C35 C41 176.91(13) . . . . ?
C34 C35 C36 C31 1.2(2) . . . . ?
C41 C35 C36 C31 -177.63(12) . . . . ?
C32 C31 C36 C35 0.5(2) . . . . ?
C5 C31 C36 C35 -179.32(12) . . . . ?
C34 C33 C37 C40 4.7(2) . . . . ?
C32 C33 C37 C40 -176.58(15) . . . . ?
C34 C33 C37 C38 -116.60(16) . . . . ?
C32 C33 C37 C38 62.09(18) . . . . ?
C34 C33 C37 C39 124.78(15) . . . . ?
C32 C33 C37 C39 -56.53(17) . . . . ?
C36 C35 C41 C44 -171.77(15) . . . . ?
C34 C35 C41 C44 9.5(2) . . . . ?
C36 C35 C41 C43 -51.54(18) . . . . ?
C34 C35 C41 C43 129.74(15) . . . . ?
C36 C35 C41 C42 67.89(17) . . . . ?
C34 C35 C41 C42 -110.84(16) . . . . ?
C4 C5 C51 C56 -133.95(13) . . . . ?
C11 C5 C51 C56 108.54(14) . . . . ?
C31 C5 C51 C56 -16.67(17) . . . . ?
C4 C5 C51 C52 47.27(15) . . . . ?
C11 C5 C51 C52 -70.25(15) . . . . ?
C31 C5 C51 C52 164.54(12) . . . . ?
C56 C51 C52 C53 0.3(2) . . . . ?
C5 C51 C52 C53 179.15(12) . . . . ?
C51 C52 C53 C54 0.8(2) . . . . ?
C51 C52 C53 C57 179.70(13) . . . . ?
C52 C53 C54 C55 -0.8(2) . . . . ?
C57 C53 C54 C55 -179.79(13) . . . . ?
C53 C54 C55 C56 -0.2(2) . . . . ?
C53 C54 C55 C61 178.39(13) . . . . ?
C52 C51 C56 C55 -1.4(2) . . . . ?
C5 C51 C56 C55 179.81(12) . . . . ?
C54 C55 C56 C51 1.4(2) . . . . ?
C61 C55 C56 C51 -177.25(13) . . . . ?
C52 C53 C57 C59 1.7(2) . . . . ?
C54 C53 C57 C59 -179.37(15) . . . . ?
C52 C53 C57 C60 -118.27(15) . . . . ?
C54 C53 C57 C60 60.66(17) . . . . ?
C52 C53 C57 C58 121.61(15) . . . . ?
C54 C53 C57 C58 -59.46(17) . . . . ?
C54 C55 C61 C64B -1.4(3) . . . . ?
C56 C55 C61 C64B 177.2(3) . . . . ?
C54 C55 C61 C63A -176.5(2) . . . . ?
C56 C55 C61 C63A 2.0(3) . . . . ?
C54 C55 C61 C63B -128.9(2) . . . . ?
C56 C55 C61 C63B 49.7(2) . . . . ?
C54 C55 C61 C62A 53.1(2) . . . . ?
C56 C55 C61 C62A -128.3(2) . . . . ?
C54 C55 C61 C62B 121.5(2) . . . . ?
C56 C55 C61 C62B -59.9(2) . . . . ?
C54 C55 C61 C64A -56.8(2) . . . . ?
C56 C55 C61 C64A 121.8(2) . . . . ?

_refine_diff_density_max         0.330
_refine_diff_density_min         -0.140
_refine_diff_density_rms         0.044


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CHCl3'
####################################################################### 
# 
# 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_Tr-H3
_database_code_depnum_ccdc_archive 'CCDC 1507659'
_audit_update_record             
;
2016-11-02 deposited with the CCDC.
2016-11-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7

_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
1,1,1-tris(3,5-di-t-butylphenyl)hepta-2,4,6-triyne
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C49 H64'
_chemical_formula_sum            'C49 H64'
_chemical_formula_weight         653.00

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      trigonal
_space_group_IT_number           159
_space_group_name_H-M_alt        'P 3 1 c'
_space_group_name_Hall           'P 3 -2c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'

_cell_length_a                   14.154(3)
_cell_length_b                   14.154(3)
_cell_length_c                   12.123(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2103.4(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2337
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      20.58

