data_global
# SUBMISSION DETAILS
_publ_contact_author_name 'Prof. Dr. Edwin Weber'
_publ_contact_author_address
; Institut f\"ur Organische Chemie
TU Bergakademie Freiberg
Leipziger Strasse 29
D-09596 Freiberg/Sachsen
Germany
;
_publ_contact_author_email Edwin.Weber@chemie.tu-freiberg.de
_publ_contact_author_fax '49(03731) 393170'
_publ_contact_author_phone '49(03731) 392386'
_publ_requested_journal 'Crystal Growth and Design'
# TITLE AND AUTHOR LIST
_publ_section_title
;
Versatility in complexation of aprotic guest molecules by terphenyl
modified bisfluorenol hosts. Solid state structures of nine inclusion
species and of an unsolvated host compound
;
loop_
_publ_author_name
_publ_author_address
'Klien, Hendrik'
; Institut f\"ur Organische Chemie
TU Bergakademie Freiberg
Leipziger Strasse 29
D-09596 Freiberg/Sachsen
Germany
;
'Seichter, Wilhelm'
; Institut f\"ur Organische Chemie
TU Bergakademie Freiberg
Leipziger Strasse 29
D-09596 Freiberg/Sachsen
Germany
;
'Weber, Edwin'
; Institut f\"ur Organische Chemie
TU Bergakademie Freiberg
Leipziger Strasse 29
D-09596 Freiberg/Sachsen
Germany
;
# TEXT
_publ_section_abstract
;
Crystalline inclusion compounds of the diol hosts 1 and 2
typical of a basic 2,2"-[1,1':4',4"]-terphenyl moiety with two attached
9-fluorenol or tert-butyl substituted 9-fluorenol units and a
variety of aprotic guest molecules have been prepared and studied with
reference to their crystal structures. Common and differing structural
features among one another and including previously described host-guest
complexes of 1 and 2 with protic instead of aprotic guest
species are distinguished indicating potential uses in practical crystal
engineering in particular of two-component molecular systems.
;
data_klien_11_0m
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C60 H62 O2, 2(C4 H8 O)'
_chemical_formula_sum
'C68 H78 O4'
_chemical_formula_weight 959.30
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'
'O' 'O' 0.0106 0.0060
'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 10.6569(2)
_cell_length_b 11.2177(3)
_cell_length_c 23.0926(5)
_cell_angle_alpha 79.9450(10)
_cell_angle_beta 80.6840(10)
_cell_angle_gamma 87.8270(10)
_cell_volume 2682.24(11)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 5519
_cell_measurement_theta_min 2.19
_cell_measurement_theta_max 24.92
_exptl_crystal_description prism
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.07
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.188
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1036
_exptl_absorpt_coefficient_mu 0.072
_exptl_absorpt_correction_type none
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% <1%
_diffrn_reflns_number 50323
_diffrn_reflns_av_R_equivalents 0.0642
_diffrn_reflns_av_sigmaI/netI 0.0736
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_theta_min 0.91
_diffrn_reflns_theta_max 27.80
_reflns_number_total 12664
_reflns_number_gt 7809
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Kappa APEX 2 (Bruker-AXS)'
_computing_cell_refinement 'SAINT-NT (Sheldrick, 2008)'
_computing_data_reduction 'SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ORTEP-3 (Farrugia)'
_computing_publication_material 'SHELXTL'
_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^)+(0.0517P)^2^+0.8994P] 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 12664
_refine_ls_number_parameters 663
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1073
_refine_ls_R_factor_gt 0.0551
_refine_ls_wR_factor_ref 0.1354
_refine_ls_wR_factor_gt 0.1127
_refine_ls_goodness_of_fit_ref 1.003
_refine_ls_restrained_S_all 1.003
_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
O1 O 0.39068(12) 0.04519(12) 0.27380(5) 0.0203(3) Uani 1 1 d . . .
H1 H 0.3199 0.0133 0.2754 0.030 Uiso 1 1 calc R . .
C1 C 0.31474(17) 0.08505(16) 0.37424(8) 0.0167(4) Uani 1 1 d . . .
C2 C 0.27469(17) 0.20419(17) 0.37089(8) 0.0178(4) Uani 1 1 d . . .
H2 H 0.3124 0.2640 0.3392 0.021 Uiso 1 1 calc R . .
C3 C 0.17834(17) 0.23654(17) 0.41438(8) 0.0193(4) Uani 1 1 d . . .
C4 C 0.12577(18) 0.14413(18) 0.45981(8) 0.0217(4) Uani 1 1 d . . .
H4 H 0.0607 0.1646 0.4899 0.026 Uiso 1 1 calc R . .
C5 C 0.16442(17) 0.02469(18) 0.46280(8) 0.0217(4) Uani 1 1 d . . .
H5 H 0.1256 -0.0357 0.4940 0.026 Uiso 1 1 calc R . .
C6 C 0.26088(17) -0.00595(17) 0.41964(8) 0.0180(4) Uani 1 1 d . . .
C7 C 0.32677(17) -0.12093(17) 0.41192(8) 0.0181(4) Uani 1 1 d . . .
C8 C 0.31365(17) -0.23587(17) 0.44511(8) 0.0192(4) Uani 1 1 d . . .
H8 H 0.2485 -0.2524 0.4787 0.023 Uiso 1 1 calc R . .
C9 C 0.39685(18) -0.32720(17) 0.42887(8) 0.0211(4) Uani 1 1 d . . .
H9 H 0.3869 -0.4063 0.4518 0.025 Uiso 1 1 calc R . .
C10 C 0.49442(18) -0.30689(17) 0.38015(8) 0.0195(4) Uani 1 1 d . . .
C11 C 0.50475(17) -0.18974(17) 0.34624(8) 0.0188(4) Uani 1 1 d . . .
H11 H 0.5685 -0.1732 0.3121 0.023 Uiso 1 1 calc R . .
C12 C 0.42309(17) -0.09897(17) 0.36226(8) 0.0179(4) Uani 1 1 d . . .
C13 C 0.42147(17) 0.03342(16) 0.33268(7) 0.0168(4) Uani 1 1 d . . .
C14 C 0.54770(17) 0.09719(16) 0.32807(8) 0.0173(4) Uani 1 1 d . . .
C15 C 0.60886(18) 0.15237(17) 0.27231(8) 0.0215(4) Uani 1 1 d . . .
H15 H 0.5724 0.1478 0.2379 0.026 Uiso 1 1 calc R . .
C16 C 0.72213(19) 0.21377(18) 0.26632(9) 0.0252(5) Uani 1 1 d . . .
H16 H 0.7623 0.2505 0.2279 0.030 Uiso 1 1 calc R . .
C17 C 0.77635(18) 0.22172(18) 0.31539(9) 0.0260(5) Uani 1 1 d . . .
H17 H 0.8534 0.2645 0.3113 0.031 Uiso 1 1 calc R . .
C18 C 0.71731(18) 0.16658(17) 0.37108(8) 0.0224(4) Uani 1 1 d . . .
H18 H 0.7551 0.1716 0.4051 0.027 Uiso 1 1 calc R . .
