# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0222 _audit_creation_date 29-08-11 _audit_creation_method 'SHELXL and local programs' _audit_update_record ; ? ; _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Fanwick, Phillip E.' _publ_contact_author_address ; Department of Chemistry Purdue University 560 Oval Dr. W. Lafayette IN 47907-2084 USA ; _publ_contact_author_email pfanwick@purdue.edu _publ_contact_author_fax 1(765)4940239 _publ_contact_author_phone 1(765)4944572 _publ_requested_category ? _publ_requested_coeditor_name ? # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis of U(IV) Imidos From Tp*2U(CH2Ph) (Tp* = hydrotris(3,5-dimethylpyrazolyl)borate) by Extrusion of Bibenzyl ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses and footnotes # of all authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote E.Matson ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; S.C.Bart ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; P.E.Fanwick ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _database_code_CSD 'EMM32 ' _publ_section_experimental ; ? ; _publ_section_references ; Beurskens, P.T., Beurskens, G., deGelder, R.,Garcia-Granda, S., Gould, A.O., Smits, J.M.M. (2008). The DIRDIF2008 Program System. Crystallography Laboratory, University. of Nijmegen, The Netherlands. Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal Structure Analysis, User Manual, ,Enraf-Nonius, Delft, The Netherlands. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J., Howard, J.A.K., and Puschmann, H. (2009), J . Appl. Cryst. 42, 339-341. Otwinowski Z. & Minor, W. (1997). Methods Enzymol., 276, 307-327. Prince, E. and Nicholson, W. L. (1983).Acta Cryst A39, 407-410. Sheldrick, G.M. (2008). Acta Cryst.,A64, 112-122. Spek A.L.(1997). J. Appl. Cryst, 36, 7-13. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; data_EMM32 _database_code_depnum_ccdc_archive 'CCDC 859611' #TrackingRef '- emm32full.cif' # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _chemical_name_systematic ; ? ; _chemical_formula_sum 'C54 H75 B2 N13 U1' _chemical_formula_moiety 'C40 H59 B2 N13 U1,2(C7 H8)' _chemical_formula_structural ? _chemical_formula_weight 1165.94 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1993(4) _cell_length_b 14.0954(6) _cell_length_c 22.3766(7) _cell_angle_alpha 97.930(3) _cell_angle_beta 101.255(3) _cell_angle_gamma 106.142(3) _cell_volume 2676.03(18) _cell_measurement_reflns_used 9427 _cell_measurement_theta_min 2 _cell_measurement_theta_max 70 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' loop_ _atom_type_symbol _atom_type_radius_bond U 1.75 N 0.75 C 0.77 B 0.82 H 0.32 _diffrn_radiation_type CU-K\a _diffrn_radiation_wavelength 1.54184 _exptl_absorpt_coefficient_mu 8.911 _cell_measurement_temperature 150.0(2) _exptl_crystal_F_000 1184 # 6. DATA COLLECTION _diffrn_ambient_temperature 150.0(2) _diffrn_measurement_device_type Rigaku_Rapid_II _diffrn_radiation_monochromator 'confocal optics' _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.1763 _exptl_absorpt_correction_T_max 0.2627 _diffrn_reflns_number 50971 _diffrn_measured_fraction_theta_max 0.9240 _diffrn_reflns_theta_full 65.0 _diffrn_measured_fraction_theta_full 0.9240 _reflns_number_total 9387 _reflns_number_gt 9373 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 70.13 