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.031
_exptl_crystal_F_000             716
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.046
_exptl_absorpt_coefficient_mu    0.057
_shelx_estimated_absorpt_T_min   0.974
_shelx_estimated_absorpt_T_max   0.997
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.9173
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15255
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.661
_diffrn_reflns_theta_max         25.716
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2685
_reflns_number_gt                1988
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.989
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0327P)²+0.3159P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 836 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.0(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2685
_refine_ls_number_parameters     148
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0411
_refine_ls_wR_factor_ref         0.0882
_refine_ls_wR_factor_gt          0.0776
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.034
_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 0.3333 0.6667 0.7765(6) 0.074(3) Uani 1 3 d S T P . .
H1 H 0.3333 0.6667 0.8548 0.089 Uiso 1 3 calc R U P . .
C2 C 0.3333 0.6667 0.6794(5) 0.0493(18) Uani 1 3 d S T P . .
C3 C 0.3333 0.6667 0.5666(5) 0.0355(14) Uani 1 3 d S T P . .
C4 C 0.3333 0.6667 0.4682(5) 0.0315(14) Uani 1 3 d S T P . .
C5 C 0.3333 0.6667 0.3547(5) 0.0235(12) Uani 1 3 d S T P . .
C6 C 0.3333 0.6667 0.2558(4) 0.0222(12) Uani 1 3 d S T P . .
C7 C 0.3333 0.6667 0.1338(4) 0.0196(11) Uani 1 3 d S T P . .
C11 C 0.2890(2) 0.5477(2) 0.0951(2) 0.0189(6) Uani 1 1 d . . . . .
C12 C 0.1903(2) 0.4669(2) 0.1368(2) 0.0205(7) Uani 1 1 d . . . . .
H12 H 0.1544 0.4856 0.1915 0.025 Uiso 1 1 calc R U . . .
C13 C 0.1420(2) 0.3592(2) 0.1011(2) 0.0212(7) Uani 1 1 d . . . . .
C14 C 0.1984(2) 0.3344(2) 0.0229(2) 0.0228(7) Uani 1 1 d . . . . .
H14 H 0.1674 0.2612 -0.0021 0.027 Uiso 1 1 calc R U . . .
C15 C 0.2986(2) 0.4128(2) -0.0199(2) 0.0222(7) Uani 1 1 d . . . . .
C16 C 0.3426(2) 0.5200(2) 0.0164(2) 0.0204(7) Uani 1 1 d . . . . .
H16 H 0.4102 0.5750 -0.0130 0.024 Uiso 1 1 calc R U . . .
C17 C 0.0293(2) 0.2756(3) 0.1454(2) 0.0251(7) Uani 1 1 d . . . . .
C18 C -0.0536(3) 0.3095(3) 0.1088(3) 0.0344(9) Uani 1 1 d . . . . .
H18A H -0.0301 0.3834 0.1353 0.041 Uiso 1 1 calc R U . . .
H18B H -0.0581 0.3080 0.0281 0.041 Uiso 1 1 calc R U . . .
H18C H -0.1254 0.2586 0.1397 0.041 Uiso 1 1 calc R U . . .
C19 C 0.0319(3) 0.2743(3) 0.2721(3) 0.0382(9) Uani 1 1 d . . . . .
H19A H 0.0566 0.3479 0.3003 0.046 Uiso 1 1 calc R U . . .
H19B H -0.0414 0.2241 0.3003 0.046 Uiso 1 1 calc R U . . .
H19C H 0.0823 0.2499 0.2966 0.046 Uiso 1 1 calc R U . . .
C20 C -0.0092(3) 0.1605(3) 0.1031(3) 0.0378(9) Uani 1 1 d . . . . .
H20A H -0.0814 0.1103 0.1337 0.045 Uiso 1 1 calc R U . . .
H20B H -0.0135 0.1598 0.0224 0.045 Uiso 1 1 calc R U . . .
H20C H 0.0425 0.1374 0.1261 0.045 Uiso 1 1 calc R U . . .
C21 C 0.3588(2) 0.3796(3) -0.1030(3) 0.0259(7) Uani 1 1 d . . . . .
C22 C 0.4648(3) 0.4764(3) -0.1439(3) 0.0539(12) Uani 1 1 d . . . . .
H22A H 0.5131 0.5127 -0.0810 0.065 Uiso 1 1 calc R U . . .
H22B H 0.5007 0.4508 -0.1952 0.065 Uiso 1 1 calc R U . . .