C19 C 0.60368(17) 0.10391(16) 0.37834(8) 0.0172(4) Uani 1 1 d . . .
C20 C 0.57649(17) -0.06950(17) 0.46441(8) 0.0182(4) Uani 1 1 d . . .
H20 H 0.6296 -0.1177 0.4403 0.022 Uiso 1 1 calc R . .
C21 C 0.54825(16) 0.04901(16) 0.44083(8) 0.0164(4) Uani 1 1 d . . .
C22 C 0.47172(17) 0.11844(17) 0.47731(8) 0.0185(4) Uani 1 1 d . . .
H22 H 0.4524 0.2001 0.4621 0.022 Uiso 1 1 calc R . .
C23 C 0.13265(18) 0.36741(17) 0.41542(8) 0.0217(4) Uani 1 1 d . . .
C24 C 0.2018(2) 0.45617(18) 0.36318(9) 0.0268(5) Uani 1 1 d . . .
H24A H 0.2933 0.4526 0.3647 0.040 Uiso 1 1 calc R . .
H24B H 0.1698 0.5385 0.3657 0.040 Uiso 1 1 calc R . .
H24C H 0.1867 0.4343 0.3256 0.040 Uiso 1 1 calc R . .
C25 C 0.1571(2) 0.40442(19) 0.47357(9) 0.0298(5) Uani 1 1 d . . .
H25A H 0.1072 0.3531 0.5076 0.045 Uiso 1 1 calc R . .
H25B H 0.1320 0.4893 0.4737 0.045 Uiso 1 1 calc R . .
H25C H 0.2478 0.3944 0.4765 0.045 Uiso 1 1 calc R . .
C26 C -0.01027(19) 0.3768(2) 0.41262(10) 0.0308(5) Uani 1 1 d . . .
H26A H -0.0262 0.3529 0.3756 0.046 Uiso 1 1 calc R . .
H26B H -0.0394 0.4604 0.4137 0.046 Uiso 1 1 calc R . .
H26C H -0.0565 0.3229 0.4468 0.046 Uiso 1 1 calc R . .
C27 C 0.58965(19) -0.40529(18) 0.36297(8) 0.0231(4) Uani 1 1 d . . .
C28 C 0.5720(2) -0.52410(19) 0.40745(9) 0.0345(5) Uani 1 1 d . . .
H28A H 0.5814 -0.5093 0.4471 0.052 Uiso 1 1 calc R . .
H28B H 0.6362 -0.5832 0.3950 0.052 Uiso 1 1 calc R . .
H28C H 0.4869 -0.5557 0.4087 0.052 Uiso 1 1 calc R . .
C29 C 0.5750(2) -0.43025(19) 0.30153(9) 0.0284(5) Uani 1 1 d . . .
H29A H 0.4885 -0.4581 0.3025 0.043 Uiso 1 1 calc R . .
H29B H 0.6363 -0.4929 0.2904 0.043 Uiso 1 1 calc R . .
H29C H 0.5908 -0.3558 0.2722 0.043 Uiso 1 1 calc R . .
C30 C 0.72533(19) -0.3615(2) 0.36117(10) 0.0310(5) Uani 1 1 d . . .
H30A H 0.7406 -0.2867 0.3321 0.047 Uiso 1 1 calc R . .
H30B H 0.7866 -0.4238 0.3496 0.047 Uiso 1 1 calc R . .
H30C H 0.7353 -0.3461 0.4007 0.047 Uiso 1 1 calc R . .
O1A O 0.89171(13) 0.62123(13) 0.22265(5) 0.0250(3) Uani 1 1 d . . .
H1A H 0.8588 0.6908 0.2204 0.038 Uiso 1 1 calc R . .
C1A C 1.00497(18) 0.69523(18) 0.12331(8) 0.0217(4) Uani 1 1 d . . .
C2A C 1.12073(19) 0.73796(18) 0.13012(9) 0.0251(4) Uani 1 1 d . . .
H2A H 1.1598 0.7040 0.1635 0.030 Uiso 1 1 calc R . .
C3A C 1.17985(19) 0.83125(19) 0.08764(9) 0.0278(5) Uani 1 1 d . . .
C4A C 1.1194(2) 0.87682(19) 0.03872(9) 0.0321(5) Uani 1 1 d . . .
H4A H 1.1600 0.9386 0.0088 0.038 Uiso 1 1 calc R . .
C5A C 1.0027(2) 0.83506(19) 0.03236(9) 0.0296(5) Uani 1 1 d . . .
H5A H 0.9636 0.8683 -0.0011 0.035 Uiso 1 1 calc R . .
C6A C 0.94393(19) 0.74431(18) 0.07543(8) 0.0236(4) Uani 1 1 d . . .
C7A C 0.82340(18) 0.68107(18) 0.08108(8) 0.0234(4) Uani 1 1 d . . .
C8A C 0.72955(19) 0.69225(19) 0.04548(9) 0.0271(5) Uani 1 1 d . . .
H8A H 0.7361 0.7515 0.0103 0.033 Uiso 1 1 calc R . .
C9A C 0.62566(19) 0.61588(19) 0.06174(9) 0.0280(5) Uani 1 1 d . . .
H9A H 0.5615 0.6239 0.0371 0.034 Uiso 1 1 calc R . .
C10A C 0.61200(18) 0.52774(19) 0.11295(9) 0.0246(4) Uani 1 1 d . . .
C11A C 0.70793(18) 0.51742(18) 0.14851(8) 0.0228(4) Uani 1 1 d . . .
H11A H 0.7014 0.4585 0.1838 0.027 Uiso 1 1 calc R . .
C12A C 0.81191(18) 0.59261(18) 0.13243(8) 0.0217(4) Uani 1 1 d . . .
C13A C 0.92698(18) 0.59302(17) 0.16410(8) 0.0209(4) Uani 1 1 d . . .
C14A C 0.99787(17) 0.47192(17) 0.17035(8) 0.0200(4) Uani 1 1 d . . .
C15A C 1.02985(18) 0.42137(18) 0.22562(8) 0.0227(4) Uani 1 1 d . . .
H15A H 1.0094 0.4643 0.2580 0.027 Uiso 1 1 calc R . .
C16A C 1.09062(19) 0.31024(19) 0.23447(9) 0.0261(5) Uani 1 1 d . . .
H16A H 1.1121 0.2781 0.2725 0.031 Uiso 1 1 calc R . .
C17A C 1.1202(2) 0.24574(19) 0.18831(9) 0.0283(5) Uani 1 1 d . . .
H17A H 1.1601 0.1684 0.1944 0.034 Uiso 1 1 calc R . .
C18A C 1.09065(19) 0.29597(19) 0.13265(9) 0.0263(5) Uani 1 1 d . . .
H18A H 1.1105 0.2517 0.1008 0.032 Uiso 1 1 calc R . .
C19A C 1.03290(18) 0.40903(18) 0.12244(8) 0.0215(4) Uani 1 1 d . . .
C20A C 1.01410(18) 0.45754(18) 0.05965(8) 0.0223(4) Uani 1 1 d . . .
