# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_publication_text _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _publ_contact_author_name 'Michel Geoffroy' _publ_contact_author_address ;Department of Physical Chemistry, University of Geneva 30 Quai Ernest Ansermet, CH-1211 Geneva, Switzerland ; _publ_contact_author_email michel.geoffroy@unige.ch loop_ _publ_author_name _publ_author_address 'Michel Geoffroy' ;Department of Physical Chemistry, University of Geneva 30 Quai Ernest Ansermet, CH-1211 Geneva, Switzerland ; "Th\'eo Berclaz" ;Department of Physical Chemistry, University of Geneva 30 Quai Ernest Ansermet, CH-1211 Geneva, Switzerland ; C.Besnard ;Department of Physical Chemistry, University of Geneva 30 Quai Ernest Ansermet, CH-1211 Geneva, Switzerland ; data_1 _database_code_depnum_ccdc_archive 'CCDC 815021' #TrackingRef 'elineBesnard_1298972567.cif' _exptl_special_details ; ; _refine_special_details ; H hydrogen were placed geometrically and allowed to ride on their delonging atom after a few cycle of heavily restrained refinemenrt. ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 9.834(5) _cell_length_b 10.871(5) _cell_length_c 25.800(10) _cell_angle_alpha 88.42(2) _cell_angle_beta 83.77(2) _cell_angle_gamma 79.06(2) _cell_volume 2692(2) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C64 H5 P2 # Dc = 1.03 Fooo = 980.00 Mu = 1.16 M = 835.69 # Found Formula = C64 H76 P2 # Dc = 1.12 FOOO = 980.00 Mu = 1.19 M = 907.25 _chemical_formula_sum 'C64 H76 P2' _chemical_formula_moiety 'C64 H76 P2' _chemical_compound_source ? _chemical_formula_weight 907.25 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 100 _exptl_crystal_description 'elongated platelets' _exptl_crystal_colour yellow _exptl_crystal_size_min 0.010 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 1.119 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 0.119 # Sheldrick geometric approximatio 0.99 0.99 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_measurement_device mar345 _diffrn_measurement_device_type Serial _diffrn_radiation_monochromator graphite _diffrn_source synchrotron _diffrn_radiation_wavelength 0.70000 _diffrn_measurement_method '\f scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'CRYSALIS (oxford diffraction)' _computing_data_reduction 'CRYSALIS (Oxford diffraction)' _computing_structure_solution 'Sir2004 (Burla et al., 2005)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 100 _diffrn_reflns_number 18200 _reflns_number_total 8700 _diffrn_reflns_av_R_equivalents 0.028 # Number of reflections with Friedels Law is 8725 # Number of reflections without Friedels Law is 15415 # Theoretical number of reflections is about 9387 _diffrn_reflns_theta_min 1.564 _diffrn_reflns_theta_max 24.508 _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 24.508 _diffrn_measured_fraction_theta_full 0.928 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -12 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _oxford_diffrn_Wilson_B_factor 0.99 _oxford_diffrn_Wilson_scale 0.02 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.72 _refine_diff_density_max 0.57 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 8700 _refine_ls_number_restraints 0 _refine_ls_number_parameters 595 _oxford_refine_ls_R_factor_ref 0.0748 _refine_ls_wR_factor_ref 0.0941 _refine_ls_goodness_of_fit_ref 1.1263 _refine_ls_shift/su_max 0.0007379 # The values computed from all data _oxford_reflns_number_all 8700 _refine_ls_R_factor_all 0.0748 _refine_ls_wR_factor_all 0.0941 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6992 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_gt 0.0933 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.169E+04 0.196E+04 572. ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined data collection reference User defined data reduction User defined cell refinement Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Burla, M. C. , Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., D Caro, L. , Giacovazzo, C., Polidori, G., & Spagna R. J. Appl. Cryst. (2005). 381-388. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens P1b P 0.48494(9) 1.03296(8) 0.76009(3) 0.0170 1.0000 Uani . . . . . . . C1b C 0.4622(3) 1.1595(3) 0.72131(12) 0.0152 1.0000 Uani . . . . . . . C2b C 0.3940(3) 1.1650(3) 0.67345(11) 0.0149 1.0000 Uani . . . . . . . C3b C 0.4246(3) 1.2468(3) 0.63236(12) 0.0153 1.0000 Uani . . . . . . . C4b C 0.3601(3) 1.2519(3) 0.58691(12) 0.0168 1.0000 Uani . . . . . . . C5b C 0.2629(3) 1.1760(3) 0.58048(11) 0.0138 1.0000 Uani . . . . . . . C8b C 0.1918(3) 1.1832(3) 0.53208(11) 0.0149 1.0000 Uani . . . . . . . C15b C 0.1916(3) 1.0712(3) 0.50304(11) 0.0138 1.0000 Uani . . . . . . . C13 C 0.2624(3) 0.9530(3) 0.51696(11) 0.0140 1.0000 Uani . . . . . . . C15a C 0.2636(3) 0.8446(3) 0.48885(11) 0.0125 1.0000 Uani . . . . . . . C14a C 0.1859(3) 0.8556(3) 0.44413(11) 0.0145 1.0000 Uani . . . . . . . C12 C 0.1172(3) 0.9747(3) 0.42956(11) 0.0159 1.0000 Uani . . . . . . . C14b C 0.1188(3) 1.0829(3) 0.45738(11) 0.0145 1.0000 Uani . . . . . . . C11b C 0.0491(3) 1.2036(3) 0.44190(12) 0.0178 1.0000 Uani . . . . . . . C10b C 0.0546(3) 1.3072(3) 0.46899(12) 0.0196 1.0000 Uani . . . . . . . C9b C 0.1273(3) 1.2970(3) 0.51400(12) 0.0167 1.0000 Uani . . . . . . . C11a C 0.1792(3) 0.7451(3) 0.41652(12) 0.0188 1.0000 Uani . . . . . . . C10a C 0.2429(3) 0.6307(3) 0.43264(12) 0.0180 1.0000 Uani . . . . . . . C9a C 0.3194(3) 0.6185(3) 0.47660(12) 0.0168 1.0000 Uani . . . . . . . C8a C 0.3325(3) 0.7212(3) 0.50441(12) 0.0139 1.0000 Uani . . . . . . . C5a C 0.4162(3) 0.7032(3) 0.54978(11) 0.0138 1.0000 Uani . . . . . . . C6a C 0.3959(3) 0.6113(3) 0.58758(12) 0.0149 1.0000 Uani . . . . . . . C7a C 0.4734(3) 0.5929(3) 0.62991(12) 0.0163 1.0000 Uani . . . . . . . C2a C 0.5739(3) 0.6650(3) 0.63658(12) 0.0147 1.0000 Uani . . . . . . . C3a C 0.5924(3) 0.7581(3) 0.59921(12) 0.0160 1.0000 Uani . . . . . . . C4a C 0.5166(3) 0.7753(3) 0.55632(12) 0.0150 1.0000 Uani . . . . . . . C1a C 0.6570(3) 0.6451(3) 0.68098(12) 0.0161 1.0000 Uani . . . . . . . P1a P 0.70044(9) 0.50603(8) 0.71050(3) 0.0158 1.0000 Uani . . . . . . . C16a C 0.7851(3) 0.5455(3) 0.76719(11) 0.0128 1.0000 Uani . . . . . . . C21a C 0.7009(3) 0.5775(3) 0.81504(12) 0.0145 1.0000 Uani . . . . . . . C20a C 0.7647(3) 0.6127(3) 0.85685(12) 0.0144 1.0000 Uani . . . . . . . C19a C 0.9058(3) 0.6131(3) 0.85471(11) 0.0143 1.0000 Uani . . . . . . . C18a C 0.9865(3) 0.5767(3) 0.80803(12) 0.0144 1.0000 Uani . . . . . . . C17a C 0.9310(3) 0.5408(3) 0.76421(11) 0.0121 1.0000 Uani . . . . . . . C22a C 1.0363(3) 0.4973(3) 0.71573(12) 0.0147 1.0000 Uani . . . . . . . C220a C 1.0194(4) 0.5937(3) 0.67071(13) 0.0237 1.0000 Uani . . . . . . . C221a C 1.0212(4) 0.3684(3) 0.69734(14) 0.0248 1.0000 Uani . . . . . . . C222a C 1.1886(3) 0.4817(3) 0.72791(12) 0.0197 1.0000 Uani . . . . . . . C23a C 0.9740(3) 0.6488(3) 0.90134(12) 0.0164 1.0000 Uani . . . . . . . C230a C 1.0885(4) 0.5390(3) 0.91507(13) 0.0216 1.0000 Uani . . . . . . . C232a C 0.8697(4) 0.6803(3) 0.94981(12) 0.0261 1.0000 Uani . . . . . . . C231a C 1.0388(4) 0.7650(3) 0.88685(13) 0.0249 1.0000 Uani . . . . . . . C24a C 0.5423(3) 0.5729(3) 0.82555(12) 0.0168 1.0000 Uani . . . . . . . C240a C 0.4888(4) 0.5946(4) 0.88312(13) 0.0298 1.0000 Uani . . . . . . . C242a C 0.5157(4) 0.4416(3) 0.81317(14) 0.0241 1.0000 Uani . . . . . . . C241a C 0.4518(4) 0.6752(3) 0.79503(14) 0.0265 1.0000 Uani . . . . . . . C89 C 0.2320(3) 1.0951(3) 0.62165(12) 0.0157 1.0000 Uani . . . . . . . C7b C 0.2962(3) 1.0905(3) 0.66700(12) 0.0141 1.0000 Uani . . . . . . . C16b C 0.5669(3) 1.0830(3) 0.81535(12) 0.0144 1.0000 Uani . . . . . . . C21b C 0.4816(3) 1.1201(3) 0.86258(11) 0.0145 1.0000 Uani . . . . . . . C24b