# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
#  of the CCDC or of third parties, and may not be copied or further 
#  disseminated in any form, whether machine-readable or not,  
#  except for the purpose of generating routine backup copies 
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#  data retrieval see:
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#
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data_pere25
_database_code_depnum_ccdc_archive 'CCDC 923794'
#TrackingRef 'web_deposit_cif_file_0_FrancineBelanger-Gariepy_1360246543.15DPSAnt.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H42'
_chemical_formula_sum            'C40 H42'
_chemical_formula_weight         522.74
_chemical_compound_source        'Synthesized by the authors. See text'
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'
_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   6.7671(3)
_cell_length_b                   10.0846(5)
_cell_length_c                   12.0321(6)
_cell_angle_alpha                98.990(2)
_cell_angle_beta                 106.294(2)
_cell_angle_gamma                104.765(3)
_cell_volume                     738.80(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100
_cell_measurement_reflns_used    8175
_cell_measurement_theta_min      3.95
_cell_measurement_theta_max      70.84
_exptl_crystal_description       NEEDLE
_exptl_crystal_colour            'PALE YELLOW'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             282
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_Type   multi-scan
_exptl_absorpt_correction_T_min  0.8054
_exptl_absorpt_correction_T_max  0.9902
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2008)'
_exptl_special_details           
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker smart diffractometer equiped with an APEX II CCD Detector,
a graphite monochromator. The crystal-to-detector distance was
5.0 cm, and the data collection was carried out in 512 x 512 pixel mode.
The initial unit cell parameters were determined by a least-squares fit
of the angular setting of strong reflections, collected by a 10.0 degree
scan in 33 frames over four different parts of the reciprocal space
(132 frames total).
;
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Incoatec I\muS Microsource '
_diffrn_radiation_monochromator  'Quazar MX'
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            18692
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.95
_diffrn_reflns_theta_max         71.17
_reflns_number_total             2724
_reflns_number_gt                2241
_reflns_threshold_expression     I>2\s(I)
_computing_data_collection       'APEX2 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'UdMX (Maris, 2004)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0973P)^2^+0.5890P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2724
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.1918
_refine_ls_wR_factor_gt          0.1836
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2195(3) 0.0667(2) 0.56170(18) 0.0266(5) Uani 1 1 d . . .
H1 H 0.3700 0.1115 0.6038 0.032 Uiso 1 1 calc R . .
C2 C 0.0808(3) 0.1485(2) 0.55513(17) 0.0255(5) Uani 1 1 d . . .
C3 C 0.1544(3) 0.2994(2) 0.60838(18) 0.0272(5) Uani 1 1 d . . .
C4 C 0.0048(3) 0.3702(2) 0.59777(19) 0.0286(5) Uani 1 1 d . . .
H4 H 0.0524 0.4687 0.6336 0.034 Uiso 1 1 calc R . .
C5 C -0.2185(3) 0.3006(2) 0.53502(19) 0.0294(5) Uani 1 1 d . . .
H5 H -0.3181 0.3528 0.5295 0.035 Uiso 1 1 calc R . .
C6 C -0.2922(3) 0.1593(2) 0.48234(18) 0.0286(5) Uani 1 1 d . . .
H6 H -0.4424 0.1142 0.4394 0.034 Uiso 1 1 calc R . .
C7 C -0.1463(3) 0.0789(2) 0.49114(17) 0.0262(5) Uani 1 1 d . . .
C8 C 0.3865(3) 0.3729(2) 0.67342(18) 0.0283(5) Uani 1 1 d . . .
H8 H 0.4699 0.3214 0.7141 0.034 Uiso 1 1 calc R . .
C9 C 0.4878(3) 0.5077(2) 0.67898(19) 0.0291(5) Uani 1 1 d . . .
H9 H 0.4014 0.5597 0.6416 0.035 Uiso 1 1 calc R . .
C10 C 0.7213(3) 0.5822(2) 0.73784(18) 0.0275(5) Uani 1 1 d . . .
C11 C 0.8168(4) 0.7015(2) 0.70103(19) 0.0306(5) Uani 1 1 d . . .
H11 H 0.7287 0.7346 0.6426 0.037 Uiso 1 1 calc R . .
C12 C 1.0382(3) 0.7705(2) 0.74958(19) 0.0307(5) Uani 1 1 d . . .
H12 H 1.0992 0.8507 0.7237 0.037 Uiso 1 1 calc R . .
C13 C 1.1730(3) 0.7256(2) 0.83505(18) 0.0287(5) Uani 1 1 d . . .
C14 C 1.0776(4) 0.6090(2) 0.87315(19) 0.0307(5) Uani 1 1 d . . .
H14 H 1.1656 0.5770 0.9326 0.037 Uiso 1 1 calc R . .
C15 C 0.8557(3) 0.5394(2) 0.82512(19) 0.0301(5) Uani 1 1 d . . .
H15 H 0.7947 0.4607 0.8527 0.036 Uiso 1 1 calc R . .
C16 C 1.4152(3) 0.8020(2) 0.8817(2) 0.0323(5) Uani 1 1 d . . .
H16A H 1.4382 0.9042 0.9092 0.039 Uiso 1 1 calc R . .
H16B H 1.4707 0.7901 0.8141 0.039 Uiso 1 1 calc R . .
C17 C 1.5513(4) 0.7558(2) 0.9826(2) 0.0337(5) Uani 1 1 d . . .
H17A H 1.5347 0.6546 0.9551 0.040 Uiso 1 1 calc R . .
H17B H 1.4963 0.7659 1.0505 0.040 Uiso 1 1 calc R . .
C18 C 1.7912(3) 0.8411(2) 1.0255(2) 0.0319(5) Uani 1 1 d . . .
H18A H 1.8489 0.8263 0.9591 0.038 Uiso 1 1 calc R . .
H18B H 1.8076 0.9430 1.0485 0.038 Uiso 1 1 calc R . .
C19 C 1.9226(4) 0.8001(3) 1.1309(2) 0.0412(6) Uani 1 1 d . . .