C21A C 0.91500(18) 0.41792(18) 0.03572(8) 0.0230(4) Uani 1 1 d . . .
H21A H 0.8564 0.3610 0.0599 0.028 Uiso 1 1 calc R . .
C22A C 0.90029(18) 0.46017(18) -0.02291(8) 0.0225(4) Uani 1 1 d . . .
H22A H 0.8311 0.4328 -0.0382 0.027 Uiso 1 1 calc R . .
C23A C 1.3068(2) 0.8850(2) 0.09253(11) 0.0372(6) Uani 1 1 d . . .
C24A C 1.4036(2) 0.8654(3) 0.03841(11) 0.0511(7) Uani 1 1 d . . .
H24D H 1.4109 0.7787 0.0366 0.077 Uiso 1 1 calc R . .
H24E H 1.4865 0.8959 0.0419 0.077 Uiso 1 1 calc R . .
H24F H 1.3754 0.9089 0.0021 0.077 Uiso 1 1 calc R . .
C25A C 1.3573(2) 0.8272(2) 0.14900(11) 0.0490(7) Uani 1 1 d . . .
H25D H 1.2946 0.8375 0.1838 0.074 Uiso 1 1 calc R . .
H25E H 1.4369 0.8662 0.1509 0.074 Uiso 1 1 calc R . .
H25F H 1.3730 0.7407 0.1486 0.074 Uiso 1 1 calc R . .
C26A C 1.2888(3) 1.0202(2) 0.09275(15) 0.0650(9) Uani 1 1 d . . .
H26D H 1.2544 1.0583 0.0570 0.098 Uiso 1 1 calc R . .
H26E H 1.3710 1.0563 0.0931 0.098 Uiso 1 1 calc R . .
H26F H 1.2295 1.0330 0.1283 0.098 Uiso 1 1 calc R . .
C27A C 0.5006(2) 0.43949(19) 0.12875(9) 0.0286(5) Uani 1 1 d . . .
C28A C 0.4442(2) 0.4272(2) 0.19486(9) 0.0348(5) Uani 1 1 d . . .
H28D H 0.5099 0.3968 0.2191 0.052 Uiso 1 1 calc R . .
H28E H 0.3733 0.3704 0.2040 0.052 Uiso 1 1 calc R . .
H28F H 0.4136 0.5065 0.2038 0.052 Uiso 1 1 calc R . .
C29A C 0.3926(2) 0.4796(2) 0.09297(10) 0.0387(6) Uani 1 1 d . . .
H29D H 0.3220 0.4227 0.1062 0.058 Uiso 1 1 calc R . .
H29E H 0.4235 0.4808 0.0505 0.058 Uiso 1 1 calc R . .
H29F H 0.3631 0.5608 0.0993 0.058 Uiso 1 1 calc R . .
C30A C 0.5502(2) 0.3153(2) 0.11473(11) 0.0380(6) Uani 1 1 d . . .
H30D H 0.6204 0.2885 0.1367 0.057 Uiso 1 1 calc R . .
H30E H 0.5805 0.3222 0.0719 0.057 Uiso 1 1 calc R . .
H30F H 0.4814 0.2563 0.1267 0.057 Uiso 1 1 calc R . .
O1B O 0.14422(13) 0.94226(12) 0.28934(6) 0.0287(3) Uani 1 1 d . . .
C1B C 0.03639(19) 1.00192(19) 0.31916(9) 0.0277(5) Uani 1 1 d . . .
H1B1 H -0.0045 1.0589 0.2899 0.033 Uiso 1 1 calc R . .
H1B2 H 0.0636 1.0477 0.3479 0.033 Uiso 1 1 calc R . .
C2B C -0.0553(2) 0.9027(2) 0.35138(10) 0.0341(5) Uani 1 1 d . . .
H2B1 H -0.1182 0.8878 0.3263 0.041 Uiso 1 1 calc R . .
H2B2 H -0.1009 0.9232 0.3893 0.041 Uiso 1 1 calc R . .
C3B C 0.0328(2) 0.7942(2) 0.36232(10) 0.0343(5) Uani 1 1 d . . .
H3B1 H 0.0723 0.7945 0.3983 0.041 Uiso 1 1 calc R . .
H3B2 H -0.0129 0.7171 0.3667 0.041 Uiso 1 1 calc R . .
C4B C 0.1305(2) 0.81331(19) 0.30662(10) 0.0335(5) Uani 1 1 d . . .
H4B1 H 0.2125 0.7748 0.3146 0.040 Uiso 1 1 calc R . .
H4B2 H 0.1014 0.7780 0.2747 0.040 Uiso 1 1 calc R . .
O1C O 0.79056(16) 0.85557(14) 0.20801(7) 0.0391(4) Uani 1 1 d . . .
C1C C 0.6793(2) 0.8855(2) 0.18129(9) 0.0336(5) Uani 1 1 d . . .
H1C1 H 0.6128 0.9201 0.2089 0.040 Uiso 1 1 calc R . .
H1C2 H 0.6451 0.8125 0.1709 0.040 Uiso 1 1 calc R . .
C2C C 0.7198(2) 0.9773(2) 0.12595(10) 0.0355(5) Uani 1 1 d . . .
H2C1 H 0.6523 1.0390 0.1195 0.043 Uiso 1 1 calc R . .
H2C2 H 0.7397 0.9376 0.0904 0.043 Uiso 1 1 calc R . .
C3C C 0.8370(3) 1.0336(3) 0.13826(11) 0.0564(8) Uani 1 1 d . . .
H3C1 H 0.9078 1.0324 0.1048 0.068 Uiso 1 1 calc R . .
H3C2 H 0.8196 1.1186 0.1437 0.068 Uiso 1 1 calc R . .
C4C C 0.8699(3) 0.9593(2) 0.19371(14) 0.0587(8) Uani 1 1 d . . .
H4C1 H 0.9605 0.9343 0.1876 0.070 Uiso 1 1 calc R . .