C 0.3225(3) 1.1192(3) 0.87276(12) 0.0177 1.0000 Uani . . . . . . . C241b C 0.2355(4) 1.2120(3) 0.83721(13) 0.0225 1.0000 Uani . . . . . . . C242b C 0.2941(4) 0.9859(3) 0.86703(14) 0.0247 1.0000 Uani . . . . . . . C240b C 0.2634(4) 1.1596(3) 0.92860(13) 0.0273 1.0000 Uani . . . . . . . C20b C 0.5456(3) 1.1582(3) 0.90388(12) 0.0150 1.0000 Uani . . . . . . . C19b C 0.6865(3) 1.1595(3) 0.90112(11) 0.0143 1.0000 Uani . . . . . . . C18b C 0.7673(3) 1.1195(3) 0.85512(12) 0.0148 1.0000 Uani . . . . . . . C17b C 0.7130(3) 1.0782(3) 0.81204(12) 0.0134 1.0000 Uani . . . . . . . C22b C 0.8200(3) 1.0280(3) 0.76475(12) 0.0164 1.0000 Uani . . . . . . . C220b C 0.8021(4) 1.1152(3) 0.71652(12) 0.0229 1.0000 Uani . . . . . . . C221b C 0.8062(4) 0.8942(3) 0.75158(14) 0.0274 1.0000 Uani . . . . . . . C222b C 0.9712(3) 1.0200(3) 0.77630(13) 0.0220 1.0000 Uani . . . . . . . C23b C 0.7553(3) 1.1992(3) 0.94692(12) 0.0171 1.0000 Uani . . . . . . . C232b C 0.6498(4) 1.2422(4) 0.99418(13) 0.0286 1.0000 Uani . . . . . . . C230b C 0.8631(4) 1.0878(3) 0.96394(13) 0.0229 1.0000 Uani . . . . . . . C231b C 0.8293(4) 1.3084(3) 0.92970(13) 0.0246 1.0000 Uani . . . . . . . H41 H 0.4905 1.2988 0.6354 0.0176 1.0000 Uiso R . . . . . . H51 H 0.3815 1.3070 0.5602 0.0201 1.0000 Uiso R . . . . . . H91 H 0.3106 0.9460 0.5465 0.0165 1.0000 Uiso R . . . . . . H121 H 0.0699 0.9820 0.3994 0.0183 1.0000 Uiso R . . . . . . H141 H -0.0008 1.2098 0.4120 0.0209 1.0000 Uiso R . . . . . . H151 H 0.0084 1.3867 0.4581 0.0239 1.0000 Uiso R . . . . . . H161 H 0.1331 1.3696 0.5322 0.0197 1.0000 Uiso R . . . . . . H211 H 0.1309 0.7524 0.3866 0.0221 1.0000 Uiso R . . . . . . H221 H 0.2368 0.5571 0.4142 0.0220 1.0000 Uiso R . . . . . . H231 H 0.3623 0.5370 0.4874 0.0198 1.0000 Uiso R . . . . . . H261 H 0.3312 0.5594 0.5838 0.0186 1.0000 Uiso R . . . . . . H271 H 0.4583 0.5313 0.6549 0.0199 1.0000 Uiso R . . . . . . H291 H 0.6549 0.8101 0.6032 0.0186 1.0000 Uiso R . . . . . . H301 H 0.5329 0.8376 0.5313 0.0184 1.0000 Uiso R . . . . . . H371 H 0.7092 0.6378 0.8891 0.0159 1.0000 Uiso R . . . . . . H391 H 1.0841 0.5752 0.8069 0.0164 1.0000 Uiso R . . . . . . H422 H 1.0905 0.5659 0.6423 0.0360 1.0000 Uiso R . . . . . . H421 H 1.0328 0.6735 0.6832 0.0350 1.0000 Uiso R . . . . . . H423 H 0.9270 0.6029 0.6584 0.0355 1.0000 Uiso R . . . . . . H463 H 1.0932 0.3405 0.6681 0.0363 1.0000 Uiso R . . . . . . H461 H 1.0322 0.3075 0.7252 0.0371 1.0000 Uiso R . . . . . . H462 H 0.9312 0.3723 0.6851 0.0370 1.0000 Uiso R . . . . . . H501 H 1.2492 0.4474 0.6971 0.0296 1.0000 Uiso R . . . . . . H503 H 1.2061 0.4246 0.7567 0.0293 1.0000 Uiso R . . . . . . H502 H 1.2106 0.5618 0.7363 0.0294 1.0000 Uiso R . . . . . . H562 H 1.1325 0.5598 0.9444 0.0321 1.0000 Uiso R . . . . . . H561 H 1.0499 0.4652 0.9254 0.0314 1.0000 Uiso R . . . . . . H563 H 1.1609 0.5162 0.8859 0.0316 1.0000 Uiso R . . . . . . H603 H 0.9171 0.7052 0.9784 0.0386 1.0000 Uiso R . . . . . . H601 H 0.8296 0.6086 0.9616 0.0386 1.0000 Uiso R . . . . . . H602 H 0.7948 0.7485 0.9420 0.0379 1.0000 Uiso R . . . . . . H641 H 1.0843 0.7881 0.9159 0.0369 1.0000 Uiso R . . . . . . H643 H 1.1048 0.7521 0.8557 0.0365 1.0000 Uiso R . . . . . . H642 H 0.9660 0.8349 0.8792 0.0367 1.0000 Uiso R . . . . . . H702 H 0.3914 0.5895 0.8882 0.0453 1.0000 Uiso R . . . . . . H701 H 0.5394 0.5311 0.9052 0.0449 1.0000 Uiso R . . . . . . H703 H 0.4995 0.6782 0.8937 0.0446 1.0000 Uiso R . . . . . . H741 H 0.4198 0.4378 0.8245 0.0361 1.0000 Uiso R . . . . . . H743 H 0.5766 0.3770 0.8312 0.0363 1.0000 Uiso R . . . . . . H742 H 0.5310 0.4280 0.7758 0.0351 1.0000 Uiso R . . . . . . H782 H 0.3565 0.6798 0.8091 0.0400 1.0000 Uiso R . . . . . . H781 H 0.4759 0.7567 0.7989 0.0396 1.0000 Uiso R . . . . . . H783 H 0.4591 0.6584 0.7576 0.0393 1.0000 Uiso R . . . . . . H891 H 0.1662 1.0443 0.6182 0.0189 1.0000 Uiso R . . . . . . H901 H 0.2723 1.0355 0.6941 0.0176 1.0000 Uiso R . . . . . . H991 H 0.1379 1.2210 0.8491 0.0339 1.0000 Uiso R . . . . . . H992 H 0.2575 1.2942 0.8391 0.0337 1.0000 Uiso R . . . . . . H993 H 0.2501 1.1900 0.8004 0.0333 1.0000 Uiso R . . . . . . H1032 H 0.1975 0.9875 0.8780 0.0363 1.0000 Uiso R . . . . . . H1033 H 0.3491 0.9299 0.8897 0.0369 1.0000 Uiso R . . . . . . H1031 H 0.3170 0.9568 0.8310 0.0365 1.0000 Uiso R . . . . . . H1073 H 0.1640 1.1599 0.9329 0.0408 1.0000 Uiso R . . . . . . H1071 H 0.3081 1.1014 0.9545 0.0412 1.0000 Uiso R . . . . . . H1072 H 0.2751 1.2443 0.9355 0.0406 1.0000 Uiso R . . . . . . H1111 H 0.4915 1.1839 0.9354 0.0173 1.0000 Uiso R . . . . . . H1131 H 0.8639 1.1205 0.8532 0.0168 1.0000 Uiso R . . . . . . H1163 H 0.8870 1.0982 0.6917 0.0335 1.0000 Uiso R . . . . . . H1161 H 0.7878 1.2037 0.7261 0.0343 1.0000 Uiso R . . . . . . H1162 H 0.7250 1.1014 0.6985 0.0339 1.0000 Uiso R . . . . . . H1201 H 0.8731 0.8643 0.7216 0.0411 1.0000 Uiso R . . . . . . H1203 H 0.8250 0.8393 0.7818 0.0413 1.0000 Uiso R . . . . . . H1202 H 0.7132 0.8925 0.7420 0.0416 1.0000 Uiso R . . . . . . H1242 H 1.0322 0.9830 0.7460 0.0328 1.0000 Uiso R . . . . . . H1241 H 0.9931 0.9683 0.8067 0.0330 1.0000 Uiso R . . . . . . H1243 H 0.9891 1.1029 0.7819 0.0327 1.0000 Uiso R . . . . . . H1303 H 0.6986 1.2656 1.0228 0.0425 1.0000 Uiso R . . . . . . H1301 H 0.6040 1.1738 1.0068 0.0427 1.0000 Uiso R . . . . . . H1302 H 0.5800 1.3123 0.9848 0.0425 1.0000 Uiso R . . . . . . H1341 H 0.9064 1.1109 0.9929 0.0341 1.0000 Uiso R . . . . . . H1343 H 0.8192 1.0169 0.9744 0.0335 1.0000 Uiso R . . . . . . H1342 H 0.9363 1.0621 0.9362 0.0335 1.0000 Uiso R . . . . . . H1382 H 0.8749 1.3333 0.9584 0.0367 1.0000 Uiso R . . . . . . H1381 H 0.7625 1.3787 0.9191 0.0365 1.0000 Uiso R . . . . . . H1383 H 0.8980 1.2869 0.8997 0.0367 1.0000 Uiso R . . . . . . H21 H 0.4951 1.2303 0.7300 0.0173 1.0000 Uiso R . . . . . . H331 H 0.6873 0.7134 0.6933 0.0189 1.0000 Uiso 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 P1b 0.0214(5) 0.0146(4) 0.0164(4) -0.0018(3) -0.0055(4) -0.0047(4) C1b 0.0145(17) 0.0129(16) 0.0185(16) -0.0049(12) -0.0020(13) -0.0026(13) C2b 0.0170(18) 0.0083(15) 0.0174(16) -0.0038(12) -0.0004(13) 0.0023(13) C3b 0.0151(18) 0.0101(15) 0.0213(17) -0.0029(12) -0.0027(13) -0.0028(13) C4b 0.0230(19) 0.0063(15) 0.0187(17) 0.0000(12) 0.0010(14) 0.0009(13) C5b 0.0119(17) 0.0087(15) 0.0194(16) -0.0039(12) -0.0026(13) 0.0026(13) C8b 0.0154(18) 0.0135(16) 0.0146(16) -0.0018(12) 0.0017(13) -0.0011(13) C15b 0.0100(17) 0.0160(16) 0.0145(16) -0.0006(12) 0.0010(12) -0.0011(13) C13 0.0126(17) 0.0172(16) 0.0123(15) -0.0004(12) -0.0032(12) -0.0022(13) C15a 0.0105(17) 0.0154(16) 0.0106(15) -0.0011(12) 0.0004(12) -0.0005(13) C14a 0.0072(16) 0.0223(17) 0.0136(16) -0.0031(13) 0.0004(12) -0.0021(13) C12 0.0112(17) 0.0222(17) 0.0147(16) 0.0007(13) -0.0043(12) -0.0028(14) C14b 0.0110(17) 0.0200(17) 0.0128(15) 0.0022(12) -0.0012(12) -0.0036(13) C11b 0.0128(18) 0.0226(18) 0.0170(17) 0.0019(13) -0.0026(13) -0.0002(14) C10b 0.0194(19) 0.0154(16) 0.0223(18) 0.0038(13) -0.0040(14) 0.0014(14) C9b 0.0158(18) 0.0139(16) 0.0191(17) -0.0019(13) -0.0025(13) 0.0011(13) C11a 0.0181(19) 0.0240(18) 0.0147(16) -0.0038(13) -0.0032(13) -0.0035(15) C10a 0.0172(18) 0.0164(16) 0.0207(17) -0.0067(13) -0.0022(13) -0.0028(14) C9a 0.0184(18) 0.0111(15) 0.0188(17) -0.0038(12) -0.0001(13) 0.0018(13) C8a 0.0061(16) 0.0170(16) 0.0173(16) -0.0020(13) 0.0015(12) 0.0000(13) C5a 0.0120(17) 0.0099(15) 0.0173(16) -0.0045(12) 0.0002(12) 0.0032(13) C6a 0.0142(17) 0.0094(15) 0.0224(17) -0.0024(12) -0.0032(13) -0.0042(13) C7a 0.0173(18) 0.0096(15) 0.0220(17) 0.0020(12) -0.0035(13) -0.0021(13) C2a 0.0118(17) 0.0124(15) 0.0182(16) -0.0019(12) -0.0031(13) 0.0034(13) C3a 0.0124(17) 0.0108(15) 0.0240(18) -0.0038(13) -0.0022(13) 0.0005(13) C4a 0.0116(17) 0.0115(15) 0.0209(17) -0.0003(12) 