H22C H 0.4489 0.5280 -0.1818 0.065 Uiso 1 1 calc R U . . .
C23 C 0.3864(3) 0.2992(3) -0.0479(3) 0.0425(9) Uani 1 1 d . . . . .
H23A H 0.3193 0.2360 -0.0209 0.051 Uiso 1 1 calc R U . . .
H23B H 0.4215 0.2749 -0.1017 0.051 Uiso 1 1 calc R U . . .
H23C H 0.4361 0.3350 0.0141 0.051 Uiso 1 1 calc R U . . .
C24 C 0.2857(3) 0.3250(4) -0.2028(3) 0.0479(10) Uani 1 1 d . . . . .
H24A H 0.2169 0.2623 -0.1782 0.057 Uiso 1 1 calc R U . . .
H24B H 0.2708 0.3775 -0.2403 0.057 Uiso 1 1 calc R U . . .
H24C H 0.3225 0.3002 -0.2538 0.057 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.177(9) . ?
C2 C3 1.368(9) . ?
C3 C4 1.192(8) . ?
C4 C5 1.377(8) . ?
C5 C6 1.199(7) . ?
C6 C7 1.478(7) . ?
C7 C11 1.547(3) 3_565 ?
C7 C11 1.547(3) . ?
C7 C11 1.547(3) 2_665 ?
C11 C12 1.384(4) . ?
C11 C16 1.393(4) . ?
C12 C13 1.393(4) . ?
C13 C14 1.393(4) . ?
C13 C17 1.531(4) . ?
C14 C15 1.392(4) . ?
C15 C16 1.392(4) . ?
C15 C21 1.539(4) . ?
C17 C20 1.525(4) . ?
C17 C19 1.537(4) . ?
C17 C18 1.538(4) . ?
C21 C22 1.522(4) . ?
C21 C24 1.527(5) . ?
C21 C23 1.529(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
C1 C2 C3 180.0 . . ?
C4 C3 C2 180.0 . . ?
C3 C4 C5 180.0 . . ?
C6 C5 C4 180.0 . . ?
C5 C6 C7 180.0 . . ?
C6 C7 C11 107.7(2) . 3_565 ?
C6 C7 C11 107.7(2) . . ?
C11 C7 C11 111.22(19) 3_565 . ?
C6 C7 C11 107.7(2) . 2_665 ?
C11 C7 C11 111.22(19) 3_565 2_665 ?
C11 C7 C11 111.22(19) . 2_665 ?
C12 C11 C16 119.0(3) . . ?
C12 C11 C7 118.7(2) . . ?
C16 C11 C7 122.2(3) . . ?
C11 C12 C13 122.1(3) . . ?
C12 C13 C14 117.3(3) . . ?
C12 C13 C17 119.2(3) . . ?
C14 C13 C17 123.5(3) . . ?
C15 C14 C13 122.4(3) . . ?
C16 C15 C14 118.3(3) . . ?
C16 C15 C21 121.7(3) . . ?
C14 C15 C21 120.0(3) . . ?
C15 C16 C11 120.9(3) . . ?
C20 C17 C13 112.7(3) . . ?
C20 C17 C19 108.7(3) . . ?
C13 C17 C19 109.7(2) . . ?
C20 C17 C18 108.4(3) . . ?
C13 C17 C18 108.7(2) . . ?
C19 C17 C18 108.6(3) . . ?
C22 C21 C24 108.1(3) . . ?
C22 C21 C23 108.0(3) . . ?
C24 C21 C23 109.3(3) . . ?
C22 C21 C15 112.7(3) . . ?
C24 C21 C15 109.5(3) . . ?
C23 C21 C15 109.2(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C7 C11 C12 52.3(2) . . . . ?
C11 C7 C11 C12 -65.4(4) 3_565 . . . ?
C11 C7 C11 C12 170.0(2) 2_665 . . . ?
C6 C7 C11 C16 -130.5(2) . . . . ?
C11 C7 C11 C16 111.8(2) 3_565 . . . ?
C11 C7 C11 C16 -12.8(4) 2_665 . . . ?
C16 C11 C12 C13 -1.1(4) . . . . ?
C7 C11 C12 C13 176.1(3) . . . . ?
C11 C12 C13 C14 1.6(4) . . . . ?
C11 C12 C13 C17 -176.1(3) . . . . ?
C12 C13 C14 C15 -0.7(4) . . . . ?
C17 C13 C14 C15 177.0(3) . . . . ?
C13 C14 C15 C16 -0.8(4) . . . . ?
C13 C14 C15 C21 177.9(3) . . . . ?
C14 C15 C16 C11 1.3(4) . . . . ?
C21 C15 C16 C11 -177.3(3) . . . . ?
C12 C11 C16 C15 -0.4(4) . . . . ?
C7 C11 C16 C15 -177.5(3) . . . . ?
C12 C13 C17 C20 -176.9(3) . . . . ?
C14 C13 C17 C20 5.6(4) . . . . ?
C12 C13 C17 C19 -55.7(4) . . . . ?
C14 C13 C17 C19 126.7(3) . . . . ?
C12 C13 C17 C18 63.0(3) . . . . ?
C14 C13 C17 C18 -114.6(3) . . . . ?
C16 C15 C21 C22 -3.4(4) . . . . ?
C14 C15 C21 C22 178.0(3) . . . . ?
C16 C15 C21 C24 -123.9(3) . . . . ?
C14 C15 C21 C24 57.6(4) . . . . ?
C16 C15 C21 C23 116.5(3) . . . . ?
C14 C15 C21 C23 -62.1(4) . . . . ?

_refine_diff_density_max         0.130
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.033



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: xylenes'