H4C2 H 0.8557 1.0068 0.2266 0.070 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
O1 0.0222(7) 0.0250(7) 0.0140(6) -0.0023(5) -0.0040(5) -0.0041(6)
C1 0.0150(9) 0.0209(10) 0.0148(9) -0.0036(7) -0.0031(7) -0.0012(7)
C2 0.0166(9) 0.0206(10) 0.0162(9) -0.0026(7) -0.0024(7) -0.0048(8)
C3 0.0163(9) 0.0221(10) 0.0216(10) -0.0073(8) -0.0049(7) -0.0020(8)
C4 0.0168(9) 0.0273(11) 0.0212(10) -0.0079(8) 0.0015(8) -0.0040(8)
C5 0.0179(10) 0.0268(11) 0.0195(10) -0.0025(8) -0.0004(8) -0.0076(8)
C6 0.0154(9) 0.0228(10) 0.0160(9) -0.0034(7) -0.0022(7) -0.0048(8)
C7 0.0172(9) 0.0224(10) 0.0153(9) -0.0036(7) -0.0031(7) -0.0033(8)
C8 0.0167(9) 0.0245(10) 0.0154(9) -0.0018(8) 0.0004(7) -0.0055(8)
C9 0.0254(10) 0.0199(10) 0.0172(9) 0.0008(8) -0.0035(8) -0.0072(8)
C10 0.0210(10) 0.0199(10) 0.0182(9) -0.0032(8) -0.0044(8) -0.0027(8)
C11 0.0178(9) 0.0235(10) 0.0141(9) -0.0020(7) 0.0000(7) -0.0044(8)
C12 0.0184(9) 0.0204(10) 0.0149(9) -0.0015(7) -0.0032(7) -0.0051(8)
C13 0.0175(9) 0.0198(10) 0.0123(9) -0.0018(7) -0.0006(7) -0.0019(8)
C14 0.0166(9) 0.0162(9) 0.0177(9) -0.0030(7) 0.0020(7) -0.0004(7)
C15 0.0250(10) 0.0215(10) 0.0167(9) -0.0022(8) 0.0002(8) -0.0028(8)
C16 0.0266(11) 0.0228(11) 0.0208(10) 0.0002(8) 0.0089(8) -0.0056(9)
C17 0.0181(10) 0.0273(11) 0.0307(11) -0.0050(9) 0.0036(8) -0.0081(8)
C18 0.0197(10) 0.0254(11) 0.0221(10) -0.0042(8) -0.0025(8) -0.0023(8)
C19 0.0169(9) 0.0155(9) 0.0186(9) -0.0033(7) -0.0001(7) -0.0004(7)
C20 0.0158(9) 0.0215(10) 0.0181(9) -0.0069(8) -0.0015(7) -0.0006(8)
C21 0.0117(9) 0.0215(10) 0.0165(9) -0.0032(7) -0.0026(7) -0.0046(7)
C22 0.0190(9) 0.0167(9) 0.0199(9) -0.0020(8) -0.0048(8) -0.0008(8)
C23 0.0186(10) 0.0237(10) 0.0236(10) -0.0077(8) -0.0018(8) -0.0001(8)
C24 0.0284(11) 0.0222(11) 0.0296(11) -0.0056(9) -0.0027(9) 0.0015(9)
C25 0.0339(12) 0.0295(12) 0.0278(11) -0.0130(9) -0.0011(9) -0.0044(10)
C26 0.0244(11) 0.0316(12) 0.0374(12) -0.0109(10) -0.0036(9) 0.0038(9)
C27 0.0235(10) 0.0223(10) 0.0221(10) -0.0028(8) -0.0007(8) 0.0001(8)
C28 0.0406(13) 0.0253(12) 0.0318(12) 0.0028(9) 0.0024(10) 0.0048(10)
C29 0.0298(11) 0.0268(11) 0.0284(11) -0.0073(9) -0.0013(9) -0.0003(9)
C30 0.0244(11) 0.0323(12) 0.0364(12) -0.0061(10) -0.0053(9) 0.0021(9)
O1A 0.0265(8) 0.0300(8) 0.0175(7) -0.0050(6) 0.0005(6) 0.0009(6)
C1A 0.0208(10) 0.0233(10) 0.0195(10) -0.0038(8) 0.0008(8) 0.0009(8)
C2A 0.0250(11) 0.0250(11) 0.0250(10) -0.0050(9) -0.0026(8) -0.0003(9)
C3A 0.0252(11) 0.0244(11) 0.0309(11) -0.0035(9) 0.0037(9) -0.0038(9)
C4A 0.0311(12) 0.0279(12) 0.0305(12) 0.0047(9) 0.0054(9) -0.0030(10)
C5A 0.0295(12) 0.0315(12) 0.0237(11) 0.0013(9) 0.0002(9) 0.0024(9)
C6A 0.0250(11) 0.0225(11) 0.0219(10) -0.0050(8) 0.0008(8) 0.0020(8)
C7A 0.0229(10) 0.0251(11) 0.0216(10) -0.0056(8) -0.0005(8) 0.0014(8)
C8A 0.0285(11) 0.0306(12) 0.0211(10) -0.0011(9) -0.0049(8) 0.0036(9)
C9A 0.0253(11) 0.0361(12) 0.0247(11) -0.0080(9) -0.0082(9) 0.0028(9)
C10A 0.0197(10) 0.0312(12) 0.0245(10) -0.0108(9) -0.0028(8) 0.0047(9)
C11A 0.0210(10) 0.0282(11) 0.0186(9) -0.0050(8) -0.0009(8) 0.0005(8)
C12A 0.0210(10) 0.0259(11) 0.0182(9) -0.0055(8) -0.0015(8) 0.0022(8)
C13A 0.0199(10) 0.0243(10) 0.0176(9) -0.0042(8) 0.0006(7) -0.0024(8)
C14A 0.0168(9) 0.0230(10) 0.0183(9) 0.0000(8) -0.0002(7) -0.0050(8)
C15A 0.0191(10) 0.0286(11) 0.0196(10) -0.0020(8) -0.0012(8) -0.0057(8)
C16A 0.0245(11) 0.0311(12) 0.0213(10) 0.0024(9) -0.0055(8) -0.0062(9)
C17A 0.0273(11) 0.0272(12) 0.0286(11) -0.0006(9) -0.0041(9) 0.0015(9)
C18A 0.0285(11) 0.0290(12) 0.0209(10) -0.0044(9) -0.0020(8) -0.0010(9)
C19A 0.0175(9) 0.0259(11) 0.0189(9) 0.0002(8) -0.0002(7) -0.0036(8)
C20A 0.0218(10) 0.0240(11) 0.0194(10) -0.0026(8) -0.0003(8) 0.0026(8)
C21A 0.0216(10) 0.0252(11) 0.0200(10) -0.0021(8) 0.0016(8) -0.0030(8)
C22A 0.0185(10) 0.0277(11) 0.0213(10) -0.0059(8) -0.0017(8) -0.0002(8)
C23A 0.0307(12) 0.0314(13) 0.0468(14) -0.0027(11) 0.0000(10) -0.0107(10)
C24A 0.0269(13) 0.0604(18) 0.0566(17) 0.0076(14) 0.0035(12) -0.0083(12)
C25A 0.0362(14) 0.0590(17) 0.0522(16) -0.0031(13) -0.0099(12) -0.0232(13)
C26A 0.0577(19) 0.0373(16) 0.104(3) -0.0139(16) -0.0206(17) -0.0126(14)
C27A 0.0261(11) 0.0333(12) 0.0281(11) -0.0087(9) -0.0055(9) -0.0001(9)
C28A 0.0231(11) 0.0443(14) 0.0374(13) -0.0088(11) -0.0022(9) -0.0082(10)
C29A 0.0292(12) 0.0484(15) 0.0413(14) -0.0087(11) -0.0115(10) -0.0053(11)
C30A 0.0367(13) 0.0369(13) 0.0441(14) -0.0130(11) -0.0106(11) -0.0038(11)
O1B 0.0265(8) 0.0276(8) 0.0302(8) -0.0016(6) -0.0009(6) -0.0063(6)
C1B 0.0244(11) 0.0267(11) 0.0325(11) -0.0021(9) -0.0084(9) -0.0023(9)
C2B 0.0246(11) 0.0333(13) 0.0403(13) 0.0035(10) -0.0023(9) -0.0037(10)
C3B 0.0262(11) 0.0290(12) 0.0439(13) 0.0046(10) -0.0054(10) -0.0047(9)
C4B 0.0328(12) 0.0272(12) 0.0411(13) -0.0071(10) -0.0048(10) -0.0057(10)
O1C 0.0470(10) 0.0382(9) 0.0335(9) -0.0068(7) -0.0125(7) 0.0100(8)
C1C 0.0353(13) 0.0341(13) 0.0303(12) -0.0043(10) -0.0033(10) 0.0016(10)
C2C 0.0376(13) 0.0345(13) 0.0315(12) -0.0010(10) -0.0024(10) 0.0044(10)
C3C 0.076(2) 0.0552(17) 0.0378(15) -0.0128(13) 0.0040(14) -0.0298(16)
C4C 0.0502(17) 0.0376(15) 0.102(2) -0.0273(16) -0.0368(16) 0.0102(13)
_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
O1 C13 1.433(2) . ?