0.0006(13) -0.0010(13) C1a 0.0117(17) 0.0176(16) 0.0200(17) -0.0049(13) -0.0028(13) -0.0037(13) P1a 0.0177(5) 0.0141(4) 0.0160(4) -0.0023(3) -0.0055(3) -0.0014(4) C16a 0.0174(18) 0.0069(15) 0.0142(16) 0.0002(12) -0.0028(13) -0.0022(13) C21a 0.0168(18) 0.0096(15) 0.0168(17) 0.0022(12) -0.0016(13) -0.0018(13) C20a 0.0164(18) 0.0135(16) 0.0123(15) -0.0028(12) 0.0024(13) -0.0021(13) C19a 0.0179(18) 0.0118(16) 0.0139(16) -0.0005(12) -0.0024(13) -0.0039(13) C18a 0.0123(17) 0.0124(15) 0.0192(17) -0.0001(12) -0.0022(13) -0.0032(13) C17a 0.0115(17) 0.0096(15) 0.0135(16) 0.0010(12) -0.0007(12) 0.0016(13) C22a 0.0132(17) 0.0120(16) 0.0174(16) -0.0022(12) 0.0003(13) 0.0008(13) C220a 0.0179(19) 0.0288(19) 0.0195(18) 0.0022(14) 0.0038(14) 0.0048(15) C221a 0.019(2) 0.0239(19) 0.030(2) -0.0127(15) -0.0004(15) -0.0004(15) C222a 0.0140(18) 0.0257(18) 0.0178(17) -0.0050(14) 0.0015(13) -0.0008(14) C23a 0.0172(18) 0.0186(17) 0.0146(16) -0.0020(13) -0.0016(13) -0.0061(14) C230a 0.022(2) 0.0269(19) 0.0185(17) -0.0001(14) -0.0078(14) -0.0068(15) C232a 0.026(2) 0.038(2) 0.0156(17) -0.0086(15) -0.0024(14) -0.0077(17) C231a 0.034(2) 0.0222(18) 0.0202(18) -0.0039(14) -0.0041(15) -0.0086(16) C24a 0.0117(18) 0.0181(17) 0.0209(18) -0.0015(13) -0.0030(13) -0.0030(14) C240a 0.019(2) 0.048(2) 0.0227(19) -0.0066(16) 0.0038(15) -0.0098(18) C242a 0.0176(19) 0.0210(18) 0.035(2) -0.0022(15) -0.0006(15) -0.0081(15) C241a 0.0183(19) 0.0253(19) 0.032(2) -0.0001(15) 0.0014(15) 0.0026(15) C89 0.0175(18) 0.0135(16) 0.0165(16) -0.0025(13) -0.0019(13) -0.0032(14) C7b 0.0130(17) 0.0114(15) 0.0180(16) 0.0003(12) -0.0012(13) -0.0030(13) C16b 0.0211(19) 0.0082(15) 0.0146(16) 0.0017(12) -0.0031(13) -0.0044(13) C21b 0.0181(18) 0.0107(15) 0.0154(16) 0.0018(12) -0.0026(13) -0.0043(13) C24b 0.0142(18) 0.0190(17) 0.0202(17) -0.0012(13) -0.0011(13) -0.0046(14) C241b 0.0153(19) 0.0251(19) 0.0260(19) -0.0032(15) -0.0030(14) 0.0002(15) C242b 0.020(2) 0.0222(19) 0.034(2) 0.0007(15) 0.0005(15) -0.0089(15) C240b 0.0180(19) 0.042(2) 0.0238(19) -0.0027(16) 0.0010(14) -0.0118(17) C20b 0.0156(18) 0.0156(16) 0.0132(16) 0.0000(12) 0.0002(13) -0.0027(13) C19b 0.0173(18) 0.0137(16) 0.0124(16) -0.0005(12) -0.0032(13) -0.0035(13) C18b 0.0126(17) 0.0137(16) 0.0181(16) 0.0008(12) -0.0016(13) -0.0027(13) C17b 0.0152(18) 0.0075(15) 0.0159(16) 0.0012(12) -0.0009(13) 0.0013(13) C22b 0.0177(18) 0.0138(16) 0.0164(16) -0.0026(13) -0.0010(13) 0.0002(14) C220b 0.0203(19) 0.0289(19) 0.0180(17) -0.0003(14) 0.0008(14) -0.0029(15) C221b 0.027(2) 0.0190(18) 0.033(2) -0.0104(15) 0.0025(16) 0.0012(16) C222b 0.0165(19) 0.0291(19) 0.0177(17) -0.0015(14) 0.0017(14) 0.0006(15) C23b 0.0176(18) 0.0207(17) 0.0136(16) -0.0037(13) -0.0027(13) -0.0040(14) C232b 0.023(2) 0.044(2) 0.0192(18) -0.0112(16) -0.0033(15) -0.0046(17) C230b 0.025(2) 0.0253(19) 0.0199(18) 0.0001(14) -0.0083(15) -0.0050(16) C231b 0.028(2) 0.0229(18) 0.0252(19) -0.0056(14) -0.0071(15) -0.0066(16) _refine_ls_extinction_method None _oxford_refine_ls_scale 7.66(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag P1b . C1b . 1.673(3) yes P1b . C16b . 1.854(3) yes C1b . C2b . 1.462(4) yes C1b . H21 . 0.931 no C2b . C3b . 1.409(4) yes C2b . C7b . 1.395(4) yes C3b . C4b . 1.388(4) yes C3b . H41 . 0.947 no C4b . C5b . 1.401(4) yes C4b . H51 . 0.933 no C5b . C8b . 1.489(4) yes C5b . C89 . 1.405(4) yes C8b . C15b . 1.447(4) yes C8b . C9b . 1.373(4) yes C15b . C13 . 1.398(4) yes C15b . C14b . 1.434(4) yes C13 . C15a . 1.399(4) yes C13 . H91 . 0.935 no C15a . C14a . 1.442(4) yes C15a . C8a . 1.450(4) yes C14a . C12 . 1.404(4) yes C14a . C11a . 1.429(4) yes C12 . C14b . 1.398(4) yes C12 . H121 . 0.943 no C14b . C11b . 1.428(4) yes C11b . C10b . 1.354(4) yes C11b . H141 . 0.952 no C10b . C9b . 1.419(4) yes C10b . H151 . 0.947 no C9b . H161 . 0.944 no C11a . C10a . 1.358(4) yes C11a . H211 . 0.943 no C10a . C9a . 1.417(4) yes C10a . H221 . 0.957 no C9a . C8a . 1.377(4) yes C9a . H231 . 0.954 no C8a . C5a . 1.491(4) yes C5a . C6a . 1.404(4) yes C5a . C4a . 1.398(5) yes C6a . C7a . 1.387(4) yes C6a . H261 . 0.940 no C7a . C2a . 1.400(5) yes C7a . H271 . 0.938 no C2a . C3a . 1.402(4) yes C2a . C1a . 1.466(4) yes C3a . C4a . 1.389(4) yes C3a . H291 . 0.926 no C4a . H301 . 0.946 no C1a . P1a . 1.676(3) yes C1a . H331 . 0.926 no P1a . C16a . 1.858(3) yes C16a . C21a . 1.422(4) yes C16a . C17a . 1.420(4) yes C21a . C20a . 1.402(4) yes C21a . C24a . 1.564(5) yes C20a . C19a . 1.383(5) yes C20a . H371 . 0.959 no C19a . C18a . 1.392(4) yes C19a . C23a . 1.533(4) yes C18a . C17a . 1.403(4) yes C18a . H391 . 0.955 no C17a . C22a . 1.558(4) yes C22a . C220a . 1.544(4) yes C22a . C221a . 1.530(4) yes C22a . C222a . 1.541(4) yes C220a . H422 . 0.968 no C220a . H421 . 0.970 no C220a . H423 . 0.982 no C221a . H463 . 0.989 no C221a . H461 . 0.965 no C221a . H462 . 0.964 no C222a . H501 . 0.978 no C222a . H503 . 0.964 no C222a . H502 . 0.971 no C23a . C230a . 1.540(4) yes C23a . C232a . 1.532(4) yes C23a . C231a . 1.539(4) yes C230a . H562 . 0.964 no C230a . H561 . 0.970 no C230a . H563 . 0.980 no C232a . H603 . 0.984 no C232a . H601 . 0.967 no C232a . H602 . 0.974 no C231a . H641 . 0.976 no C231a . H643 . 0.971 no C231a . H642 . 0.972 no C24a . C240a . 1.530(4) yes C24a . C242a . 1.548(4) yes C24a . C241a . 1.541(4) yes C240a . H702 . 0.964 no C240a . H701 . 0.979 no C240a . H703 . 0.983 no C242a . H741 . 0.965 no C242a . H743 . 0.976 no C242a . H742 . 0.970 no C241a . H782 . 0.960 no C241a . H781 . 0.970 no C241a . H783 . 0.980 no C89 . C7b . 1.384(4) yes C89 . H891 . 0.939 no C7b . H901 . 0.946 no C16b . C21b . 1.424(4) yes C16b . C17b . 1.421(5) yes C21b . C24b . 1.560(5) yes C21b . C20b . 1.404(4) yes C24b . C241b . 1.544(4) yes C24b . C242b . 1.541(4) yes C24b . C240b . 1.537(4) yes C241b . H991 . 0.963 no C241b . H992 . 0.963 no C241b . H993 . 0.974 no C242b . H1032 . 0.959 no C242b . H1033 . 0.964 no C242b . H1031 . 0.978 no C240b . H1073 . 0.971 no C240b . H1071 . 0.987 no C240b . H1072 . 0.974 no C20b . C19b . 1.383(5) yes C20b . H1111 . 0.942 no C19b . C18b . 1.386(4) yes C19b . C23b . 1.534(4) yes C18b . C17b . 1.403(4) yes C18b . H1131 . 0.948 no C17b . C22b . 1.560(4) yes C22b . C220b . 1.548(4) yes C22b . C221b . 1.537(4) yes C22b . C222b . 1.534(5) yes C220b . H1163 . 0.986 no C220b . H1161 . 0.981 no C220b . H1162 . 0.968 no C221b . H1201 . 0.979 no C221b . H1203 . 0.982 no C221b . H1202 . 0.976 no C222b . H1242 . 0.978 no C222b . H1241 . 0.970 no C222b . H1243 . 0.968 no C23b . C232b . 1.534(4) yes C23b . C230b . 1.539(4) yes C23b . C231b . 1.537(5) yes C232b . H1303 . 0.986 no C232b . H1301 . 0.972 no C232b . H1302 . 0.969 no C230b . H1341 . 0.960 no C230b . H1343 . 0.972 no C230b . H1342 . 0.965 no C231b . H1382 . 0.976 no C231b . H1381 . 0.963 no C231b . H1383 . 0.974 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1b . P1b . C16b . 104.07(15) yes P1b . C1b . C2b . 123.3(2) yes P1b . C1b . H21 . 119.2 no C2b . C1b . H21 . 117.4 no C1b . C2b . C3b . 120.8(3) yes C1b . C2b . C7b . 121.4(3) yes C3b . C2b . C7b . 117.8(3) yes C2b . C3b . C4b . 120.9(3) yes C2b . C3b . H41 . 120.2 no C4b . C3b . H41 . 119.0 no C3b . C4b . C5b . 121.1(3) yes C3b . C4b . H51 . 119.6 no C5b . C4b . H51 . 119.3 no C4b . C5b . C8b . 121.1(3) yes C4b . C5b . C89 . 118.0(3) yes C8b . C5b . C89 . 121.0(3) yes C5b . C8b . C15b . 120.7(3) yes C5b . C8b . C9b . 120.1(3) yes C15b . C8b . C9b . 119.1(3) yes C8b . C15b . C13 . 122.6(3) yes C8b . C15b . C14b . 118.5(3) yes C13 . C15b . C14b . 118.9(3) yes C15b . C13 . C15a . 123.0(3) yes C15b . C13 . H91 . 118.6 no C15a . C13 . H91 . 118.5 no C13 . C15a . C14a . 118.2(3) yes C13 . C15a . C8a . 123.0(3) yes C14a . C15a . C8a . 118.7(3) yes C15a . C14a . C12 . 118.8(3) yes C15a . C14a . C11a . 