H19A H 1.8635 0.8150 1.1967 0.049 Uiso 1 1 calc R . .
H19B H 1.9035 0.6979 1.1075 0.049 Uiso 1 1 calc R . .
C20 C 2.1611(4) 0.8801(3) 1.1771(2) 0.0408(6) Uani 1 1 d . . .
H20A H 2.2225 0.8648 1.1133 0.061 Uiso 1 1 calc R . .
H20B H 2.2336 0.8464 1.2444 0.061 Uiso 1 1 calc R . .
H20C H 2.1827 0.9813 1.2037 0.061 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0169(10) 0.0304(10) 0.0284(10) 0.0090(8) 0.0063(8) 0.0008(8)
C2 0.0185(11) 0.0289(10) 0.0272(10) 0.0094(8) 0.0081(8) 0.0023(8)
C3 0.0213(11) 0.0310(11) 0.0272(10) 0.0091(8) 0.0091(8) 0.0022(8)
C4 0.0254(12) 0.0276(10) 0.0310(11) 0.0080(8) 0.0109(8) 0.0035(8)
C5 0.0224(11) 0.0348(11) 0.0336(11) 0.0119(9) 0.0106(8) 0.0101(9)
C6 0.0177(10) 0.0348(11) 0.0311(11) 0.0109(8) 0.0074(8) 0.0038(8)
C7 0.0195(11) 0.0306(11) 0.0269(10) 0.0100(8) 0.0082(8) 0.0032(8)
C8 0.0216(11) 0.0304(10) 0.0298(10) 0.0075(8) 0.0061(8) 0.0057(8)
C9 0.0214(11) 0.0309(11) 0.0321(11) 0.0085(9) 0.0074(8) 0.0046(9)
C10 0.0224(11) 0.0265(10) 0.0302(10) 0.0056(8) 0.0088(8) 0.0027(8)
C11 0.0244(12) 0.0312(11) 0.0336(11) 0.0116(9) 0.0076(9) 0.0046(9)
C12 0.0245(12) 0.0297(11) 0.0348(11) 0.0100(9) 0.0106(9) 0.0010(9)
C13 0.0238(12) 0.0276(10) 0.0302(11) 0.0040(8) 0.0091(8) 0.0021(9)
C14 0.0247(12) 0.0303(11) 0.0321(11) 0.0095(8) 0.0053(8) 0.0036(9)
C15 0.0245(12) 0.0274(10) 0.0331(11) 0.0085(8) 0.0085(9) -0.0002(8)
C16 0.0243(12) 0.0302(11) 0.0377(12) 0.0083(9) 0.0090(9) 0.0021(9)
C17 0.0237(12) 0.0359(12) 0.0375(12) 0.0094(9) 0.0091(9) 0.0034(9)
C18 0.0238(12) 0.0323(11) 0.0353(12) 0.0078(9) 0.0091(9) 0.0026(9)
C19 0.0295(14) 0.0446(13) 0.0437(13) 0.0166(11) 0.0077(10) 0.0035(10)
C20 0.0278(13) 0.0486(14) 0.0394(13) 0.0118(11) 0.0021(10) 0.0107(11)
_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_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . . 1.393(3) y
C1 C7 . 2_556 1.402(3) y
C1 H1 . . 0.9500 ?
C2 C7 . . 1.437(3) y
C2 C3 . . 1.451(3) y
C3 C4 . . 1.369(3) y
C3 C8 . . 1.471(3) y
C4 C5 . . 1.414(3) y
C4 H4 . . 0.9500 ?
C5 C6 . . 1.363(3) y
C5 H5 . . 0.9500 ?
C6 C7 . . 1.421(3) y
C6 H6 . . 0.9500 ?
C7 C1 . 2_556 1.402(3) y
C8 C9 . . 1.339(3) y
C8 H8 . . 0.9500 ?
C9 C10 . . 1.470(3) y
C9 H9 . . 0.9500 ?
C10 C15 . . 1.386(3) y
C10 C11 . . 1.411(3) y
C11 C12 . . 1.386(3) y
C11 H11 . . 0.9500 ?
C12 C13 . . 1.388(3) y
C12 H12 . . 0.9500 ?
C13 C14 . . 1.399(3) y
C13 C16 . . 1.517(3) y
C14 C15 . . 1.389(3) y
C14 H14 . . 0.9500 ?
C15 H15 . . 0.9500 ?
C16 C17 . . 1.519(3) y
C16 H16a . . 0.9900 ?
C16 H16b . . 0.9900 ?
C17 C18 . . 1.524(3) y
C17 H17a . . 0.9900 ?
C17 H17b . . 0.9900 ?
C18 C19 . . 1.513(3) y
C18 H18a . . 0.9900 ?
C18 H18b . . 0.9900 ?
C19 C20 . . 1.502(3) y
C19 H19a . . 0.9900 ?
C19 H19b . . 0.9900 ?
C20 H20a . . 0.9800 ?
C20 H20b . . 0.9800 ?
C20 H20c . . 0.9800 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C7 . . 2_556 122.77(19) y
C2 C1 H1 . . . 118.6 ?
C7 C1 H1 2_556 . . 118.6 ?
C1 C2 C7 . . . 117.80(19) y
C1 C2 C3 . . . 123.40(19) y
C7 C2 C3 . . . 118.80(19) y
C4 C3 C2 . . . 118.93(19) y
C4 C3 C8 . . . 121.42(19) y
C2 C3 C8 . . . 119.65(19) y
C3 C4 C5 . . . 121.8(2) y
C3 C4 H4 . . . 119.1 ?
C5 C4 H4 . . . 119.1 ?
C6 C5 C4 . . . 120.6(2) y
C6 C5 H5 . . . 119.7 ?
C4 C5 H5 . . . 119.7 ?
C5 C6 C7 . . . 120.5(2) y
C5 C6 H6 . . . 119.7 ?
C7 C6 H6 . . . 119.7 ?