O1 H1 0.8400 . ?
C1 C2 1.380(3) . ?
C1 C6 1.395(2) . ?
C1 C13 1.530(2) . ?
C2 C3 1.400(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.401(3) . ?
C3 C23 1.532(3) . ?
C4 C5 1.380(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.470(3) . ?
C7 C8 1.380(3) . ?
C7 C12 1.403(2) . ?
C8 C9 1.391(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.396(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.406(2) . ?
C10 C27 1.531(3) . ?
C11 C12 1.375(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.523(2) . ?
C13 C14 1.527(2) . ?
C14 C15 1.395(2) . ?
C14 C19 1.403(3) . ?
C15 C16 1.388(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.370(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.386(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.395(2) . ?
C18 H18 0.9500 . ?
C19 C21 1.501(2) . ?
C20 C22 1.384(2) 2_656 ?
C20 C21 1.387(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.393(3) . ?
C22 C20 1.384(2) 2_656 ?
C22 H22 0.9500 . ?
C23 C24 1.529(3) . ?
C23 C26 1.534(3) . ?
C23 C25 1.536(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C29 1.527(3) . ?
C27 C28 1.531(3) . ?
C27 C30 1.537(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
O1A C13A 1.430(2) . ?
O1A H1A 0.8400 . ?
C1A C2A 1.382(3) . ?
C1A C6A 1.394(3) . ?
C1A C13A 1.528(2) . ?
C2A C3A 1.395(3) . ?
C2A H2A 0.9500 . ?
C3A C4A 1.400(3) . ?
C3A C23A 1.530(3) . ?
C4A C5A 1.384(3) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.383(3) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.467(3) . ?
C7A C8A 1.383(3) . ?
C7A C12A 1.399(3) . ?
C8A C9A 1.388(3) . ?
C8A H8A 0.9500 . ?
C9A C10A 1.394(3) . ?
C9A H9A 0.9500 . ?
C10A C11A 1.401(3) . ?
C10A C27A 1.532(3) . ?
C11A C12A 1.380(3) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.527(3) . ?
C13A C14A 1.525(3) . ?
C14A C15A 1.393(3) . ?
C14A C19A 1.407(3) . ?
C15A C16A 1.381(3) . ?
C15A H15A 0.9500 . ?
C16A C17A 1.379(3) . ?
C16A H16A 0.9500 . ?
C17A C18A 1.390(3) . ?
C17A H17A 0.9500 . ?
C18A C19A 1.388(3) . ?
C18A H18A 0.9500 . ?
C19A C20A 1.500(3) . ?
C20A C21A 1.389(3) . ?
C20A C22A 1.394(3) 2_765 ?
C21A C22A 1.386(3) . ?
C21A H21A 0.9500 . ?
C22A C20A 1.394(3) 2_765 ?
C22A H22A 0.9500 . ?
C23A C25A 1.522(3) . ?
C23A C26A 1.523(3) . ?
C23A C24A 1.528(3) . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
C25A H25D 0.9800 . ?
C25A H25E 0.9800 . ?
C25A H25F 0.9800 . ?
C26A H26D 0.9800 . ?
C26A H26E 0.9800 . ?
C26A H26F 0.9800 . ?
C27A C28A 1.532(3) . ?
C27A C29A 1.532(3) . ?
C27A C30A 1.540(3) . ?
C28A H28D 0.9800 . ?
C28A H28E 0.9800 . ?
C28A H28F 0.9800 . ?
C29A H29D 0.9800 . ?
C29A H29E 0.9800 . ?
C29A H29F 0.9800 . ?
C30A H30D 0.9800 . ?
C30A H30E 0.9800 . ?
C30A H30F 0.9800 . ?
O1B C4B 1.438(2) . ?
O1B C1B 1.445(2) . ?
C1B C2B 1.518(3) . ?
C1B H1B1 0.9900 . ?
C1B H1B2 0.9900 . ?
C2B C3B 1.520(3) . ?
C2B H2B1 0.9900 . ?
C2B H2B2 0.9900 . ?
C3B C4B 1.507(3) . ?
C3B H3B1 0.9900 . ?
C3B H3B2 0.9900 . ?
C4B H4B1 0.9900 . ?
C4B H4B2 0.9900 . ?
O1C C4C 1.425(3) . ?
O1C C1C 1.426(3) . ?
C1C C2C 1.509(3) . ?
C1C H1C1 0.9900 . ?
C1C H1C2 0.9900 . ?
C2C C3C 1.509(3) . ?
C2C H2C1 0.9900 . ?
C2C H2C2 0.9900 . ?
C3C C4C 1.486(4) . ?
C3C H3C1 0.9900 . ?
C3C H3C2 0.9900 . ?
C4C H4C1 0.9900 . ?
C4C H4C2 0.9900 . ?
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
C13 O1 H1 109.5 . . ?
C2 C1 C6 121.97(16) . . ?
C2 C1 C13 127.38(15) . . ?
C6 C1 C13 110.63(16) . . ?
C1 C2 C3 119.80(16) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C2 C3 C4 117.47(17) . . ?
C2 C3 C23 123.02(16) . . ?
C4 C3 C23 119.47(16) . . ?
C5 C4 C3 122.84(17) . . ?
C5 C4 H4 118.6 . . ?
C3 C4 H4 118.6 . . ?
C4 C5 C6 119.07(17) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C5 C6 C1 118.84(17) . . ?
C5 C6 C7 132.37(17) . . ?
C1 C6 C7 108.75(15) . . ?
C8 C7 C12 119.29(17) . . ?
C8 C7 C6 132.11(16) . . ?
C12 C7 C6 108.51(15) . . ?
C7 C8 C9 119.25(16) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C8 C9 C10 122.37(17) . . ?
C8 C9 H9 118.8 . . ?
C10 C9 H9 118.8 . . ?
C9 C10 C11 117.52(17) . . ?
C9 C10 C27 123.03(16) . . ?