119.2(3) yes C12 . C14a . C11a . 122.0(3) yes C14a . C12 . C14b . 122.6(3) yes C14a . C12 . H121 . 118.5 no C14b . C12 . H121 . 118.9 no C15b . C14b . C12 . 118.6(3) yes C15b . C14b . C11b . 119.5(3) yes C12 . C14b . C11b . 121.9(3) yes C14b . C11b . C10b . 120.7(3) yes C14b . C11b . H141 . 118.6 no C10b . C11b . H141 . 120.7 no C11b . C10b . C9b . 120.3(3) yes C11b . C10b . H151 . 119.8 no C9b . C10b . H151 . 119.9 no C10b . C9b . C8b . 121.8(3) yes C10b . C9b . H161 . 120.1 no C8b . C9b . H161 . 118.1 no C14a . C11a . C10a . 120.6(3) yes C14a . C11a . H211 . 119.3 no C10a . C11a . H211 . 120.1 no C11a . C10a . C9a . 120.8(3) yes C11a . C10a . H221 . 120.1 no C9a . C10a . H221 . 119.1 no C10a . C9a . C8a . 121.7(3) yes C10a . C9a . H231 . 119.3 no C8a . C9a . H231 . 119.1 no C15a . C8a . C9a . 119.0(3) yes C15a . C8a . C5a . 121.5(3) yes C9a . C8a . C5a . 119.5(3) yes C8a . C5a . C6a . 120.0(3) yes C8a . C5a . C4a . 122.1(3) yes C6a . C5a . C4a . 117.8(3) yes C5a . C6a . C7a . 120.8(3) yes C5a . C6a . H261 . 120.0 no C7a . C6a . H261 . 119.2 no C6a . C7a . C2a . 121.5(3) yes C6a . C7a . H271 . 119.7 no C2a . C7a . H271 . 118.8 no C7a . C2a . C3a . 117.5(3) yes C7a . C2a . C1a . 121.7(3) yes C3a . C2a . C1a . 120.8(3) yes C2a . C3a . C4a . 121.1(3) yes C2a . C3a . H291 . 119.9 no C4a . C3a . H291 . 119.0 no C5a . C4a . C3a . 121.2(3) yes C5a . C4a . H301 . 119.6 no C3a . C4a . H301 . 119.2 no C2a . C1a . P1a . 123.8(2) yes C2a . C1a . H331 . 117.8 no P1a . C1a . H331 . 118.4 no C1a . P1a . C16a . 103.01(15) yes P1a . C16a . C21a . 118.5(2) yes P1a . C16a . C17a . 121.7(2) yes C21a . C16a . C17a . 119.7(3) yes C16a . C21a . C20a . 118.0(3) yes C16a . C21a . C24a . 125.2(3) yes C20a . C21a . C24a . 116.8(3) yes C21a . C20a . C19a . 123.6(3) yes C21a . C20a . H371 . 119.4 no C19a . C20a . H371 . 117.0 no C20a . C19a . C18a . 117.1(3) yes C20a . C19a . C23a . 122.7(3) yes C18a . C19a . C23a . 120.2(3) yes C19a . C18a . C17a . 123.1(3) yes C19a . C18a . H391 . 117.0 no C17a . C18a . H391 . 119.9 no C16a . C17a . C18a . 118.4(3) yes C16a . C17a . C22a . 125.0(3) yes C18a . C17a . C22a . 116.7(3) yes C17a . C22a . C220a . 111.4(2) yes C17a . C22a . C221a . 111.2(3) yes C220a . C22a . C221a . 110.3(3) yes C17a . C22a . C222a . 112.1(3) yes C220a . C22a . C222a . 106.3(3) yes C221a . C22a . C222a . 105.3(3) yes C22a . C220a . H422 . 108.7 no C22a . C220a . H421 . 108.4 no H422 . C220a . H421 . 109.0 no C22a . C220a . H423 . 111.2 no H422 . C220a . H423 . 109.6 no H421 . C220a . H423 . 110.0 no C22a . C221a . H463 . 109.6 no C22a . C221a . H461 . 110.8 no H463 . C221a . H461 . 108.7 no C22a . C221a . H462 . 110.6 no H463 . C221a . H462 . 108.0 no H461 . C221a . H462 . 109.2 no C22a . C222a . H501 . 108.2 no C22a . C222a . H503 . 110.9 no H501 . C222a . H503 . 108.6 no C22a . C222a . H502 . 110.9 no H501 . C222a . H502 . 109.1 no H503 . C222a . H502 . 109.0 no C19a . C23a . C230a . 109.5(3) yes C19a . C23a . C232a . 112.5(3) yes C230a . C23a . C232a . 108.3(3) yes C19a . C23a . C231a . 109.0(3) yes C230a . C23a . C231a . 109.6(3) yes C232a . C23a . C231a . 107.9(3) yes C23a . C230a . H562 . 110.6 no C23a . C230a . H561 . 111.2 no H562 . C230a . H561 . 106.2 no C23a . C230a . H563 . 112.4 no H562 . C230a . H563 . 108.1 no H561 . C230a . H563 . 108.1 no C23a . C232a . H603 . 109.8 no C23a . C232a . H601 . 111.1 no H603 . C232a . H601 . 107.7 no C23a . C232a . H602 . 110.0 no H603 . C232a . H602 . 109.5 no H601 . C232a . H602 . 108.7 no C23a . C231a . H641 . 110.1 no C23a . C231a . H643 . 112.3 no H641 . C231a . H643 . 109.9 no C23a . C231a . H642 . 109.4 no H641 . C231a . H642 . 108.5 no H643 . C231a . H642 . 106.5 no C21a . C24a . C240a . 111.6(3) yes C21a . C24a . C242a . 110.6(2) yes C240a . C24a . C242a . 105.4(3) yes C21a . C24a . C241a . 112.3(3) yes C240a . C24a . C241a . 106.0(3) yes C242a . C24a . C241a . 110.7(3) yes C24a . C240a . H702 . 109.2 no C24a . C240a . H701 . 111.0 no H702 . C240a . H701 . 108.4 no C24a . C240a . H703 . 110.1 no H702 . C240a . H703 . 108.8 no H701 . C240a . H703 . 109.3 no C24a . C242a . H741 . 108.9 no C24a . C242a . H743 . 110.3 no H741 . C242a . H743 . 109.5 no C24a . C242a . H742 . 109.7 no H741 . C242a . H742 . 108.0 no H743 . C242a . H742 . 110.5 no C24a . C241a . H782 . 107.8 no C24a . C241a . H781 . 111.6 no H782 . C241a . H781 . 108.1 no C24a . C241a . H783 . 113.5 no H782 . C241a . H783 . 108.3 no H781 . C241a . H783 . 107.5 no C5b . C89 . C7b . 120.8(3) yes C5b . C89 . H891 . 119.1 no C7b . C89 . H891 . 120.1 no C2b . C7b . C89 . 121.5(3) yes C2b . C7b . H901 . 119.9 no C89 . C7b . H901 . 118.6 no P1b . C16b . C21b . 118.7(2) yes P1b . C16b . C17b . 121.1(2) yes C21b . C16b . C17b . 120.2(3) yes C16b . C21b . C24b . 125.2(3) yes C16b . C21b . C20b . 117.8(3) yes C24b . C21b . C20b . 117.0(3) yes C21b . C24b . C241b . 112.7(3) yes C21b . C24b . C242b . 110.7(3) yes C241b . C24b . C242b . 110.5(3) yes C21b . C24b . C240b . 111.9(3) yes C241b . C24b . C240b . 104.9(3) yes C242b . C24b . C240b . 105.8(3) yes C24b . C241b . H991 . 110.1 no C24b . C241b . H992 . 110.5 no H991 . C241b . H992 . 105.9 no C24b . C241b . H993 . 114.6 no H991 . C241b . H993 . 109.2 no H992 . C241b . H993 . 106.1 no C24b . C242b . H1032 . 107.8 no C24b . C242b . H1033 . 108.9 no H1032 . C242b . H1033 . 108.6 no C24b . C242b . H1031 . 111.4 no H1032 . C242b . H1031 . 110.4 no H1033 . C242b . H1031 . 109.7 no C24b . C240b . H1073 . 109.1 no C24b . C240b . H1071 . 111.1 no H1073 . C240b . H1071 . 108.8 no C24b . C240b . H1072 . 111.5 no H1073 . C240b . H1072 . 106.9 no H1071 . C240b . H1072 . 109.4 no C21b . C20b . C19b . 123.4(3) yes C21b . C20b . H1111 . 119.5 no C19b . C20b . H1111 . 117.1 no C20b . C19b . C18b . 117.4(3) yes C20b . C19b . C23b . 122.7(3) yes C18b . C19b . C23b . 119.8(3) yes C19b . C18b . C17b . 123.3(3) yes C19b . C18b . H1131 . 117.4 no C17b . C18b . H1131 . 119.3 no C16b . C17b . C18b . 117.8(3) yes C16b . C17b . C22b . 125.5(3) yes C18b . C17b . C22b . 116.6(3) yes C17b . C22b . C220b . 111.6(2) yes C17b . C22b . C221b . 110.1(3) yes C220b . C22b . C221b . 110.7(3) yes C17b . C22b . C222b . 112.4(3) yes C220b . C22b . C222b . 105.7(3) yes C221b . C22b . C222b . 106.1(3) yes C22b . C220b . H1163 . 109.9 no C22b . C220b . H1161 . 111.6 no H1163 . C220b . H1161 . 106.9 no C22b . C220b . H1162 . 111.2 no H1163 . C220b . H1162 . 107.7 no H1161 . C220b . H1162 . 109.4 no C22b . C221b . H1201 . 109.2 no C22b . C221b . H1203 . 109.3 no H1201 . C221b . H1203 . 109.9 no C22b . C221b . H1202 . 110.9 no H1201 . C221b . H1202 . 107.6 no H1203 . C221b . H1202 . 109.9 no C22b . C222b . H1242 . 108.0 no C22b . C222b . H1241 . 112.4 no H1242 . C222b . H1241 . 108.6 no C22b . C222b . H1243 . 110.2 no H1242 . C222b . H1243 . 108.8 no H1241 . C222b . H1243 . 108.8 no C19b . C23b . C232b . 112.5(3) yes C19b . C23b . C230b . 109.2(3) yes C232b . C23b . C230b . 108.3(3) yes C19b . C23b . C231b . 109.5(3) yes C232b . C23b . C231b . 108.1(3) yes C230b . C23b . C231b . 109.2(3) yes C23b . C232b . H1303 . 109.7 no C23b . C232b . H1301 . 109.9 no H1303 . C232b . H1301 . 107.4 no C23b . C232b . H1302 . 110.4 no H1303 . C232b . H1302 . 110.3 no H1301 . C232b . H1302 . 109.0 no C23b . C230b . H1341 . 110.3 no C23b . C230b . H1343 . 110.8 no H1341 . C230b . H1343 . 108.5 no C23b . C230b . H1342 . 111.2 no H1341 . C230b . H1342 . 107.0 no H1343 . C230b . H1342 . 108.9 no C23b . C231b . H1382 . 110.1 no C23b . C231b . H1381 . 109.7 no H1382 . C231b . H1381 . 109.4 no C23b . C231b . H1383 . 112.1 no H1382 . C231b . H1383 . 109.3 no H1381 . C231b . H1383 . 106.2 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C13 . H91 . C4a . 122 0.93 2.50 3.102(4) yes C13 . H91 . C89 . 