C1 C7 C6 2_556 . . 121.32(19) y
C1 C7 C2 2_556 . . 119.43(19) y
C6 C7 C2 . . . 119.25(19) y
C9 C8 C3 . . . 124.3(2) y
C9 C8 H8 . . . 117.9 ?
C3 C8 H8 . . . 117.9 ?
C8 C9 C10 . . . 125.7(2) y
C8 C9 H9 . . . 117.1 ?
C10 C9 H9 . . . 117.1 ?
C15 C10 C11 . . . 117.7(2) y
C15 C10 C9 . . . 123.81(19) y
C11 C10 C9 . . . 118.5(2) y
C12 C11 C10 . . . 120.5(2) y
C12 C11 H11 . . . 119.8 ?
C10 C11 H11 . . . 119.8 ?
C11 C12 C13 . . . 121.7(2) y
C11 C12 H12 . . . 119.1 ?
C13 C12 H12 . . . 119.1 ?
C12 C13 C14 . . . 117.7(2) y
C12 C13 C16 . . . 119.40(19) y
C14 C13 C16 . . . 122.8(2) y
C15 C14 C13 . . . 120.9(2) y
C15 C14 H14 . . . 119.6 ?
C13 C14 H14 . . . 119.6 ?
C10 C15 C14 . . . 121.5(2) y
C10 C15 H15 . . . 119.3 ?
C14 C15 H15 . . . 119.3 ?
C13 C16 C17 . . . 116.76(19) y
C13 C16 H16A . . . 108.1 ?
C17 C16 H16A . . . 108.1 ?
C13 C16 H16B . . . 108.1 ?
C17 C16 H16B . . . 108.1 ?
H16A C16 H16B . . . 107.3 ?
C16 C17 C18 . . . 112.92(19) y
C16 C17 H17A . . . 109.0 ?
C18 C17 H17A . . . 109.0 ?
C16 C17 H17B . . . 109.0 ?
C18 C17 H17B . . . 109.0 ?
H17A C17 H17B . . . 107.8 ?
C19 C18 C17 . . . 112.33(19) y
C19 C18 H18A . . . 109.1 ?
C17 C18 H18A . . . 109.1 ?
C19 C18 H18B . . . 109.1 ?
C17 C18 H18B . . . 109.1 ?
H18A C18 H18B . . . 107.9 ?
C20 C19 C18 . . . 114.9(2) y
C20 C19 H19A . . . 108.5 ?
C18 C19 H19A . . . 108.5 ?
C20 C19 H19B . . . 108.5 ?
C18 C19 H19B . . . 108.5 ?
H19A C19 H19B . . . 107.5 ?
C19 C20 H20A . . . 109.5 ?
C19 C20 H20B . . . 109.5 ?
H20A C20 H20B . . . 109.5 ?
C19 C20 H20C . . . 109.5 ?
H20A C20 H20C . . . 109.5 ?
H20B C20 H20C . . . 109.5 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C7 C1 C2 C7 2_556 . . . 0.0(3) y
C7 C1 C2 C3 2_556 . . . -179.40(18) y
C1 C2 C3 C4 . . . . -179.46(19) y
C7 C2 C3 C4 . . . . 1.1(3) y
C1 C2 C3 C8 . . . . -0.1(3) y
C7 C2 C3 C8 . . . . -179.51(18) y
C2 C3 C4 C5 . . . . -0.9(3) y
C8 C3 C4 C5 . . . . 179.75(19) y
C3 C4 C5 C6 . . . . -0.2(3) y
C4 C5 C6 C7 . . . . 1.0(3) y
C5 C6 C7 C1 . . . 2_556 179.52(19) y
C5 C6 C7 C2 . . . . -0.7(3) y
C1 C2 C7 C1 . . . 2_556 0.0(3) y
C3 C2 C7 C1 . . . 2_556 179.42(18) y
C1 C2 C7 C6 . . . . -179.77(18) y
C3 C2 C7 C6 . . . . -0.3(3) y
C4 C3 C8 C9 . . . . -32.2(3) y
C2 C3 C8 C9 . . . . 148.4(2) y
C3 C8 C9 C10 . . . . -176.65(19) y
C8 C9 C10 C15 . . . . -20.6(3) y
C8 C9 C10 C11 . . . . 157.2(2) y
C15 C10 C11 C12 . . . . 1.3(3) y
C9 C10 C11 C12 . . . . -176.6(2) y
C10 C11 C12 C13 . . . . 0.1(3) y
C11 C12 C13 C14 . . . . -1.3(3) y
C11 C12 C13 C16 . . . . 177.7(2) y
C12 C13 C14 C15 . . . . 1.1(3) y
C16 C13 C14 C15 . . . . -177.9(2) y
C11 C10 C15 C14 . . . . -1.4(3) y
C9 C10 C15 C14 . . . . 176.3(2) y
C13 C14 C15 C10 . . . . 0.2(3) y
C12 C13 C16 C17 . . . . 174.9(2) y
C14 C13 C16 C17 . . . . -6.1(3) y
C13 C16 C17 C18 . . . . -178.45(18) y
C16 C17 C18 C19 . . . . 176.5(2) y
C17 C18 C19 C20 . . . . 179.7(2) y
_diffrn_measured_fraction_theta_max 0.952
_diffrn_reflns_theta_full        71.17
_diffrn_measured_fraction_theta_full 0.952
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.066
_vrf_DIFMX01_pere25              
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00
_refine_diff_density_max given = 0.646
Test value = 0.600
RESPONSE: The highest peak is between C15 and C17.
Disorder of the chain is suspected but no good model could be found.
;
_vrf_PLAT029_pere25              
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.952
RESPONSE: Missing data is due to geometric restraints of the instruments,
which are especially severe for triclinic crystals.
;
_vrf_PLAT934_pere25              
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW .gt. 10 Outliers . 2
RESPONSE: If we omit these two reflections in the final refinement,
there is no observable change.
So we keep them as part of all measured reflections for this crystal.