C11 C10 C27 119.45(16) . . ?
C12 C11 C10 120.33(16) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C7 121.22(17) . . ?
C11 C12 C13 128.17(16) . . ?
C7 C12 C13 110.60(16) . . ?
O1 C13 C12 111.05(15) . . ?
O1 C13 C14 107.76(13) . . ?
C12 C13 C14 113.45(15) . . ?
O1 C13 C1 110.97(14) . . ?
C12 C13 C1 101.45(13) . . ?
C14 C13 C1 112.16(15) . . ?
C15 C14 C19 118.60(17) . . ?
C15 C14 C13 119.27(17) . . ?
C19 C14 C13 122.13(15) . . ?
C16 C15 C14 121.12(18) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C17 C16 C15 120.45(17) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 119.16(18) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
C17 C18 C19 121.57(18) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 H18 119.2 . . ?
C18 C19 C14 119.10(16) . . ?
C18 C19 C21 116.69(16) . . ?
C14 C19 C21 124.20(16) . . ?
C22 C20 C21 120.80(17) 2_656 . ?
C22 C20 H20 119.6 2_656 . ?
C21 C20 H20 119.6 . . ?
C20 C21 C22 118.58(16) . . ?
C20 C21 C19 121.07(16) . . ?
C22 C21 C19 120.28(16) . . ?
C20 C22 C21 120.61(17) 2_656 . ?
C20 C22 H22 119.7 2_656 . ?
C21 C22 H22 119.7 . . ?
C24 C23 C3 112.31(15) . . ?
C24 C23 C26 108.35(17) . . ?
C3 C23 C26 109.66(16) . . ?
C24 C23 C25 108.30(16) . . ?
C3 C23 C25 108.91(16) . . ?
C26 C23 C25 109.26(16) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C29 C27 C10 109.46(16) . . ?
C29 C27 C28 108.65(17) . . ?
C10 C27 C28 112.69(15) . . ?
C29 C27 C30 109.26(16) . . ?
C10 C27 C30 109.23(16) . . ?
C28 C27 C30 107.49(17) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C13A O1A H1A 109.5 . . ?
C2A C1A C6A 121.74(18) . . ?
C2A C1A C13A 127.35(18) . . ?
C6A C1A C13A 110.90(17) . . ?
C1A C2A C3A 119.58(19) . . ?
C1A C2A H2A 120.2 . . ?
C3A C2A H2A 120.2 . . ?
C2A C3A C4A 118.01(19) . . ?
C2A C3A C23A 122.7(2) . . ?
C4A C3A C23A 119.25(18) . . ?
C5A C4A C3A 122.34(18) . . ?
C5A C4A H4A 118.8 . . ?
C3A C4A H4A 118.8 . . ?
C6A C5A C4A 119.0(2) . . ?
C6A C5A H5A 120.5 . . ?
C4A C5A H5A 120.5 . . ?
C5A C6A C1A 119.23(19) . . ?
C5A C6A C7A 132.0(2) . . ?
C1A C6A C7A 108.75(17) . . ?
C8A C7A C12A 119.31(18) . . ?
C8A C7A C6A 132.22(18) . . ?
C12A C7A C6A 108.43(17) . . ?
C7A C8A C9A 119.19(19) . . ?
C7A C8A H8A 120.4 . . ?
C9A C8A H8A 120.4 . . ?
C8A C9A C10A 122.37(19) . . ?
C8A C9A H9A 118.8 . . ?
C10A C9A H9A 118.8 . . ?
C9A C10A C11A 117.76(18) . . ?
C9A C10A C27A 121.93(18) . . ?
C11A C10A C27A 120.22(18) . . ?
C12A C11A C10A 120.20(18) . . ?
C12A C11A H11A 119.9 . . ?
C10A C11A H11A 119.9 . . ?
C11A C12A C7A 121.17(19) . . ?
C11A C12A C13A 127.94(17) . . ?
C7A C12A C13A 110.89(16) . . ?
O1A C13A C14A 107.24(15) . . ?
O1A C13A C12A 111.76(15) . . ?
C14A C13A C12A 112.94(16) . . ?
O1A C13A C1A 110.68(15) . . ?
C14A C13A C1A 113.22(15) . . ?
C12A C13A C1A 101.03(15) . . ?
C15A C14A C19A 118.45(18) . . ?
C15A C14A C13A 118.85(17) . . ?
C19A C14A C13A 122.70(16) . . ?
C16A C15A C14A 121.50(19) . . ?
C16A C15A H15A 119.3 . . ?
C14A C15A H15A 119.3 . . ?
C17A C16A C15A 120.28(19) . . ?
C17A C16A H16A 119.9 . . ?
C15A C16A H16A 119.9 . . ?
C16A C17A C18A 118.8(2) . . ?
C16A C17A H17A 120.6 . . ?
C18A C17A H17A 120.6 . . ?
C19A C18A C17A 121.74(19) . . ?
C19A C18A H18A 119.1 . . ?
C17A C18A H18A 119.1 . . ?
C18A C19A C14A 119.08(17) . . ?
C18A C19A C20A 116.90(17) . . ?
C14A C19A C20A 124.01(18) . . ?
C21A C20A C22A 118.27(17) . 2_765 ?
C21A C20A C19A 121.19(17) . . ?
C22A C20A C19A 120.48(18) 2_765 . ?
C22A C21A C20A 121.01(17) . . ?
C22A C21A H21A 119.5 . . ?
C20A C21A H21A 119.5 . . ?
C21A C22A C20A 120.72(18) . 2_765 ?
C21A C22A H22A 119.6 . . ?
C20A C22A H22A 119.6 2_765 . ?
C25A C23A C26A 108.6(2) . . ?
C25A C23A C24A 109.1(2) . . ?
C26A C23A C24A 109.3(2) . . ?
C25A C23A C3A 112.31(18) . . ?
C26A C23A C3A 109.0(2) . . ?
C24A C23A C3A 108.5(2) . . ?
C23A C24A H24D 109.5 . . ?
C23A C24A H24E 109.5 . . ?
H24D C24A H24E 109.5 . . ?
C23A C24A H24F 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
C23A C25A H25D 109.5 . . ?
C23A C25A H25E 109.5 . . ?
H25D C25A H25E 109.5 . . ?
C23A C25A H25F 109.5 . . ?
H25D C25A H25F 109.5 . . ?
H25E C25A H25F 109.5 . . ?
C23A C26A H26D 109.5 . . ?
C23A C26A H26E 109.5 . . ?
H26D C26A H26E 109.5 . . ?
C23A C26A H26F 109.5 . . ?
H26D C26A H26F 109.5 . . ?
H26E C26A H26F 109.5 . . ?
C10A C27A C28A 110.80(17) . . ?
C10A C27A C29A 112.70(18) . . ?
C28A C27A C29A 107.38(17) . . ?
C10A C27A C30A 108.17(17) . . ?
C28A C27A C30A 109.62(18) . . ?
C29A C27A C30A 108.11(18) . . ?
C27A C28A H28D 109.5 . . ?
C27A C28A H28E 109.5 . . ?