121 0.93 2.52 3.106(4) yes C220b . H1162 . C1b . 132 0.97 2.55 3.274(4) yes # Attachment 'elineBesnard_1298972567.cif' data_geml2 _database_code_depnum_ccdc_archive 'CCDC 815022' #TrackingRef 'elineBesnard_1298972567.cif' _exptl_special_details ; ; _refine_special_details ; The tertiobutyl groups all show large anisotropic displacement parameters indicating possible thermal motion / disorder. On a Fourier diffence map, extra peaks appeared clearly around the C104 carbon, showing a second possible orientation for this tertiobutyl group. This orientation was included in the model and the two tertiobutyl groups to which C20b belongs were refined using restrains on angles and distances. The anisotropic displacement parameters of opposed carbons were also restrained to be equivalent. The final occupancy for each group were 0.798(3)/0.202(3). The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 10.185(10) _cell_length_b 17.940(5) _cell_length_c 29.06(2) _cell_angle_alpha 90 _cell_angle_beta 96.79(5) _cell_angle_gamma 90 _cell_volume 5272(7) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C60 H74 P2 # Dc = 1.08 Fooo = 1856.00 Mu = 1.18 M = 857.20 # Found Formula = C60 H74 P2 # Dc = 1.08 FOOO = 1856.00 Mu = 1.18 M = 857.20 _chemical_formula_sum 'C60 H74 P2' _chemical_formula_moiety 'C60 H74 P2' _chemical_compound_source ? _chemical_formula_weight 857.20 _cell_measurement_reflns_used 20430 _cell_measurement_theta_min 5 _cell_measurement_theta_max 29 _cell_measurement_temperature 293 _exptl_crystal_description unknown _exptl_crystal_colour white _exptl_crystal_size_min 0.300 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_max 0.700 _exptl_crystal_density_diffrn 1.080 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 0.118 # Sheldrick geometric approximatio 0.94 0.97 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_measurement_device 'Stoe IPDS' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'IPDS (Stoe & Cie, 1996)' _computing_cell_refinement 'IPDS (Stoe & Cie, 1996)' _computing_data_reduction 'XDS (Kabsch 1993)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 46338 _reflns_number_total 10372 _diffrn_reflns_av_R_equivalents 0.060 # Number of reflections with Friedels Law is 12986 # Number of reflections without Friedels Law is 10372 # Theoretical number of reflections is about 13085 _diffrn_reflns_theta_min 4.701 _diffrn_reflns_theta_max 29.221 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.454 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 38 _oxford_diffrn_Wilson_B_factor 3.85 _oxford_diffrn_Wilson_scale 0.04 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.32 _refine_diff_density_max 0.29 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 10255 _refine_ls_number_restraints 30 _refine_ls_number_parameters 587 _oxford_refine_ls_R_factor_ref 0.0757 _refine_ls_wR_factor_ref 0.0811 _refine_ls_goodness_of_fit_ref 0.9830 _refine_ls_shift/su_max 0.0002530 _refine_ls_shift/su_mean 2.1075139 # The values computed from all data _oxford_reflns_number_all 10255 _refine_ls_R_factor_all 0.0757 _refine_ls_wR_factor_all 0.0811 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7342 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_gt 0.0696 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.124E+04 0.166E+04 890. 245. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Kabsch, W. J.(1993). Appl. Cryst. 26, 795-800 (1993). Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Stoe & Cie (1996). IPDS Software. Stoe & Cie (1996). XRED V1.08. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens P1a P 0.44671(7) 0.11410(4) 0.23450(2) 0.0615 1.0000 Uani . . . . . . . C14a C 0.3332(2) 0.18189(12) 0.25725(7) 0.0462 1.0000 Uani . . . . . . . C15a C 0.1953(2) 0.16561(12) 0.25647(7) 0.0489 1.0000 Uani . . . . . . . C22a C 0.1287(2) 0.08973(13) 0.24169(9) 0.0643 1.0000 Uani . . . . . . . C220a C 0.1225(3) 0.07599(15) 0.18965(8) 0.0764 1.0000 Uani . . . . . . . H51 H 0.0723 0.0310 0.1814 0.1106 1.0000 Uiso R . . . . . . H52 H 0.2103 0.0704 0.1797 0.1100 1.0000 Uiso R . . . . . . H53 H 0.0772 0.1175 0.1728 0.1102 1.0000 Uiso R . . . . . . C221a C 0.2003(3) 0.02591(15) 0.26933(10) 0.0973 1.0000 Uani . . . . . . . H93 H 0.1576 -0.0210 0.2591 0.1438 1.0000 Uiso R . . . . . . H92 H 0.1879 0.0354 0.3013 0.1446 1.0000 Uiso R . . . . . . H91 H 0.2958 0.0237 0.2661 0.1444 1.0000 Uiso R . . . . . . C222a C -0.0171(3) 0.08663(17) 0.25230(11) 0.1084 1.0000 Uani . . . . . . . H133 H -0.0529 0.0376 0.2451 0.1539 1.0000 Uiso R . . . . . . H132 H -0.0184 0.0950 0.2857 0.1548 1.0000 Uiso R . . . . . . H131 H -0.0701 0.1257 0.2349 0.1550 1.0000 Uiso R . . . . . . C16a C 0.1145(2) 0.22030(12) 0.27169(7) 0.0519 1.0000 Uani . . . . . . . C17a C 0.1598(2) 0.28832(11) 0.28929(7) 0.0467 1.0000 Uani . . . . . . . C20a C 0.0626(2) 0.34449(13) 0.30593(8) 0.0585 1.0000 Uani . . . . . . . C200a C 0.1320(3) 0.41101(15) 0.33059(11) 0.0913 1.0000 Uani . . . . . . . H202 H 0.0648 0.4419 0.3422 0.1321 1.0000 Uiso R . . . . . . H201 H 0.1940 0.3925 0.3563 0.1331 1.0000 Uiso R . . . . . . H203 H 0.1775 0.4377 0.3076 0.1335 1.0000 Uiso R . . . . . . C201a C -0.0302(3) 0.37303(19) 0.26436(11) 0.1085 1.0000 Uani . . . . . . . H242 H -0.0920 0.4084 0.2746 0.1611 1.0000 Uiso R . . . . . . H243 H 0.0247 0.3993 0.2441 0.1617 1.0000 Uiso R . . . . . . H241 H -0.0751 0.3292 0.2493 0.1615 1.0000 Uiso R . . . . . . C202a C -0.0181(3) 0.30658(17) 0.34068(12) 0.1109 1.0000 Uani . . . . . . . H281 H -0.0802 0.3416 0.3507 0.1580 1.0000 Uiso R . . . . . . H283 H 0.0405 0.2928 0.3674 0.1601 1.0000 Uiso R . . . . . . H282 H -0.0651 0.2633 0.3266 0.1591 1.0000 Uiso R . . . . . . C18a C 0.2940(2) 0.30105(12) 0.29185(7) 0.0486 1.0000 Uani . . . . . . . C19a C 0.38355(19) 0.24988(12) 0.27681(7) 0.0462 1.0000 Uani . . . . . . . C21a C 0.5326(2) 0.27208(14) 0.28434(8) 0.0581 1.0000 Uani . . . . . . . C210a C 0.5852(3) 0.28965(19) 0.23865(9) 0.0967 1.0000 Uani . . . . . . . H352 H 0.6759 0.3042 0.2455 0.1406 1.0000 Uiso R . . . . . . H351 H 0.5335 0.3300 0.2221 0.1417 1.0000 Uiso R . . . . . . H353 H 0.5823 0.2458 0.2187 0.1403 1.0000 Uiso R . . . . . . C211a C 0.5561(3) 0.34333(18) 0.31404(11) 0.1045 1.0000 Uani . . . . . . . H391 H 0.6512 0.3533 0.3185 0.1491 1.0000 Uiso R . . . . . . H393 H 0.5208 0.3343 0.3434 0.1499 1.0000 Uiso R . . . . . . H392 H 0.5078 0.3833 0.2966 0.1504 1.0000 Uiso R . . . . . . C212a C 0.6157(3) 0.21191(19) 0.31128(11) 0.1114 1.0000 Uani . . . . . . . H431 H 0.7023 0.2312 0.3212 0.1649 1.0000 Uiso R . . . . . . H432 H 0.5715 0.1985 0.3380 0.1666 1.0000 Uiso R . . . . . . H433 H 0.6218 0.1686 0.2920 0.1664 1.0000 Uiso R . . . . . . H321 H 0.3261 0.3445 0.3045 0.0574 1.0000 Uiso R . . . . . . H171 H 0.0234 0.2095 0.2702 0.0613 1.0000 Uiso R . . . . . . C1a C 0.43753(19) 0.13425(12) 0.17846(7) 0.0497 1.0000 Uani . . . . . . . C2a C 0.51456(19) 0.09511(11) 0.14617(7) 0.0456 1.0000 Uani . . . . . . . C3a C 0.46202(19) 0.08204(11) 0.10038(7) 0.0465 1.0000 Uani . . . . . . . C4a C 0.53063(18) 0.04114(11) 0.07050(7) 0.0452 1.0000 Uani . . . . . . . C5a C 0.65700(19) 0.01377(11) 0.08489(7) 0.0449 1.0000 Uani . . . . . . . C6a C 0.7099(2) 0.02733(12) 0.13047(7) 0.0524 1.0000 Uani . . . . . . . C7a C 0.6412(2) 0.06725(13) 0.16064(7) 0.0537 1.0000 Uani . . . . . . . H551 H 0.6806 0.0759 0.1917 0.0639 1.0000 Uiso R . . . . . . H541 H 0.7943 0.0086 0.1410 0.0598 1.0000 Uiso R . . . . . . C8a C 0.73292(19) -0.03344(11) 0.05452(7) 0.0458 1.0000 Uani . . . . . . . C13 C 0.78023(18) -0.01020(11) 0.01193(7) 0.0425 1.0000 Uani . . . . . . . C8b C 0.76642(18) 0.06267(12) -0.00849(7) 0.0443 1.0000 Uani . . . . . . . C5b C 0.69720(19) 0.12766(11) 0.01031(7) 0.0444 1.0000 Uani . . . . . . . C6b C 0.74396(19) 