;
_iucr_refine_instructions_details 
;
TITL pere25 in P-1
CELL 1.54178 6.7671 10.0846 12.0321 98.990 106.294 104.765
ZERR 1.00 0.0003 0.0005 0.0006 0.002 0.002 0.003
LATT 1
SFAC C H
UNIT 40 42
SIZE 0.02 0.03 0.2
TEMP -173
ACTA
L.S. 8
BOND $H
CONF
WPDB -1
FMAP 2
PLAN -5
WGHT 0.097300 0.589000
FVAR 0.32996
C1 1 0.219492 0.066707 0.561703 11.00000 0.01689 0.03040 =
0.02845 0.00901 0.00632 0.00083
AFIX 43
H1 2 0.370024 0.111468 0.603763 11.00000 -1.20000
AFIX 0
C2 1 0.080819 0.148466 0.555130 11.00000 0.01846 0.02886 =
0.02718 0.00941 0.00814 0.00229
C3 1 0.154436 0.299449 0.608385 11.00000 0.02126 0.03098 =
0.02723 0.00906 0.00911 0.00219
C4 1 0.004840 0.370172 0.597771 11.00000 0.02541 0.02763 =
0.03104 0.00801 0.01087 0.00351
AFIX 43
H4 2 0.052369 0.468741 0.633557 11.00000 -1.20000
AFIX 0
C5 1 -0.218487 0.300607 0.535024 11.00000 0.02243 0.03479 =
0.03359 0.01187 0.01056 0.01007
AFIX 43
H5 2 -0.318074 0.352818 0.529526 11.00000 -1.20000
AFIX 0
C6 1 -0.292221 0.159309 0.482343 11.00000 0.01765 0.03481 =
0.03107 0.01094 0.00738 0.00384
AFIX 43
H6 2 -0.442363 0.114236 0.439403 11.00000 -1.20000
AFIX 0
C7 1 -0.146294 0.078884 0.491142 11.00000 0.01955 0.03061 =
0.02686 0.00997 0.00824 0.00323
C8 1 0.386474 0.372900 0.673424 11.00000 0.02159 0.03045 =
0.02979 0.00754 0.00615 0.00573
AFIX 43
H8 2 0.469865 0.321365 0.714143 11.00000 -1.20000
AFIX 0
C9 1 0.487841 0.507670 0.678985 11.00000 0.02136 0.03086 =
0.03209 0.00847 0.00742 0.00460
AFIX 43
H9 2 0.401384 0.559722 0.641638 11.00000 -1.20000
AFIX 0
C10 1 0.721272 0.582162 0.737837 11.00000 0.02240 0.02654 =
0.03016 0.00563 0.00884 0.00271
C11 1 0.816797 0.701453 0.701034 11.00000 0.02435 0.03121 =
0.03358 0.01162 0.00757 0.00455
AFIX 43
H11 2 0.728695 0.734638 0.642551 11.00000 -1.20000
AFIX 0
C12 1 1.038180 0.770538 0.749583 11.00000 0.02448 0.02968 =
0.03476 0.00997 0.01058 0.00102
AFIX 43
H12 2 1.099187 0.850734 0.723675 11.00000 -1.20000
AFIX 0
C13 1 1.173037 0.725609 0.835055 11.00000 0.02381 0.02760 =
0.03017 0.00400 0.00907 0.00212
C14 1 1.077560 0.609006 0.873147 11.00000 0.02472 0.03027 =
0.03206 0.00952 0.00530 0.00355
AFIX 43
H14 2 1.165616 0.577006 0.932641 11.00000 -1.20000
AFIX 0
C15 1 0.855684 0.539399 0.825119 11.00000 0.02454 0.02741 =
0.03308 0.00852 0.00847 -0.00015
AFIX 43
H15 2 0.794701 0.460718 0.852718 11.00000 -1.20000
AFIX 0
C16 1 1.415239 0.801970 0.881654 11.00000 0.02431 0.03017 =
0.03773 0.00831 0.00899 0.00213
AFIX 23
H16A 2 1.438234 0.904229 0.909244 11.00000 -1.20000
H16B 2 1.470709 0.790059 0.814081 11.00000 -1.20000
AFIX 0
C17 1 1.551303 0.755842 0.982571 11.00000 0.02366 0.03591 =
0.03746 0.00945 0.00908 0.00343
AFIX 23
H17A 2 1.534652 0.654565 0.955071 11.00000 -1.20000
H17B 2 1.496290 0.765938 1.050457 11.00000 -1.20000
AFIX 0
C18 1 1.791230 0.841131 1.025546 11.00000 0.02377 0.03229 =
0.03534 0.00777 0.00913 0.00262
AFIX 23
H18A 2 1.848852 0.826266 0.959140 11.00000 -1.20000
H18B 2 1.807560 0.942991 1.048545 11.00000 -1.20000
AFIX 0
C19 1 1.922566 0.800101 1.130930 11.00000 0.02950 0.04456 =
0.04372 0.01657 0.00769 0.00354
AFIX 23
H19A 2 1.863461 0.814973 1.196714 11.00000 -1.20000
H19B 2 1.903486 0.697863 1.107480 11.00000 -1.20000
AFIX 0
C20 1 2.161071 0.880084 1.177103 11.00000 0.02779 0.04860 =
0.03945 0.01178 0.00214 0.01073
AFIX 137
H20A 2 2.222482 0.864778 1.113308 11.00000 -1.50000
H20B 2 2.233571 0.846381 1.244425 11.00000 -1.50000
H20C 2 2.182725 0.981263 1.203694 11.00000 -1.50000
HKLF 4
REM pere25 in P-1
REM R1 = 0.0649 for 2241 Fo > 4sig(Fo) and 0.0749 for all 2724 data
REM 182 parameters refined using 0 restraints
END
WGHT 0.1066 0.4743
REM Highest difference peak 0.646, deepest hole -0.338, 1-sigma level 0.066
Q1 1 1.6646 0.6348 1.0470 11.00000 0.05 0.65
Q2 1 1.8938 0.7903 1.0457 11.00000 0.05 0.31
Q3 1 2.0985 0.8012 1.1632 11.00000 0.05 0.25
Q4 1 1.1417 0.7261 0.7504 11.00000 0.05 0.23
Q5 1 0.2302 -0.1228 0.5600 11.00000 0.05 0.22
;


data_pere26
_database_code_depnum_ccdc_archive 'CCDC 923795'
#TrackingRef 'web_deposit_cif_file_1_FrancineBelanger-Gariepy_1360246543.910DPSAnt.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H42'
_chemical_formula_sum            'C40 H42'
_chemical_formula_weight         522.74
_chemical_compound_source        'Synthesized by the authors. See text'
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'
_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   6.5844(3)
_cell_length_b                   9.2194(3)
_cell_length_c                   13.5405(5)
_cell_angle_alpha                100.0975(16)
_cell_angle_beta                 99.8398(18)
_cell_angle_gamma                105.7088(16)
_cell_volume                     758.05(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100
_cell_measurement_reflns_used    12181
_cell_measurement_theta_min      3.41
_cell_measurement_theta_max      70.50
_exptl_crystal_description       needle
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             282
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_Type   multi-scan
_exptl_absorpt_correction_T_min  0.8227
_exptl_absorpt_correction_T_max  0.9952
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2008)'
_exptl_special_details           
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker smart diffractometer equiped with an APEX II CCD Detector,
a graphite monochromator. The crystal-to-detector distance was
5.0 cm, and the data collection was carried out in 512 x 512 pixel mode.