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_max 26 _diffrn_special_details 'mosaicity from Denzo/Scalepack is 0.51' _diffrn_standards_number 0 _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_measurement_details ; Data were collected on a Rigaku Rapid which has a quarter chi circle and a 200 degree curved image plate at a fixed distance of 127.4mm. Strategy was optimized using the CrystalClear software. The completeness is the best that can be obtained with this geometry. The missing data are not cusp data but mostly high angle data. Also the use of HKL2000/SCALEPACK lowers the number of observed data as inconsistent equivalents are removed from the data set and not included in the collected total ; # 7. REFINEMENT DATA _refine_special_details ; Outlier data were removed using a local program based on the method of Prince and Nicholson. Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_all 0.036 _refine_ls_R_factor_gt 0.036 _refine_ls_wR_factor_ref 0.096 _refine_ls_wR_factor_gt 0.096 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 9387 _refine_ls_number_parameters 652 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+4.3016P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 2.39 _refine_diff_density_min -1.46 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection 'CrystalClear(Rigaku, 2001)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1996)' _computing_structure_solution ; PATTY (DIRDIF, Beurskins, 2008) ; _computing_structure_refinement 'SHELX97 (Sheldrick, 2008)' _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLATON (Spek, 2003) ; _computing_publication_material 'SHELX97(Sheldrick, 2008) and local programs' # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _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 U1 0.035105(12) 0.463187(9) 0.268637(5) 0.02034(7) Uani 1 1 d . . . N4 0.0150(4) 0.5548(3) 0.33815(15) 0.0252(7) Uani 1 1 d . . . N11 0.0671(4) 0.3019(3) 0.20015(16) 0.0253(7) Uani 1 1 d . . . N12 0.1341(4) 0.2415(3) 0.23221(16) 0.0238(7) Uani 1 1 d . . . N21 0.2591(4) 0.4230(3) 0.33673(16) 0.0266(7) Uani 1 1 d . . . N22 0.2462(4) 0.3275(3) 0.34557(15) 0.0249(7) Uani 1 1 d . . . N31 -0.0980(4) 0.3054(3) 0.30395(16) 0.0249(7) Uani 1 1 d . . . N32 -0.0400(4) 0.2264(3) 0.30754(16) 0.0253(7) Uani 1 1 d . . . N61 -0.1805(4) 0.4473(3) 0.17073(16) 0.0246(7) Uani 1 1 d . . . N62 -0.1496(4) 0.5307(3) 0.14389(15) 0.0231(7) Uani 1 1 d . . . N71 0.2287(4) 0.5552(3) 0.20974(16) 0.0235(7) Uani 1 1 d . . . N72 0.1505(4) 0.5929(3) 0.16355(15) 0.0222(7) Uani 1 1 d . . . N81 0.0677(5) 0.7702(3) 0.12869(18) 0.0313(8) Uani 1 1 d . . . N82 -0.0089(4) 0.7184(3) 0.16767(16) 0.0256(7) Uani 1 1 d . . . C13 0.1934(5) 0.1880(3) 0.1945(2) 0.0275(9) Uani 1 1 d . . . C14 0.1638(5) 0.2125(4) 0.1367(2) 0.0293(9) Uani 1 1 d . . . C15 0.0841(5) 0.2828(3) 0.1419(2) 0.0253(9) Uani 1 1 d . . . C16 0.2761(6) 0.1157(4) 0.2152(2) 0.0372(11) Uani 1 1 d . . . C17 0.0191(6) 0.3304(4) 0.0912(2) 0.0332(11) Uani 1 1 d . . . C23 0.3595(5) 0.3325(4) 0.39609(19) 0.0307(10) Uani 1 1 d . . . C24 0.4452(5) 0.4311(4) 0.4193(2) 0.0336(10) Uani 1 1 d . . . C25 0.3807(5) 0.4864(4) 0.3811(2) 0.0304(10) Uani 1 1 d . . . C26 0.3788(6) 0.2411(4) 0.4192(2) 0.0421(12) Uani 1 1 d . . . C27 0.4306(5) 0.5972(4) 0.3822(2) 0.0361(11) Uani 1 1 d . . . C33 -0.1462(5) 0.1481(4) 