0.16456(11) 0.05112(7) 0.0480 1.0000 Uani . . . . . . . C7b C 0.6794(2) 0.22649(12) 0.06601(7) 0.0510 1.0000 Uani . . . . . . . C2b C 0.5641(2) 0.25408(11) 0.04012(7) 0.0480 1.0000 Uani . . . . . . . C3b C 0.5200(2) 0.21791(12) -0.00110(8) 0.0536 1.0000 Uani . . . . . . . C4b C 0.5846(2) 0.15624(12) -0.01584(7) 0.0510 1.0000 Uani . . . . . . . H661 H 0.5517 0.1334 -0.0433 0.0593 1.0000 Uiso R . . . . . . H651 H 0.4432 0.2361 -0.0202 0.0637 1.0000 Uiso R . . . . . . C1b C 0.4922(2) 0.31891(12) 0.05526(8) 0.0546 1.0000 Uani . . . . . . . P1b P 0.49656(7) 0.34844(4) 0.10941(2) 0.0679 1.0000 Uani . . . . . . . C14b C 0.3902(2) 0.43245(12) 0.10165(7) 0.0515 1.0000 Uani . . . . . . . C19b C 0.4473(2) 0.50287(13) 0.09339(8) 0.0545 1.0000 Uani . . . . . . . C21b C 0.5992(2) 0.51948(15) 0.09686(9) 0.0702 1.0000 Uani . . . . . . . C210b C 0.6582(3) 0.49105(18) 0.05408(11) 0.1013 1.0000 Uani . . . . . . . H741 H 0.7520 0.5029 0.0556 0.1494 1.0000 Uiso R . . . . . . H742 H 0.6108 0.5148 0.0265 0.1501 1.0000 Uiso R . . . . . . H743 H 0.6482 0.4376 0.0510 0.1497 1.0000 Uiso R . . . . . . C211b C 0.6274(3) 0.60393(16) 0.10023(12) 0.1052 1.0000 Uani . . . . . . . H782 H 0.7233 0.6128 0.1061 0.1556 1.0000 Uiso R . . . . . . H781 H 0.5855 0.6251 0.1252 0.1557 1.0000 Uiso R . . . . . . H783 H 0.5923 0.6280 0.0719 0.1569 1.0000 Uiso R . . . . . . C212b C 0.6752(3) 0.4857(2) 0.14116(11) 0.1126 1.0000 Uani . . . . . . . H821 H 0.7647 0.5040 0.1453 0.1693 1.0000 Uiso R . . . . . . H823 H 0.6347 0.4960 0.1687 0.1704 1.0000 Uiso R . . . . . . H822 H 0.6803 0.4318 0.1380 0.1700 1.0000 Uiso R . . . . . . C18b C 0.3626(2) 0.56219(12) 0.08105(8) 0.0553 1.0000 Uani . . . . . . . C17b C 0.2262(2) 0.55700(11) 0.07764(7) 0.0484 1.0000 Uani . . . . . . . C16b C 0.1743(2) 0.48933(12) 0.08910(7) 0.0497 1.0000 Uani . . . . . . . C15b C 0.2513(2) 0.42677(12) 0.10222(7) 0.0494 1.0000 Uani . . . . . . . C22b C 0.1781(2) 0.35650(12) 0.11791(8) 0.0590 1.0000 Uani . . . . . . . C220b C 0.0332(2) 0.37431(15) 0.12542(10) 0.0829 1.0000 Uani . . . . . . . H912 H -0.0026 0.3309 0.1402 0.1190 1.0000 Uiso R . . . . . . H913 H 0.0341 0.4180 0.1451 0.1194 1.0000 Uiso R . . . . . . H911 H -0.0183 0.3839 0.0954 0.1201 1.0000 Uiso R . . . . . . C221b C 0.2450(3) 0.32878(15) 0.16494(9) 0.0807 1.0000 Uani . . . . . . . H951 H 0.1951 0.2873 0.1754 0.1176 1.0000 Uiso R . . . . . . H953 H 0.2440 0.3683 0.1866 0.1192 1.0000 Uiso R . . . . . . H952 H 0.3367 0.3130 0.1636 0.1183 1.0000 Uiso R . . . . . . C222b C 0.1714(3) 0.29353(15) 0.08212(10) 0.0841 1.0000 Uani . . . . . . . H992 H 0.1064 0.2556 0.0886 0.1221 1.0000 Uiso R . . . . . . H991 H 0.2581 0.2699 0.0814 0.1230 1.0000 Uiso R . . . . . . H993 H 0.1435 0.3135 0.0515 0.1222 1.0000 Uiso R . . . . . . H881 H 0.0821 0.4845 0.0880 0.0566 1.0000 Uiso R . . . . . . C20b C 0.1396(2) 0.62488(12) 0.06375(8) 0.0572 1.0000 Uani D . . . . . . C200b C -0.0076(3) 0.6103(2) 0.06249(19) 0.0977 0.798(3) Uani D U P . 1 . . C201b C 0.0599(15) 0.6396(8) 0.1049(4) 0.0954 0.202(3) Uani D U P . 2 . . H1051 H -0.0219 0.5951 0.0946 0.1597 0.798(3) Uiso R . P . 1 . . H1063 H 0.0044 0.5991 0.1120 0.1389 0.202(3) Uiso R . P . 2 . . C202b C 0.1783(4) 0.6892(2) 0.09852(15) 0.0963 0.798(3) Uani D U P . 1 . . C203b C 0.2030(14) 0.6965(6) 0.0506(7) 0.1148 0.202(3) Uani D U P . 2 . . H1101 H 0.2551 0.7165 0.0774 0.1710 0.202(3) Uiso R . P . 2 . . H1091 H 0.2725 0.7016 0.0978 0.1587 0.798(3) Uiso R . P . 1 . . C204b C 0.1647(4) 0.6521(2) 0.01563(13) 0.0951 0.798(3) Uani D U P . 1 . . H1103 H 0.2615 0.6808 0.0290 0.1711 0.202(3) Uiso R . P . 2 . . H1131 H 0.2584 0.6639 0.0169 0.1507 0.798(3) Uiso R . P . 1 . . C205b C 0.0386(14) 0.5988(7) 0.0227(5) 0.1023 0.202(3) Uani D U P . 2 . . H1053 H -0.0320 0.5701 0.0397 0.1594 0.798(3) Uiso R . P . 1 . . H1161 H -0.0107 0.5559 0.0302 0.1609 0.202(3) Uiso R . P . 2 . . H1162 H -0.0213 0.6395 0.0146 0.1610 0.202(3) Uiso R . P . 2 . . H1163 H 0.0851 0.5864 -0.0030 0.1610 0.202(3) Uiso R . P . 2 . . H1133 H 0.1413 0.6103 -0.0053 0.1509 0.798(3) Uiso R . P . 1 . . H1132 H 0.1110 0.6966 0.0081 0.1493 0.798(3) Uiso R . P . 1 . . H1102 H 0.1452 0.7346 0.0369 0.1709 0.202(3) Uiso R . P . 2 . . H1093 H 0.1221 0.7320 0.0902 0.1578 0.798(3) Uiso R . P . 1 . . H1092 H 0.1651 0.6679 0.1298 0.1588 0.798(3) Uiso R . P . 1 . . H1062 H 0.1211 0.6493 0.1320 0.1389 0.202(3) Uiso R . P . 2 . . H1061 H 0.0057 0.6829 0.0968 0.1389 0.202(3) Uiso R . P . 2 . . H1052 H -0.0553 0.6566 0.0536 0.1575 0.798(3) Uiso R . P . 1 . . H861 H 0.3977 0.6095 0.0745 0.0651 1.0000 Uiso R . . . . . . H691 H 0.4362 0.3438 0.0322 0.0669 1.0000 Uiso R . . . . . . H631 H 0.7126 0.2504 0.0936 0.0582 1.0000 Uiso R . . . . . . H621 H 0.8234 0.1472 0.0696 0.0554 1.0000 Uiso R . . . . . . C9b C 0.8172(2) 0.07648(13) -0.04959(7) 0.0557 1.0000 Uani . . . . . . . C10b C 0.8831(2) 0.02187(15) -0.07264(8) 0.0624 1.0000 Uani . . . . . . . C11b C 0.8979(2) -0.04709(14) -0.05438(8) 0.0578 1.0000 Uani . . . . . . . C12 C 0.84905(19) -0.06513(12) -0.01232(7) 0.0493 1.0000 Uani . . . . . . . C11a C 0.8699(2) -0.13752(13) 0.00583(9) 0.0622 1.0000 Uani . . . . . . . C10a C 0.8274(2) -0.15711(14) 0.04644(9) 0.0690 1.0000 Uani . . . . . . . C9a C 0.7592(2) -0.10463(13) 0.07054(8) 0.0613 1.0000 Uani . . . . . . . H1391 H 0.7275 -0.1184 0.0982 0.0724 1.0000 Uiso R . . . . . . H1381 H 0.8420 -0.2045 0.0586 0.0810 1.0000 Uiso R . . . . . . H1371 H 0.9139 -0.1726 -0.0108 0.0726 1.0000 Uiso R . . . . . . H1351 H 0.9435 -0.0838 -0.0684 0.0692 1.0000 Uiso R . . . . . . H1341 H 0.9163 0.0345 -0.1009 0.0744 1.0000 Uiso R . . . . . . H1331 H 0.8066 0.1250 -0.0621 0.0671 1.0000 Uiso R . . . . . . H521 H 0.4922 0.0318 0.0396 0.0546 1.0000 Uiso R . . . . . . H511 H 0.3811 0.1012 0.0896 0.0543 1.0000 Uiso R . . . . . . H491 H 0.3738 0.1713 0.1652 0.0592 1.0000 Uiso 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 P1a 0.0689(4) 0.0635(4) 0.0554(4) 0.0036(3) 0.0209(3) 0.0214(3) C14a 0.0511(12) 0.0510(12) 0.0386(11) 0.0005(9) 0.0133(9) 0.0072(10) C15a 0.0574(13) 0.0451(12) 0.0468(12) -0.0059(10) 0.0162(10) -0.0046(10) C22a 0.0753(17) 0.0502(14) 0.0717(16) -0.0148(12) 0.0268(13) -0.0128(12) C220a 0.0823(18) 0.0736(18) 0.0741(17) -0.0236(14) 0.0126(14) -0.0154(15) C221a 0.145(3) 0.0566(17) 0.092(2) 0.0036(16) 0.021(2) -0.0163(18) C222a 0.099(2) 0.084(2) 0.155(3) -0.049(2) 0.065(2) -0.0496(18) C16a 0.0427(12) 0.0538(13) 0.0613(14) -0.0101(11) 0.0145(10) -0.0085(10) C17a 0.0451(11) 0.0468(12) 0.0497(12) -0.0058(10) 0.0118(9) -0.0019(9) C20a 0.0533(13) 0.0525(13) 0.0721(15) -0.0136(12) 0.0177(11) 0.0035(11) C200a 0.083(2) 0.0673(18) 0.126(2) -0.0407(18) 0.0219(18) 0.0043(15) C201a 0.087(2) 0.112(3) 0.122(3) -0.020(2) -0.0084(19) 0.045(2) C202a 0.111(2) 0.086(2) 0.153(3) -0.020(2) 0.092(2) -0.0002(19) C18a 0.0478(12) 0.0467(12) 0.0515(12) -0.0053(10) 0.0067(10) -0.0054(10) C19a 0.0419(11) 0.0565(13) 0.0408(11) 0.0016(10) 0.0073(9) -0.0009(10) C21a 0.0401(12) 0.0740(16) 0.0598(14) -0.0006(12) 0.0040(10) -0.0027(11) C210a 0.0718(18) 0.143(3) 0.0780(19) -0.0011(19) 0.0194(15) -0.0446(19) C211a 0.0520(16) 0.134(3) 0.124(3) -0.048(2) -0.0018(16) -0.0243(17) C212a 0.0588(18) 0.135(3) 0.132(3) 0.036(2) -0.0234(18) 0.0038(19) C1a 0.0449(12) 0.0501(13) 0.0563(13) -0.0043(10) 0.0143(10) 0.0026(10) C2a 0.0426(11) 0.0480(12) 0.0486(12) -0.0004(10) 0.0151(9) 0.0009(9) C3a 0.0354(10) 0.0512(12) 0.0536(12) 0.0030(10) 0.0090(9) 0.0027(9) C4a 0.0395(11) 0.0511(12) 0.0456(11) -0.0024(10) 0.0071(9) -0.0002(9) C5a 0.0409(11) 0.0476(12) 0.0480(12) -0.0016(10) 0.0124(9) 0.0003(9) C6a 0.0399(11) 0.0652(15) 0.0522(13) -0.0010(11) 0.0056(9) 0.0112(10) C7a 0.0497(12) 0.0668(15) 0.0447(12) -0.0049(11) 0.0055(10) 0.0049(11) C8a 0.0374(11) 0.0476(12) 0.0526(12) -0.0063(10) 