The initial unit cell parameters were determined by a least-squares fit
of the angular setting of strong reflections, collected by a 10.0 degree
scan in 33 frames over four different parts of the reciprocal space
(132 frames total).
;
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Incoatec I\muS Microsource '
_diffrn_radiation_monochromator  'Quazar MX'
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            24364
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_sigmaI/netI    0.0139
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.41
_diffrn_reflns_theta_max         70.81
_reflns_number_total             2804
_reflns_number_gt                2527
_reflns_threshold_expression     I>2\s(I)
_computing_data_collection       'APEX2 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'UdMX (Maris, 2004)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1082P)^2^+0.2318P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2804
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1636
_refine_ls_wR_factor_gt          0.1582
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1347(2) 0.91825(16) 0.45910(10) 0.0263(3) Uani 1 1 d . . .
C2 C 0.0152(2) 0.86273(15) 0.52928(10) 0.0263(3) Uani 1 1 d . . .
C3 C 0.0173(2) 0.72005(16) 0.55706(11) 0.0299(3) Uani 1 1 d . . .
H3 H 0.1084 0.6660 0.5313 0.036 Uiso 1 1 calc R . .
C4 C -0.1078(3) 0.66006(17) 0.61932(11) 0.0333(4) Uani 1 1 d . . .
H4 H -0.1037 0.5650 0.6362 0.040 Uiso 1 1 calc R . .
C5 C -0.2446(3) 0.73941(17) 0.65919(11) 0.0331(4) Uani 1 1 d . . .
H5 H -0.3323 0.6970 0.7024 0.040 Uiso 1 1 calc R . .
C6 C -0.2500(2) 0.87601(16) 0.63547(11) 0.0299(3) Uani 1 1 d . . .
H6 H -0.3417 0.9278 0.6631 0.036 Uiso 1 1 calc R . .
C7 C -0.1220(2) 0.94407(15) 0.57029(10) 0.0261(3) Uani 1 1 d . . .
C8 C 0.2700(2) 0.82923(15) 0.41732(11) 0.0272(3) Uani 1 1 d . . .
H8 H 0.3806 0.8126 0.4648 0.033 Uiso 1 1 calc R . .
C9 C 0.2464(2) 0.77090(15) 0.31728(11) 0.0277(3) Uani 1 1 d . . .
H9 H 0.1399 0.7930 0.2707 0.033 Uiso 1 1 calc R . .
C10 C 0.3688(2) 0.67573(15) 0.27171(11) 0.0276(3) Uani 1 1 d . . .
C11 C 0.2962(2) 0.59731(16) 0.16821(11) 0.0304(3) Uani 1 1 d . . .
H11 H 0.1727 0.6104 0.1275 0.036 Uiso 1 1 calc R . .
C12 C 0.4012(3) 0.50025(16) 0.12340(11) 0.0327(4) Uani 1 1 d . . .
H12 H 0.3462 0.4461 0.0532 0.039 Uiso 1 1 calc R . .
C13 C 0.5856(3) 0.48127(16) 0.17994(12) 0.0320(4) Uani 1 1 d . . .
C14 C 0.6616(2) 0.56274(17) 0.28281(12) 0.0339(4) Uani 1 1 d . . .
H14 H 0.7888 0.5530 0.3225 0.041 Uiso 1 1 calc R . .
C15 C 0.5555(2) 0.65752(17) 0.32828(11) 0.0318(3) Uani 1 1 d . . .
H15 H 0.6101 0.7108 0.3987 0.038 Uiso 1 1 calc R . .
C16 C 0.6971(3) 0.37318(18) 0.13255(13) 0.0384(4) Uani 1 1 d . . .
H16A H 0.8560 0.4226 0.1563 0.046 Uiso 1 1 calc R . .
H16B H 0.6592 0.3581 0.0567 0.046 Uiso 1 1 calc R . .
C17 C 0.6376(3) 0.21464(17) 0.15894(12) 0.0337(4) Uani 1 1 d . . .
H17A H 0.6679 0.2289 0.2348 0.040 Uiso 1 1 calc R . .
H17B H 0.4805 0.1613 0.1312 0.040 Uiso 1 1 calc R . .
C18 C 0.7655(3) 0.11396(17) 0.11429(12) 0.0346(4) Uani 1 1 d . . .
H18A H 0.7257 0.0936 0.0381 0.042 Uiso 1 1 calc R . .
H18B H 0.9221 0.1722 0.1372 0.042 Uiso 1 1 calc R . .
C19 C 0.7266(3) -0.04003(18) 0.14554(13) 0.0400(4) Uani 1 1 d . . .