H28D C28A H28E 109.5 . . ?
C27A C28A H28F 109.5 . . ?
H28D C28A H28F 109.5 . . ?
H28E C28A H28F 109.5 . . ?
C27A C29A H29D 109.5 . . ?
C27A C29A H29E 109.5 . . ?
H29D C29A H29E 109.5 . . ?
C27A C29A H29F 109.5 . . ?
H29D C29A H29F 109.5 . . ?
H29E C29A H29F 109.5 . . ?
C27A C30A H30D 109.5 . . ?
C27A C30A H30E 109.5 . . ?
H30D C30A H30E 109.5 . . ?
C27A C30A H30F 109.5 . . ?
H30D C30A H30F 109.5 . . ?
H30E C30A H30F 109.5 . . ?
C4B O1B C1B 109.19(15) . . ?
O1B C1B C2B 106.42(16) . . ?
O1B C1B H1B1 110.4 . . ?
C2B C1B H1B1 110.4 . . ?
O1B C1B H1B2 110.4 . . ?
C2B C1B H1B2 110.4 . . ?
H1B1 C1B H1B2 108.6 . . ?
C1B C2B C3B 102.41(17) . . ?
C1B C2B H2B1 111.3 . . ?
C3B C2B H2B1 111.3 . . ?
C1B C2B H2B2 111.3 . . ?
C3B C2B H2B2 111.3 . . ?
H2B1 C2B H2B2 109.2 . . ?
C4B C3B C2B 102.11(17) . . ?
C4B C3B H3B1 111.3 . . ?
C2B C3B H3B1 111.3 . . ?
C4B C3B H3B2 111.3 . . ?
C2B C3B H3B2 111.3 . . ?
H3B1 C3B H3B2 109.2 . . ?
O1B C4B C3B 106.00(17) . . ?
O1B C4B H4B1 110.5 . . ?
C3B C4B H4B1 110.5 . . ?
O1B C4B H4B2 110.5 . . ?
C3B C4B H4B2 110.5 . . ?
H4B1 C4B H4B2 108.7 . . ?
C4C O1C C1C 107.66(18) . . ?
O1C C1C C2C 106.16(18) . . ?
O1C C1C H1C1 110.5 . . ?
C2C C1C H1C1 110.5 . . ?
O1C C1C H1C2 110.5 . . ?
C2C C1C H1C2 110.5 . . ?
H1C1 C1C H1C2 108.7 . . ?
C1C C2C C3C 104.15(19) . . ?
C1C C2C H2C1 110.9 . . ?
C3C C2C H2C1 110.9 . . ?
C1C C2C H2C2 110.9 . . ?
C3C C2C H2C2 110.9 . . ?
H2C1 C2C H2C2 108.9 . . ?
C4C C3C C2C 106.0(2) . . ?
C4C C3C H3C1 110.5 . . ?
C2C C3C H3C1 110.5 . . ?
C4C C3C H3C2 110.5 . . ?
C2C C3C H3C2 110.5 . . ?
H3C1 C3C H3C2 108.7 . . ?
O1C C4C C3C 107.7(2) . . ?
O1C C4C H4C1 110.2 . . ?
C3C C4C H4C1 110.2 . . ?
O1C C4C H4C2 110.2 . . ?
C3C C4C H4C2 110.2 . . ?
H4C1 C4C H4C2 108.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.8(3) . . . . ?
C13 C1 C2 C3 -177.38(17) . . . . ?
C1 C2 C3 C4 -0.5(3) . . . . ?
C1 C2 C3 C23 177.21(17) . . . . ?
C2 C3 C4 C5 -0.4(3) . . . . ?
C23 C3 C4 C5 -178.20(18) . . . . ?
C3 C4 C5 C6 1.0(3) . . . . ?
C4 C5 C6 C1 -0.6(3) . . . . ?
C4 C5 C6 C7 176.54(19) . . . . ?
C2 C1 C6 C5 -0.3(3) . . . . ?
C13 C1 C6 C5 178.22(16) . . . . ?
C2 C1 C6 C7 -178.05(17) . . . . ?
C13 C1 C6 C7 0.4(2) . . . . ?
C5 C6 C7 C8 0.2(4) . . . . ?
C1 C6 C7 C8 177.6(2) . . . . ?
C5 C6 C7 C12 -176.1(2) . . . . ?
C1 C6 C7 C12 1.3(2) . . . . ?
C12 C7 C8 C9 0.5(3) . . . . ?
C6 C7 C8 C9 -175.50(19) . . . . ?
C7 C8 C9 C10 0.4(3) . . . . ?
C8 C9 C10 C11 -1.6(3) . . . . ?
C8 C9 C10 C27 177.80(18) . . . . ?
C9 C10 C11 C12 1.8(3) . . . . ?
C27 C10 C11 C12 -177.57(17) . . . . ?
C10 C11 C12 C7 -1.0(3) . . . . ?
C10 C11 C12 C13 178.00(18) . . . . ?
C8 C7 C12 C11 -0.2(3) . . . . ?
C6 C7 C12 C11 176.65(17) . . . . ?
C8 C7 C12 C13 -179.36(16) . . . . ?
C6 C7 C12 C13 -2.5(2) . . . . ?
C11 C12 C13 O1 65.5(2) . . . . ?
C7 C12 C13 O1 -115.40(16) . . . . ?
C11 C12 C13 C14 -56.0(3) . . . . ?
C7 C12 C13 C14 123.06(17) . . . . ?
C11 C12 C13 C1 -176.48(18) . . . . ?
C7 C12 C13 C1 2.58(19) . . . . ?
C2 C1 C13 O1 -65.4(2) . . . . ?
C6 C1 C13 O1 116.26(16) . . . . ?
C2 C1 C13 C12 176.60(18) . . . . ?
C6 C1 C13 C12 -1.77(19) . . . . ?
C2 C1 C13 C14 55.2(2) . . . . ?
C6 C1 C13 C14 -123.16(17) . . . . ?
O1 C13 C14 C15 0.0(2) . . . . ?
C12 C13 C14 C15 123.32(18) . . . . ?
C1 C13 C14 C15 -122.46(18) . . . . ?
O1 C13 C14 C19 178.93(16) . . . . ?
C12 C13 C14 C19 -57.7(2) . . . . ?
C1 C13 C14 C19 56.5(2) . . . . ?
C19 C14 C15 C16 -0.6(3) . . . . ?
C13 C14 C15 C16 178.43(17) . . . . ?
C14 C15 C16 C17 -0.2(3) . . . . ?
C15 C16 C17 C18 0.7(3) . . . . ?
C16 C17 C18 C19 -0.4(3) . . . . ?
C17 C18 C19 C14 -0.3(3) . . . . ?
C17 C18 C19 C21 -179.46(18) . . . . ?
C15 C14 C19 C18 0.8(3) . . . . ?
C13 C14 C19 C18 -178.18(17) . . . . ?
C15 C14 C19 C21 179.88(17) . . . . ?
C13 C14 C19 C21 0.9(3) . . . . ?
C22 C20 C21 C22 0.9(3) 2_656 . . . ?