0.0067(9) 0.0054(9) C13 0.0321(10) 0.0476(12) 0.0474(11) -0.0112(9) 0.0034(8) 0.0028(9) C8b 0.0350(10) 0.0514(12) 0.0467(11) -0.0080(10) 0.0057(9) 0.0037(9) C5b 0.0430(11) 0.0419(11) 0.0494(12) -0.0008(9) 0.0107(9) 0.0032(9) C6b 0.0393(11) 0.0480(12) 0.0565(13) -0.0045(10) 0.0052(9) 0.0041(9) C7b 0.0516(13) 0.0477(12) 0.0539(13) -0.0080(10) 0.0074(10) 0.0022(10) C2b 0.0487(12) 0.0417(12) 0.0555(13) 0.0013(10) 0.0140(10) 0.0063(9) C3b 0.0503(13) 0.0533(13) 0.0568(13) 0.0029(11) 0.0051(10) 0.0123(10) C4b 0.0511(12) 0.0504(13) 0.0511(12) -0.0050(10) 0.0036(10) 0.0057(10) C1b 0.0549(13) 0.0474(13) 0.0628(14) 0.0045(11) 0.0121(11) 0.0133(10) P1b 0.0791(5) 0.0653(4) 0.0597(4) 0.0007(3) 0.0101(3) 0.0338(4) C14b 0.0566(13) 0.0497(13) 0.0484(12) -0.0052(10) 0.0068(10) 0.0151(11) C19b 0.0474(12) 0.0600(14) 0.0575(14) -0.0093(11) 0.0124(10) 0.0099(11) C21b 0.0466(13) 0.0766(18) 0.0883(19) -0.0187(15) 0.0118(13) 0.0080(12) C210b 0.0719(19) 0.113(3) 0.128(3) -0.042(2) 0.0498(18) -0.0164(18) C211b 0.0519(16) 0.089(2) 0.175(3) -0.040(2) 0.0137(18) -0.0118(15) C212b 0.0677(19) 0.140(3) 0.124(3) -0.020(2) -0.0177(19) 0.017(2) C18b 0.0514(13) 0.0466(13) 0.0710(15) -0.0020(11) 0.0194(11) 0.0025(10) C17b 0.0485(12) 0.0450(12) 0.0536(12) 0.0006(10) 0.0140(10) 0.0084(10) C16b 0.0442(12) 0.0485(12) 0.0570(13) 0.0015(10) 0.0092(10) 0.0039(10) C15b 0.0582(13) 0.0449(12) 0.0451(12) -0.0024(10) 0.0067(10) 0.0071(10) C22b 0.0699(15) 0.0456(13) 0.0613(14) 0.0048(11) 0.0067(12) 0.0006(11) C220b 0.0757(18) 0.0696(18) 0.107(2) 0.0221(16) 0.0264(16) -0.0052(14) C221b 0.100(2) 0.0681(18) 0.0733(17) 0.0183(14) 0.0086(16) -0.0022(16) C222b 0.096(2) 0.0651(17) 0.090(2) -0.0165(15) 0.0082(17) -0.0153(15) C20b 0.0538(13) 0.0491(13) 0.0705(15) 0.0075(12) 0.0157(11) 0.0102(11) C200b 0.051(2) 0.068(2) 0.176(5) 0.032(3) 0.023(2) 0.0197(17) C201b 0.102(8) 0.088(7) 0.100(8) 0.023(7) 0.030(7) 0.058(7) C202b 0.106(3) 0.060(2) 0.121(3) -0.020(2) 0.002(3) 0.030(2) C203b 0.084(8) 0.075(7) 0.185(10) 0.037(8) 0.016(8) 0.009(7) C204b 0.093(3) 0.099(3) 0.098(3) 0.041(2) 0.027(2) 0.039(2) C205b 0.112(8) 0.073(7) 0.117(8) 0.003(7) -0.003(8) 0.042(7) C9b 0.0525(13) 0.0629(15) 0.0528(13) -0.0029(11) 0.0105(10) 0.0062(11) C10b 0.0537(14) 0.0862(19) 0.0498(13) -0.0096(13) 0.0162(11) 0.0086(13) C11b 0.0426(12) 0.0727(17) 0.0582(14) -0.0244(13) 0.0070(10) 0.0121(11) C12 0.0370(11) 0.0556(13) 0.0542(13) -0.0158(11) 0.0014(9) 0.0066(10) C11a 0.0562(14) 0.0530(14) 0.0773(17) -0.0210(13) 0.0073(12) 0.0122(11) C10a 0.0702(16) 0.0481(14) 0.0891(19) -0.0012(13) 0.0115(14) 0.0144(12) C9a 0.0619(15) 0.0548(14) 0.0695(15) 0.0027(12) 0.0171(12) 0.0080(12) _refine_ls_extinction_method None _oxford_refine_ls_scale 5.94(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag P1a . C14a . 1.853(2) yes P1a . C1a . 1.660(2) yes C14a . C15a . 1.432(3) yes C14a . C19a . 1.416(3) yes C15a . C22a . 1.558(3) yes C15a . C16a . 1.386(3) yes C22a . C220a . 1.526(3) yes C22a . C221a . 1.533(4) yes C22a . C222a . 1.553(4) yes C220a . H51 . 0.971 no C220a . H52 . 0.977 no C220a . H53 . 0.976 no C221a . H93 . 0.978 no C221a . H92 . 0.967 no C221a . H91 . 0.988 no C222a . H133 . 0.966 no C222a . H132 . 0.984 no C222a . H131 . 0.987 no C16a . C17a . 1.381(3) yes C16a . H171 . 0.944 no C17a . C20a . 1.530(3) yes C17a . C18a . 1.379(3) yes C20a . C200a . 1.522(3) yes C20a . C201a . 1.531(4) yes C20a . C202a . 1.535(3) yes C200a . H202 . 0.971 no C200a . H201 . 0.979 no C200a . H203 . 0.983 no C201a . H242 . 0.965 no C201a . H243 . 0.980 no C201a . H241 . 0.985 no C202a . H281 . 0.961 no C202a . H283 . 0.956 no C202a . H282 . 0.976 no C18a . C19a . 1.400(3) yes C18a . H321 . 0.906 no C19a . C21a . 1.560(3) yes C21a . C210a . 1.522(3) yes C21a . C211a . 1.545(3) yes C21a . C212a . 1.529(3) yes C210a . H352 . 0.958 no C210a . H351 . 0.985 no C210a . H353 . 0.977 no C211a . H391 . 0.978 no C211a . H393 . 0.977 no C211a . H392 . 0.977 no C212a . H431 . 0.960 no C212a . H432 . 0.972 no C212a . H433 . 0.964 no C1a . C2a . 1.471(3) yes C1a . H491 . 0.975 no C2a . C3a . 1.394(3) yes C2a . C7a . 1.401(3) yes C3a . C4a . 1.387(3) yes C3a . H511 . 0.913 no C4a . C5a . 1.395(3) yes C4a . H521 . 0.951 no C5a . C6a . 1.391(3) yes C5a . C8a . 1.502(3) yes C6a . C7a . 1.384(3) yes C6a . H541 . 0.939 no C7a . H551 . 0.957 no C8a . C13 . 1.442(3) yes C8a . C9a . 1.375(3) yes C13 . C8b . 1.436(3) yes C13 . C12 . 1.441(3) yes C8b . C5b . 1.498(3) yes C8b . C9b . 1.379(3) yes C5b . C6b . 1.392(3) yes C5b . C4b . 1.396(3) yes C6b . C7b . 1.386(3) yes C6b . H621 . 0.969 no C7b . C2b . 1.408(3) yes C7b . H631 . 0.935 no C2b . C3b . 1.389(3) yes C2b . C1b . 1.469(3) yes C3b . C4b . 1.381(3) yes C3b . H651 . 0.962 no C4b . H661 . 0.924 no C1b . P1b . 1.656(2) yes C1b . H691 . 0.939 no P1b . C14b . 1.854(2) yes C14b . C19b . 1.423(3) yes C14b . C15b . 1.421(3) yes C19b . C21b . 1.567(3) yes C19b . C18b . 1.390(3) yes C21b . C210b . 1.531(3) yes C21b . C211b . 1.543(4) yes C21b . C212b . 1.545(4) yes C210b . H741 . 0.975 no C210b . H742 . 0.983 no C210b . H743 . 0.966 no C211b . H782 . 0.984 no C211b . H781 . 0.963 no C211b . H783 . 0.960 no C212b . H821 . 0.963 no C212b . H823 . 0.962 no C212b . H822 . 0.973 no C18b . C17b . 1.384(3) yes C18b . H861 . 0.949 no C17b . C16b . 1.380(3) yes C17b . C20b . 1.529(3) yes C16b . C15b . 1.396(3) yes C16b . H881 . 0.940 no C15b . C22b . 1.560(3) yes C22b . C220b . 1.550(3) yes C22b . C221b . 1.536(3) yes C22b . C222b . 1.532(3) yes C220b . H912 . 0.980 no C220b . H913 . 0.970 no C220b . H911 . 0.979 no C221b . H951 . 0.971 no C221b . H953 . 0.948 no C221b . H952 . 0.981 no C222b . H992 . 0.983 no C222b . H991 . 0.982 no C222b . H993 . 0.971 no C20b . C200b . 1.517(4) yes C20b . C202b . 1.554(4) yes C20b . C204b . 1.531(4) yes C200b . H1051 . 0.998 no C200b . H1053 . 0.990 no C200b . H1052 . 0.983 no C201b . H1063 . 0.957 no C201b . H1062 . 0.961 no C201b . H1061 . 0.965 no C202b . H1091 . 0.988 no C202b . H1093 . 0.971 no C202b . H1092 . 1.008 no C203b . H1101 . 0.957 no C203b . H1103 . 0.958 no C203b . H1102 . 0.959 no C204b . H1131 . 0.974 no C204b . H1133 . 0.979 no C204b . H1132 . 0.977 no C205b . H1161 . 0.959 no C205b . H1162 . 0.962 no C205b . H1163 . 0.956 no C9b . C10b . 1.402(3) yes C9b . H1331 . 0.944 no C10b . C11b . 1.347(3) yes C10b . H1341 . 0.953 no C11b . C12 . 1.410(3) yes C11b . H1351 . 0.927 no C12 . C11a . 1.408(3) yes C11a . C10a . 1.350(3) yes C11a . H1371 . 0.938 no C10a . C9a . 1.405(3) yes C10a . H1381 . 0.925 no C9a . H1391 . 0.935 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C14a . P1a . C1a . 104.00(11) yes P1a . C14a . C15a . 120.83(17) yes P1a . C14a . C19a . 119.82(16) yes C15a . C14a . C19a . 119.33(18) yes C14a . C15a . C22a . 125.22(19) yes C14a . C15a . C16a . 117.96(19) yes C22a . C15a . C16a . 116.78(19) yes C15a . C22a . C220a . 112.3(2) yes C15a . C22a . C221a . 110.1(2) yes C220a . C22a . C221a . 111.1(2) yes C15a . C22a . C222a . 111.8(2) yes C220a . C22a . C222a . 105.2(2) yes C221a . C22a . C222a . 106.0(2) yes C22a . C220a . H51 . 109.7 no C22a . C220a . H52 . 112.2 no H51 . C220a . H52 . 108.5 no C22a . C220a . H53 . 109.5 no H51 . C220a . H53 . 107.8 no H52 . C220a . H53 . 109.0 no C22a . C221a . H93 . 108.5 no C22a . C221a . H92 . 105.2 no H93 . C221a . H92 . 109.8 no C22a . C221a . H91 . 113.1 no H93 . C221a . H91 . 110.1 no H92 . C221a . H91 . 109.9 no C22a . C222a . H133 . 109.6 no C22a . C222a . H132 . 108.4 no H133 . C222a . H132 . 107.7 no C22a . C222a . H131 . 110.5 no H133 . C222a . H131 . 111.5 no H132 . C222a . H131 . 109.1 no C15a . C16a . C17a . 124.0(2) yes C15a . C16a . H171 . 117.3 no C17a . C16a . H171 . 118.8 no C16a . C17a . C20a . 119.91(19) yes C16a . C17a . C18a . 