H19A H 0.7644 -0.0205 0.2217 0.048 Uiso 1 1 calc R . .
H19B H 0.5707 -0.1000 0.1213 0.048 Uiso 1 1 calc R . .
C20 C 0.8587(3) -0.13439(18) 0.10148(13) 0.0441(4) Uani 1 1 d . . .
H20A H 0.8217 -0.1541 0.0261 0.066 Uiso 1 1 calc R . .
H20B H 0.8270 -0.2332 0.1223 0.066 Uiso 1 1 calc R . .
H20C H 1.0134 -0.0771 0.1274 0.066 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0233(7) 0.0274(7) 0.0273(6) 0.0024(5) 0.0031(5) 0.0105(5)
C2 0.0247(7) 0.0270(7) 0.0268(6) 0.0028(5) 0.0040(5) 0.0110(5)
C3 0.0314(8) 0.0294(7) 0.0326(7) 0.0059(5) 0.0077(6) 0.0162(6)
C4 0.0389(8) 0.0287(7) 0.0372(8) 0.0099(6) 0.0108(6) 0.0158(6)
C5 0.0354(8) 0.0319(8) 0.0356(7) 0.0091(6) 0.0135(6) 0.0123(6)
C6 0.0294(8) 0.0289(7) 0.0333(7) 0.0045(5) 0.0100(6) 0.0124(6)
C7 0.0237(7) 0.0269(7) 0.0271(6) 0.0026(5) 0.0039(5) 0.0102(5)
C8 0.0232(7) 0.0273(7) 0.0332(7) 0.0067(5) 0.0071(5) 0.0112(5)
C9 0.0251(7) 0.0262(7) 0.0339(7) 0.0064(5) 0.0079(6) 0.0111(5)
C10 0.0261(7) 0.0246(7) 0.0342(7) 0.0061(5) 0.0116(6) 0.0087(5)
C11 0.0304(8) 0.0292(7) 0.0335(7) 0.0071(6) 0.0099(6) 0.0106(6)
C12 0.0386(8) 0.0282(7) 0.0329(7) 0.0045(5) 0.0148(6) 0.0105(6)
C13 0.0346(8) 0.0257(7) 0.0416(8) 0.0085(6) 0.0204(6) 0.0111(6)
C14 0.0276(8) 0.0319(7) 0.0442(8) 0.0058(6) 0.0107(6) 0.0131(6)
C15 0.0269(7) 0.0304(7) 0.0370(7) 0.0006(6) 0.0082(6) 0.0112(6)
C16 0.0442(9) 0.0328(8) 0.0468(9) 0.0096(7) 0.0237(7) 0.0175(7)
C17 0.0336(8) 0.0331(8) 0.0372(8) 0.0075(6) 0.0114(6) 0.0131(6)
C18 0.0376(9) 0.0318(8) 0.0368(8) 0.0063(6) 0.0098(6) 0.0149(6)
C19 0.0409(9) 0.0354(8) 0.0446(9) 0.0110(7) 0.0058(7) 0.0147(7)
C20 0.0565(11) 0.0287(8) 0.0443(9) 0.0041(6) -0.0022(8) 0.0197(7)
_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_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . . 1.411(2) y
C1 C7 . 2_576 1.4141(19) y
C1 C8 . . 1.4807(18) y
C2 C3 . . 1.4330(19) y
C2 C7 . . 1.4422(18) y
C3 C4 . . 1.360(2) y
C3 H3 . . 0.9500 ?
C4 C5 . . 1.422(2) y
C4 H4 . . 0.9500 ?
C5 C6 . . 1.361(2) y
C5 H5 . . 0.9500 ?
C6 C7 . . 1.430(2) y
C6 H6 . . 0.9500 ?
C7 C1 . 2_576 1.4141(19) y
C8 C9 . . 1.333(2) y
C8 H8 . . 0.9500 ?
C9 C10 . . 1.4707(18) y
C9 H9 . . 0.9500 ?
C10 C11 . . 1.394(2) y
C10 C15 . . 1.400(2) y
C11 C12 . . 1.3910(19) y
C11 H11 . . 0.9500 ?
C12 C13 . . 1.391(2) y
C12 H12 . . 0.9500 ?
C13 C14 . . 1.395(2) y
C13 C16 . . 1.5088(18) y
C14 C15 . . 1.3855(19) y
C14 H14 . . 0.9500 ?
C15 H15 . . 0.9500 ?
C16 C17 . . 1.529(2) y
C16 H16a . . 0.9900 ?
C16 H16b . . 0.9900 ?
C17 C18 . . 1.5287(19) y
C17 H17a . . 0.9900 ?
C17 H17b . . 0.9900 ?
C18 C19 . . 1.520(2) y
C18 H18a . . 0.9900 ?
C18 H18b . . 0.9900 ?
C19 C20 . . 1.508(2) y
C19 H19a . . 0.9900 ?
C19 H19b . . 0.9900 ?
C20 H20a . . 0.9800 ?
C20 H20b . . 0.9800 ?
C20 H20c . . 0.9800 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 C7 . . 2_576 119.75(12) y
C2 C1 C8 . . . 118.73(12) y
C7 C1 C8 2_576 . . 121.52(12) y
C1 C2 C3 . . . 121.05(12) y
C1 C2 C7 . . . 120.59(12) y
C3 C2 C7 . . . 118.27(13) y
C4 C3 C2 . . . 121.72(13) y
C4 C3 H3 . . . 119.1 ?
C2 C3 H3 . . . 119.1 ?
C3 C4 C5 . . . 120.12(13) y
C3 C4 H4 . . . 119.9 ?
C5 C4 H4 . . . 119.9 ?
C6 C5 C4 . . . 120.06(13) y
C6 C5 H5 . . . 120.0 ?
C4 C5 H5 . . . 120.0 ?
C5 C6 C7 . . . 122.08(13) y
C5 C6 H6 . . . 119.0 ?
C7 C6 H6 . . . 119.0 ?