C22 C20 C21 C19 177.95(17) 2_656 . . . ?
C18 C19 C21 C20 -92.4(2) . . . . ?
C14 C19 C21 C20 88.5(2) . . . . ?
C18 C19 C21 C22 84.6(2) . . . . ?
C14 C19 C21 C22 -94.5(2) . . . . ?
C20 C21 C22 C20 -0.9(3) . . . 2_656 ?
C19 C21 C22 C20 -177.97(17) . . . 2_656 ?
C2 C3 C23 C24 1.4(3) . . . . ?
C4 C3 C23 C24 178.99(17) . . . . ?
C2 C3 C23 C26 121.90(19) . . . . ?
C4 C3 C23 C26 -60.5(2) . . . . ?
C2 C3 C23 C25 -118.58(19) . . . . ?
C4 C3 C23 C25 59.0(2) . . . . ?
C9 C10 C27 C29 116.8(2) . . . . ?
C11 C10 C27 C29 -63.9(2) . . . . ?
C9 C10 C27 C28 -4.2(3) . . . . ?
C11 C10 C27 C28 175.10(18) . . . . ?
C9 C10 C27 C30 -123.6(2) . . . . ?
C11 C10 C27 C30 55.7(2) . . . . ?
C6A C1A C2A C3A -1.1(3) . . . . ?
C13A C1A C2A C3A 178.86(18) . . . . ?
C1A C2A C3A C4A -1.1(3) . . . . ?
C1A C2A C3A C23A 178.92(19) . . . . ?
C2A C3A C4A C5A 2.0(3) . . . . ?
C23A C3A C4A C5A -178.0(2) . . . . ?
C3A C4A C5A C6A -0.6(3) . . . . ?
C4A C5A C6A C1A -1.6(3) . . . . ?
C4A C5A C6A C7A -179.2(2) . . . . ?
C2A C1A C6A C5A 2.5(3) . . . . ?
C13A C1A C6A C5A -177.51(17) . . . . ?
C2A C1A C6A C7A -179.36(17) . . . . ?
C13A C1A C6A C7A 0.7(2) . . . . ?
C5A C6A C7A C8A -0.5(4) . . . . ?
C1A C6A C7A C8A -178.3(2) . . . . ?
C5A C6A C7A C12A 177.4(2) . . . . ?
C1A C6A C7A C12A -0.4(2) . . . . ?
C12A C7A C8A C9A 0.4(3) . . . . ?
C6A C7A C8A C9A 178.1(2) . . . . ?
C7A C8A C9A C10A 0.1(3) . . . . ?
C8A C9A C10A C11A -0.1(3) . . . . ?
C8A C9A C10A C27A -176.69(19) . . . . ?
C9A C10A C11A C12A -0.2(3) . . . . ?
C27A C10A C11A C12A 176.38(18) . . . . ?
C10A C11A C12A C7A 0.7(3) . . . . ?
C10A C11A C12A C13A -178.17(18) . . . . ?
C8A C7A C12A C11A -0.8(3) . . . . ?
C6A C7A C12A C11A -178.99(18) . . . . ?
C8A C7A C12A C13A 178.26(17) . . . . ?
C6A C7A C12A C13A 0.1(2) . . . . ?
C11A C12A C13A O1A -63.0(3) . . . . ?
C7A C12A C13A O1A 118.03(17) . . . . ?
C11A C12A C13A C14A 58.0(2) . . . . ?
C7A C12A C13A C14A -120.94(17) . . . . ?
C11A C12A C13A C1A 179.27(19) . . . . ?
C7A C12A C13A C1A 0.3(2) . . . . ?
C2A C1A C13A O1A 60.9(2) . . . . ?
C6A C1A C13A O1A -119.09(18) . . . . ?
C2A C1A C13A C14A -59.5(3) . . . . ?
C6A C1A C13A C14A 120.46(18) . . . . ?
C2A C1A C13A C12A 179.43(19) . . . . ?
C6A C1A C13A C12A -0.6(2) . . . . ?
O1A C13A C14A C15A -8.3(2) . . . . ?
C12A C13A C14A C15A -131.87(18) . . . . ?
C1A C13A C14A C15A 114.08(19) . . . . ?
O1A C13A C14A C19A 171.93(16) . . . . ?
C12A C13A C14A C19A 48.4(2) . . . . ?
C1A C13A C14A C19A -65.7(2) . . . . ?
C19A C14A C15A C16A -2.2(3) . . . . ?
C13A C14A C15A C16A 178.02(17) . . . . ?
C14A C15A C16A C17A -0.6(3) . . . . ?
C15A C16A C17A C18A 1.6(3) . . . . ?
C16A C17A C18A C19A 0.3(3) . . . . ?
C17A C18A C19A C14A -3.1(3) . . . . ?
C17A C18A C19A C20A 175.78(18) . . . . ?
C15A C14A C19A C18A 4.0(3) . . . . ?
C13A C14A C19A C18A -176.26(17) . . . . ?
C15A C14A C19A C20A -174.80(17) . . . . ?
C13A C14A C19A C20A 5.0(3) . . . . ?
C18A C19A C20A C21A 78.9(2) . . . . ?
C14A C19A C20A C21A -102.3(2) . . . . ?
C18A C19A C20A C22A -98.2(2) . . . 2_765 ?
C14A C19A C20A C22A 80.6(2) . . . 2_765 ?
C22A C20A C21A C22A -0.9(3) 2_765 . . . ?
C19A C20A C21A C22A -177.97(18) . . . . ?
C20A C21A C22A C20A 0.9(3) . . . 2_765 ?
C2A C3A C23A C25A -1.4(3) . . . . ?
C4A C3A C23A C25A 178.6(2) . . . . ?
C2A C3A C23A C26A -121.8(2) . . . . ?
C4A C3A C23A C26A 58.2(3) . . . . ?
C2A C3A C23A C24A 119.3(2) . . . . ?
C4A C3A C23A C24A -60.7(3) . . . . ?
C9A C10A C27A C28A -135.5(2) . . . . ?
C11A C10A C27A C28A 48.0(3) . . . . ?
C9A C10A C27A C29A -15.1(3) . . . . ?
C11A C10A C27A C29A 168.38(18) . . . . ?
C9A C10A C27A C30A 104.3(2) . . . . ?
C11A C10A C27A C30A -72.2(2) . . . . ?
C4B O1B C1B C2B -6.3(2) . . . . ?
O1B C1B C2B C3B 26.9(2) . . . . ?
C1B C2B C3B C4B -36.3(2) . . . . ?
C1B O1B C4B C3B -17.4(2) . . . . ?
C2B C3B C4B O1B 33.6(2) . . . . ?
C4C O1C C1C C2C 30.1(2) . . . . ?
O1C C1C C2C C3C -23.8(2) . . . . ?
C1C C2C C3C C4C 9.2(3) . . . . ?
C1C O1C C4C C3C -24.2(3) . . . . ?
C2C C3C C4C O1C 8.5(3) . . . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 27.80
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.301
_refine_diff_density_min -0.251
_refine_diff_density_rms 0.049