116.85(19) yes C20a . C17a . C18a . 123.2(2) yes C17a . C20a . C200a . 112.6(2) yes C17a . C20a . C201a . 109.5(2) yes C200a . C20a . C201a . 108.5(2) yes C17a . C20a . C202a . 109.4(2) yes C200a . C20a . C202a . 107.0(2) yes C201a . C20a . C202a . 109.8(2) yes C20a . C200a . H202 . 107.7 no C20a . C200a . H201 . 108.4 no H202 . C200a . H201 . 110.1 no C20a . C200a . H203 . 107.0 no H202 . C200a . H203 . 111.6 no H201 . C200a . H203 . 111.8 no C20a . C201a . H242 . 110.0 no C20a . C201a . H243 . 107.0 no H242 . C201a . H243 . 107.9 no C20a . C201a . H241 . 107.1 no H242 . C201a . H241 . 112.1 no H243 . C201a . H241 . 112.6 no C20a . C202a . H281 . 109.5 no C20a . C202a . H283 . 108.5 no H281 . C202a . H283 . 107.0 no C20a . C202a . H282 . 110.5 no H281 . C202a . H282 . 109.8 no H283 . C202a . H282 . 111.4 no C17a . C18a . C19a . 123.6(2) yes C17a . C18a . H321 . 118.2 no C19a . C18a . H321 . 118.3 no C14a . C19a . C18a . 118.16(19) yes C14a . C19a . C21a . 125.20(19) yes C18a . C19a . C21a . 116.6(2) yes C19a . C21a . C210a . 111.55(19) yes C19a . C21a . C211a . 111.93(19) yes C210a . C21a . C211a . 105.6(2) yes C19a . C21a . C212a . 111.2(2) yes C210a . C21a . C212a . 111.3(2) yes C211a . C21a . C212a . 105.0(2) yes C21a . C210a . H352 . 107.7 no C21a . C210a . H351 . 110.8 no H352 . C210a . H351 . 110.4 no C21a . C210a . H353 . 111.3 no H352 . C210a . H353 . 107.7 no H351 . C210a . H353 . 109.0 no C21a . C211a . H391 . 108.1 no C21a . C211a . H393 . 107.6 no H391 . C211a . H393 . 112.0 no C21a . C211a . H392 . 106.4 no H391 . C211a . H392 . 111.5 no H393 . C211a . H392 . 111.1 no C21a . C212a . H431 . 109.5 no C21a . C212a . H432 . 107.6 no H431 . C212a . H432 . 110.2 no C21a . C212a . H433 . 109.9 no H431 . C212a . H433 . 110.2 no H432 . C212a . H433 . 109.4 no P1a . C1a . C2a . 123.33(16) yes P1a . C1a . H491 . 119.5 no C2a . C1a . H491 . 117.0 no C1a . C2a . C3a . 121.04(19) yes C1a . C2a . C7a . 121.4(2) yes C3a . C2a . C7a . 117.55(19) yes C2a . C3a . C4a . 121.42(19) yes C2a . C3a . H511 . 119.5 no C4a . C3a . H511 . 119.1 no C3a . C4a . C5a . 120.9(2) yes C3a . C4a . H521 . 120.1 no C5a . C4a . H521 . 118.9 no C4a . C5a . C6a . 117.65(19) yes C4a . C5a . C8a . 122.91(19) yes C6a . C5a . C8a . 119.30(18) yes C5a . C6a . C7a . 121.7(2) yes C5a . C6a . H541 . 118.9 no C7a . C6a . H541 . 119.4 no C2a . C7a . C6a . 120.7(2) yes C2a . C7a . H551 . 119.7 no C6a . C7a . H551 . 119.6 no C5a . C8a . C13 . 126.07(18) yes C5a . C8a . C9a . 114.72(19) yes C13 . C8a . C9a . 119.19(19) yes C8a . C13 . C8b . 126.28(17) yes C8a . C13 . C12 . 116.96(19) yes C8b . C13 . C12 . 116.76(18) yes C13 . C8b . C5b . 125.82(17) yes C13 . C8b . C9b . 119.54(19) yes C5b . C8b . C9b . 114.62(19) yes C8b . C5b . C6b . 123.51(19) yes C8b . C5b . C4b . 118.62(19) yes C6b . C5b . C4b . 117.72(19) yes C5b . C6b . C7b . 121.3(2) yes C5b . C6b . H621 . 120.0 no C7b . C6b . H621 . 118.7 no C6b . C7b . C2b . 120.8(2) yes C6b . C7b . H631 . 119.8 no C2b . C7b . H631 . 119.4 no C7b . C2b . C3b . 117.43(19) yes C7b . C2b . C1b . 122.1(2) yes C3b . C2b . C1b . 120.4(2) yes C2b . C3b . C4b . 121.6(2) yes C2b . C3b . H651 . 119.8 no C4b . C3b . H651 . 118.6 no C5b . C4b . C3b . 121.1(2) yes C5b . C4b . H661 . 119.9 no C3b . C4b . H661 . 119.0 no C2b . C1b . P1b . 125.43(17) yes C2b . C1b . H691 . 116.4 no P1b . C1b . H691 . 118.1 no C1b . P1b . C14b . 101.24(12) yes P1b . C14b . C19b . 119.84(17) yes P1b . C14b . C15b . 120.57(18) yes C19b . C14b . C15b . 119.56(19) yes C14b . C19b . C21b . 125.3(2) yes C14b . C19b . C18b . 118.0(2) yes C21b . C19b . C18b . 116.7(2) yes C19b . C21b . C210b . 111.3(2) yes C19b . C21b . C211b . 111.5(2) yes C210b . C21b . C211b . 106.9(2) yes C19b . C21b . C212b . 111.9(2) yes C210b . C21b . C212b . 109.9(2) yes C211b . C21b . C212b . 105.1(2) yes C21b . C210b . H741 . 111.6 no C21b . C210b . H742 . 108.4 no H741 . C210b . H742 . 109.1 no C21b . C210b . H743 . 110.9 no H741 . C210b . H743 . 108.2 no H742 . C210b . H743 . 108.6 no C21b . C211b . H782 . 110.0 no C21b . C211b . H781 . 109.9 no H782 . C211b . H781 . 108.9 no C21b . C211b . H783 . 109.8 no H782 . C211b . H783 . 109.7 no H781 . C211b . H783 . 108.4 no C21b . C212b . H821 . 110.2 no C21b . C212b . H823 . 113.4 no H821 . C212b . H823 . 108.9 no C21b . C212b . H822 . 109.8 no H821 . C212b . H822 . 106.8 no H823 . C212b . H822 . 107.6 no C19b . C18b . C17b . 123.7(2) yes C19b . C18b . H861 . 119.9 no C17b . C18b . H861 . 116.4 no C18b . C17b . C16b . 116.83(19) yes C18b . C17b . C20b . 120.52(19) yes C16b . C17b . C20b . 122.60(19) yes C17b . C16b . C15b . 123.7(2) yes C17b . C16b . H881 . 118.8 no C15b . C16b . H881 . 117.5 no C14b . C15b . C16b . 117.8(2) yes C14b . C15b . C22b . 124.93(19) yes C16b . C15b . C22b . 117.2(2) yes C15b . C22b . C220b . 111.74(19) yes C15b . C22b . C221b . 110.2(2) yes C220b . C22b . C221b . 105.7(2) yes C15b . C22b . C222b . 112.45(19) yes C220b . C22b . C222b . 106.3(2) yes C221b . C22b . C222b . 110.2(2) yes C22b . C220b . H912 . 107.9 no C22b . C220b . H913 . 107.9 no H912 . C220b . H913 . 111.1 no C22b . C220b . H911 . 109.2 no H912 . C220b . H911 . 110.0 no H913 . C220b . H911 . 110.5 no C22b . C221b . H951 . 109.5 no C22b . C221b . H953 . 108.0 no H951 . C221b . H953 . 108.5 no C22b . C221b . H952 . 112.5 no H951 . C221b . H952 . 109.1 no H953 . C221b . H952 . 109.1 no C22b . C222b . H992 . 110.9 no C22b . C222b . H991 . 111.4 no H992 . C222b . H991 . 109.4 no C22b . C222b . H993 . 109.6 no H992 . C222b . H993 . 107.4 no H991 . C222b . H993 . 107.9 no C17b . C20b . C200b . 113.9(2) yes C17b . C20b . C202b . 109.0(2) yes C200b . C20b . C202b . 108.6(3) yes C17b . C20b . C204b . 110.0(2) yes C200b . C20b . C204b . 107.7(3) yes C202b . C20b . C204b . 107.4(3) yes C20b . C200b . H1051 . 106.1 no C20b . C200b . H1053 . 108.2 no H1051 . C200b . H1053 . 112.0 no C20b . C200b . H1052 . 108.4 no H1051 . C200b . H1052 . 110.8 no H1053 . C200b . H1052 . 111.2 no C20b . C201b . H1063 . 114.4 no C20b . C201b . H1062 . 108.4 no H1063 . C201b . H1062 . 107.7 no C20b . C201b . H1061 . 106.7 no H1063 . C201b . H1061 . 109.1 no H1062 . C201b . H1061 . 110.5 no C20b . C202b . H1091 . 109.0 no C20b . C202b . H1093 . 109.2 no H1091 . C202b . H1093 . 111.2 no C20b . C202b . H1092 . 104.7 no H1091 . C202b . H1092 . 109.8 no H1093 . C202b . H1092 . 112.7 no C20b . C203b . H1101 . 109.1 no C20b . C203b . H1103 . 103.6 no H1101 . C203b . H1103 . 108.4 no C20b . C203b . H1102 . 116.9 no H1101 . C203b . H1102 . 108.9 no H1103 . C203b . H1102 . 109.5 no C20b . C204b . H1131 . 107.6 no C20b . C204b . H1133 . 105.6 no H1131 . C204b . H1133 . 110.9 no C20b . C204b . H1132 . 108.3 no H1131 . C204b . H1132 . 110.5 no H1133 . C204b . H1132 . 113.6 no C20b . C205b . H1161 . 112.6 no C20b . C205b . H1162 . 107.7 no H1161 . C205b . H1162 . 109.4 no C20b . C205b . H1163 . 109.0 no H1161 . C205b . H1163 . 108.1 no H1162 . C205b . H1163 . 110.1 no C8b . C9b . C10b . 122.6(2) yes C8b . C9b . H1331 . 117.5 no C10b . C9b . H1331 . 120.0 no C9b . C10b . C11b . 119.4(2) yes C9b . C10b . H1341 . 119.0 no C11b . C10b . H1341 . 121.6 no C10b . C11b . C12 . 121.2(2) yes C10b . C11b . H1351 . 121.1 no C12 . C11b . H1351 . 117.7 no C13 . C12 . C11b . 120.6(2) yes C13 . C12 . C11a . 120.5(2) yes C11b . C12 . C11a . 118.9(2) yes C12 . C11a . C10a . 121.2(2) yes C12 . C11a . H1371 . 119.0 no C10a . C11a . H1371 . 119.8 no C11a . C10a . C9a . 119.3(2) yes C11a . C10a . H1381 . 121.3 no C9a . C10a . H1381 . 119.4 no C10a . C9a . C8a . 122.8(2) yes C10a . C9a . H1391 . 119.6 no C8a . C9a . H1391 . 117.6 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C220a . H52 . C1a . 144 0.98 2.59 3.426(4) yes C212a . H432 . C201b 3_545 167 0.97 2.49 3.441(4) yes