C1 C7 C6 2_576 . . 122.51(12) y
C1 C7 C2 2_576 . . 119.66(13) y
C6 C7 C2 . . . 117.74(12) y
C9 C8 C1 . . . 124.15(12) y
C9 C8 H8 . . . 117.9 ?
C1 C8 H8 . . . 117.9 ?
C8 C9 C10 . . . 126.54(13) y
C8 C9 H9 . . . 116.7 ?
C10 C9 H9 . . . 116.7 ?
C11 C10 C15 . . . 117.73(13) y
C11 C10 C9 . . . 119.40(13) y
C15 C10 C9 . . . 122.87(13) y
C12 C11 C10 . . . 121.22(14) y
C12 C11 H11 . . . 119.4 ?
C10 C11 H11 . . . 119.4 ?
C11 C12 C13 . . . 120.97(13) y
C11 C12 H12 . . . 119.5 ?
C13 C12 H12 . . . 119.5 ?
C12 C13 C14 . . . 117.83(13) y
C12 C13 C16 . . . 121.23(13) y
C14 C13 C16 . . . 120.92(14) y
C15 C14 C13 . . . 121.42(14) y
C15 C14 H14 . . . 119.3 ?
C13 C14 H14 . . . 119.3 ?
C14 C15 C10 . . . 120.80(13) y
C14 C15 H15 . . . 119.6 ?
C10 C15 H15 . . . 119.6 ?
C13 C16 C17 . . . 113.88(12) y
C13 C16 H16A . . . 108.8 ?
C17 C16 H16A . . . 108.8 ?
C13 C16 H16B . . . 108.8 ?
C17 C16 H16B . . . 108.8 ?
H16A C16 H16B . . . 107.7 ?
C18 C17 C16 . . . 111.48(12) y
C18 C17 H17A . . . 109.3 ?
C16 C17 H17A . . . 109.3 ?
C18 C17 H17B . . . 109.3 ?
C16 C17 H17B . . . 109.3 ?
H17A C17 H17B . . . 108.0 ?
C19 C18 C17 . . . 113.76(13) y
C19 C18 H18A . . . 108.8 ?
C17 C18 H18A . . . 108.8 ?
C19 C18 H18B . . . 108.8 ?
C17 C18 H18B . . . 108.8 ?
H18A C18 H18B . . . 107.7 ?
C20 C19 C18 . . . 112.04(14) y
C20 C19 H19A . . . 109.2 ?
C18 C19 H19A . . . 109.2 ?
C20 C19 H19B . . . 109.2 ?
C18 C19 H19B . . . 109.2 ?
H19A C19 H19B . . . 107.9 ?
C19 C20 H20A . . . 109.5 ?
C19 C20 H20B . . . 109.5 ?
H20A C20 H20B . . . 109.5 ?
C19 C20 H20C . . . 109.5 ?
H20A C20 H20C . . . 109.5 ?
H20B C20 H20C . . . 109.5 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C7 C1 C2 C3 2_576 . . . 177.25(12) y
C8 C1 C2 C3 . . . . -2.3(2) y
C7 C1 C2 C7 2_576 . . . 0.8(2) y
C8 C1 C2 C7 . . . . -178.76(11) y
C1 C2 C3 C4 . . . . -175.70(13) y
C7 C2 C3 C4 . . . . 0.8(2) y
C2 C3 C4 C5 . . . . -0.3(2) y
C3 C4 C5 C6 . . . . -0.3(2) y
C4 C5 C6 C7 . . . . 0.4(2) y
C5 C6 C7 C1 . . . 2_576 176.68(13) y
C5 C6 C7 C2 . . . . 0.2(2) y
C1 C2 C7 C1 . . . 2_576 -0.8(2) y
C3 C2 C7 C1 . . . 2_576 -177.35(12) y
C1 C2 C7 C6 . . . . 175.81(12) y
C3 C2 C7 C6 . . . . -0.72(19) y
C2 C1 C8 C9 . . . . 121.22(15) y
C7 C1 C8 C9 2_576 . . . -58.3(2) y
C1 C8 C9 C10 . . . . -176.96(12) y
C8 C9 C10 C11 . . . . 166.90(14) y
C8 C9 C10 C15 . . . . -12.0(2) y
C15 C10 C11 C12 . . . . 2.1(2) y
C9 C10 C11 C12 . . . . -176.90(12) y
C10 C11 C12 C13 . . . . -1.6(2) y
C11 C12 C13 C14 . . . . 0.0(2) y
C11 C12 C13 C16 . . . . 178.49(12) y
C12 C13 C14 C15 . . . . 1.1(2) y
C16 C13 C14 C15 . . . . -177.39(13) y
C13 C14 C15 C10 . . . . -0.6(2) y
C11 C10 C15 C14 . . . . -1.0(2) y
C9 C10 C15 C14 . . . . 177.96(12) y
C12 C13 C16 C17 . . . . -98.74(17) y
C14 C13 C16 C17 . . . . 79.74(18) y
C13 C16 C17 C18 . . . . -176.57(13) y
C16 C17 C18 C19 . . . . 175.23(13) y
C17 C18 C19 C20 . . . . -178.97(12) y
_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        70.81
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.048
_vrf_DIFMX01_pere26              
;
PROBLEM: TThe maximum difference density is > 0.1*ZMAX*0.75
_refine_diff_density_max given = 0.507
Test value = 0.450
RESPONSE: The highest peak is between C17 and C19.
Disorder of the chain is suspected but no good model could be found.
;
_vrf_PLAT029_pere26              
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.966
RESPONSE: Missing data is due to geometric restraints of the instruments,
which are especially severe for triclinic crystals.
;
_iucr_refine_instructions_details 
;
TITL pere26 in P-1
CELL 1.54178 6.5844 9.2194 13.5405 100.098 99.840 105.709
ZERR 1.00 0.0003 0.0003 0.0005 0.002 0.002 0.002
LATT 1
SFAC C H
UNIT 40 42
SIZE 0.01 0.06 0.26
TEMP -173
ACTA
L.S. 10
BOND $H
CONF
WPDB -1
FMAP 2
PLAN -5
WGHT 0.108200 0.231800
FVAR 0.45210
C1 1 0.134705 0.918249 0.459095 11.00000 0.02330 0.02743 =
0.02725 0.00239 0.00314 0.01051
C2 1 0.015212 0.862731 0.529277 11.00000 0.02465 0.02702 =
0.02681 0.00278 0.00395 0.01096
C3 1 0.017271 0.720052 0.557063 11.00000 0.03145 0.02937 =
0.03264 0.00593 0.00772 0.01621
AFIX 43
H3 2 0.108378 0.665975 0.531311 11.00000 -1.20000
AFIX 0
C4 1 -0.107763 0.660060 0.619320 11.00000 0.03892 0.02866 =
0.03724 0.00991 0.01083 0.01581
AFIX 43
H4 2 -0.103721 0.564974 0.636224 11.00000 -1.20000
AFIX 0
C5 1 -0.244618 0.739406 0.659192 11.00000 0.03542 0.03191 =
0.03563 0.00906 0.01354 0.01228
AFIX 43
H5 2 -0.332338 0.697018 0.702422 11.00000 -1.20000
AFIX 0
C6 1 -0.250012 0.876010 0.635466 11.00000 0.02943 0.02893 =
0.03326 0.00454 0.01000 0.01239
AFIX 43
H6 2 -0.341697 0.927767 0.663079 11.00000 -1.20000
AFIX 0
C7 1 -0.122032 0.944069 0.570292 11.00000 0.02369 0.02686 =
0.02708 0.00258 0.00394 0.01024
C8 1 0.270000 0.829225 0.417317 11.00000 0.02323 0.02727 =
0.03315 0.00671 0.00711 0.01118
AFIX 43
H8 2 0.380601 0.812640 0.464846 11.00000 -1.20000
AFIX 0
C9 1 0.246449 0.770898 0.317277 11.00000 0.02505 0.02625 =
0.03388 0.00640 0.00794 0.01111
AFIX 43
H9 2 0.139909 0.793014 0.270717 11.00000 -1.20000
AFIX 0
C10 1 0.368833 0.675727 0.271711 11.00000 0.02613 0.02455 =
0.03421 0.00611 0.01164 0.00867
C11 1 0.296198 0.597307 0.168205 11.00000 0.03035 0.02915 =
0.03351 0.00714 0.00993 0.01064
AFIX 43
H11 2 0.172709 0.610407 0.127529 11.00000 -1.20000
AFIX 0
C12 1 0.401201 0.500250 0.123402 11.00000 0.03855 0.02817 =
0.03291 0.00454 0.01479 0.01051
AFIX 43
H12 2 0.346172 0.446129 0.053171 11.00000 -1.20000
AFIX 0
C13 1 0.585647 0.481266 0.179935 11.00000 0.03463 0.02572 =
0.04155 0.00850 0.02039 0.01113
C14 1 0.661595 0.562736 0.282812 11.00000 0.02763 0.03187 =
0.04421 0.00577 0.01074 0.01312
AFIX 43
H14 2 0.788797 0.553012 0.322542 11.00000 -1.20000
AFIX 0
C15 1 0.555506 0.657521 0.328284 11.00000 0.02692 0.03037 =
0.03700 0.00059 0.00824 0.01117
AFIX 43
H15 2 0.610069 0.710804 0.398696 11.00000 -1.20000
AFIX 0
C16 1 0.697142 0.373177 0.132549 11.00000 0.04417 0.03282 =
0.04678 0.00960 0.02372 0.01752
AFIX 23
H16A 2 0.855955 0.422586 0.156280 11.00000 -1.20000
H16B 2 0.659190 0.358078 0.056693 11.00000 -1.20000
AFIX 0
C17 1 0.637580 0.214637 0.158945 11.00000 0.03359 0.03306 =
0.03722 0.00753 0.01141 0.01306
AFIX 23
H17A 2 0.667885 0.228899 0.234786 11.00000 -1.20000
H17B 2 0.480480 0.161272 0.131159 11.00000 -1.20000
AFIX 0
C18 1 0.765485 0.113964 0.114288 11.00000 0.03756 0.03185 =
0.03679 0.00629 0.00978 0.01489
AFIX 23
H18A 2 0.725718 0.093592 0.038142 11.00000 -1.20000
H18B 2 0.922067 0.172223 0.137223 11.00000 -1.20000
AFIX 0
C19 1 0.726569 -0.040027 0.145544 11.00000 0.04087 0.03543 =
0.04458 0.01101 0.00580 0.01468
AFIX 23
H19A 2 0.764376 -0.020460 0.221682 11.00000 -1.20000
H19B 2 0.570747 -0.099978 0.121295 11.00000 -1.20000
AFIX 0
C20 1 0.858722 -0.134391 0.101475 11.00000 0.05647 0.02870 =
0.04426 0.00407 -0.00222 0.01968
AFIX 137
H20A 2 0.821689 -0.154116 0.026086 11.00000 -1.50000
H20B 2 0.826984 -0.233233 0.122276 11.00000 -1.50000
H20C 2 1.013351 -0.077130 0.127434 11.00000 -1.50000
HKLF 4
REM pere26 in P-1
REM R1 = 0.0532 for 2527 Fo > 4sig(Fo) and 0.0568 for all 2804 data
REM 182 parameters refined using 0 restraints
END
WGHT 0.0979 0.2444
REM Highest difference peak 0.507, deepest hole -0.231, 1-sigma level 0.048
Q1 1 0.5065 0.0414 0.1658 11.00000 0.05 0.51
Q2 1 0.8989 0.1829 0.0938 11.00000 0.05 0.49
Q3 1 0.7599 -0.1339 0.1338 11.00000 0.05 0.23
Q4 1 0.8006 0.0580 0.1520 11.00000 0.05 0.22
Q5 1 0.5966 0.5000 0.2360 11.00000 0.05 0.20
;