0.31946(19) 0.0294(9) Uani 1 1 d . . . C34 -0.2761(5) 0.1765(4) 0.3236(2) 0.0313(10) Uani 1 1 d . . . C35 -0.2417(5) 0.2751(3) 0.31395(19) 0.0267(9) Uani 1 1 d . . . C36 -0.1195(6) 0.0492(4) 0.3264(3) 0.0408(11) Uani 1 1 d . . . C37 -0.3381(5) 0.3449(4) 0.3138(2) 0.0357(10) Uani 1 1 d . . . C41 0.0207(5) 0.6278(4) 0.39194(19) 0.0256(9) Uani 1 1 d . . . C42 0.1168(5) 0.7335(3) 0.38837(19) 0.0292(9) Uani 1 1 d . . . C43 -0.1441(5) 0.6293(4) 0.3964(2) 0.0312(10) Uani 1 1 d . . . C44 0.0963(6) 0.6000(4) 0.4519(2) 0.0317(10) Uani 1 1 d . . . C45 0.1274(6) 0.8114(4) 0.4456(2) 0.0343(10) Uani 1 1 d . . . C46 -0.0357(6) 0.8130(4) 0.4489(2) 0.0365(11) Uani 1 1 d . . . C47 -0.1334(5) 0.7074(4) 0.4537(2) 0.0357(11) Uani 1 1 d . . . C48 -0.0570(6) 0.6800(4) 0.5129(2) 0.0390(11) Uani 1 1 d . . . C49 0.1075(6) 0.6779(4) 0.5096(2) 0.0375(12) Uani 1 1 d . . . C4A 0.2044(6) 0.7824(4) 0.5045(2) 0.0398(12) Uani 1 1 d . . . C63 -0.2617(5) 0.5146(4) 0.09100(19) 0.0282(9) Uani 1 1 d . . . C64 -0.3643(5) 0.4191(4) 0.0834(2) 0.0295(9) Uani 1 1 d . . . C65 -0.3103(5) 0.3792(4) 0.13330(19) 0.0265(9) Uani 1 1 d . . . C66 -0.2683(6) 0.5921(4) 0.0519(2) 0.0370(11) Uani 1 1 d . . . C67 -0.3751(6) 0.2789(4) 0.1482(3) 0.0402(12) Uani 1 1 d . . . C73 0.2196(5) 0.5938(3) 0.11544(19) 0.0279(9) Uani 1 1 d . . . C74 0.3459(5) 0.5596(4) 0.1307(2) 0.0293(9) Uani 1 1 d . . . C75 0.3472(5) 0.5348(4) 0.1889(2) 0.0267(9) Uani 1 1 d . . . C76 0.1602(6) 0.6189(5) 0.0545(2) 0.0370(12) Uani 1 1 d . . . C77 0.4548(5) 0.4893(4) 0.2252(2) 0.0353(11) Uani 1 1 d . . . C83 -0.1085(5) 0.7648(4) 0.1861(2) 0.0309(9) Uani 1 1 d . . . C84 -0.0959(6) 0.8492(4) 0.1600(2) 0.0384(11) Uani 1 1 d . . . C85 0.0135(6) 0.8477(4) 0.1242(2) 0.0356(10) Uani 1 1 d . . . C86 -0.2107(6) 0.7263(4) 0.2279(2) 0.0375(11) Uani 1 1 d . . . C87 0.0704(7) 0.9192(4) 0.0828(3) 0.0482(13) Uani 1 1 d . . . C911 0.4681(6) 0.0892(4) 0.6115(2) 0.0406(11) Uani 1 1 d . . . C912 0.5659(7) 0.0305(4) 0.6166(3) 0.0438(12) Uani 1 1 d . . . C913 0.6761(7) 0.0435(5) 0.6708(3) 0.0551(15) Uani 1 1 d . . . C914 0.6904(8) 0.1159(6) 0.7217(3) 0.0638(18) Uani 1 1 d . . . C915 0.5925(9) 0.1757(5) 0.7178(3) 0.0621(19) Uani 1 1 d . . . C916 0.4832(8) 0.1626(4) 0.6633(3) 0.0512(14) Uani 1 1 d . . . C917 0.3514(8) 0.0756(6) 0.5518(3) 0.0606(16) Uani 1 1 d . . . C921 -0.3677(6) 0.9400(4) 0.0545(2) 0.0409(11) Uani 1 1 d . . . C922 -0.4862(7) 0.8731(5) 0.0715(3) 0.0507(14) Uani 1 1 d . . . C923 -0.5154(7) 0.8930(5) 0.1296(3) 0.0541(15) Uani 1 1 d . . . C924 -0.4233(7) 0.9804(5) 0.1722(3) 0.0507(14) Uani 1 1 d . . . C925 -0.3045(7) 1.0467(4) 0.1555(3) 0.0461(13) Uani 1 1 d . . . C926 -0.2763(6) 1.0270(4) 0.0975(3) 0.0439(12) Uani 1 1 d . . . C927 -0.3368(8) 0.9163(6) -0.0090(3) 0.0612(17) Uani 1 1 d . . . B1 0.1269(6) 0.2346(4) 0.3000(2) 0.0265(10) Uani 1 1 d . . . B2 0.0064(5) 0.6176(4) 0.1784(2) 0.0249(10) Uani 1 1 d . . . H1 0.154(6) 0.170(4) 0.309(2) 0.035(14) Uiso 1 1 d . . . H2 0.020(6) 0.612(4) 0.234(2) 0.030 Uiso 1 1 d . . . H14 0.1920 0.1867 0.1007 0.035 Uiso 1 1 calc R . . H24 0.5317 0.4569 0.4545 0.040 Uiso 1 1 calc R . . H34 -0.3698 0.1371 0.3314 0.038 Uiso 1 1 calc R . . H45 0.1915 0.8798 0.4425 0.041 Uiso 1 1 calc R . . H47 -0.2408 0.7081 0.4555 0.043 Uiso 1 1 calc R . . H49 0.1582 0.6594 0.5480 0.045 Uiso 1 1 calc R . . H64 -0.4547 0.3868 0.0503 0.035 Uiso 1 1 calc R . . H74 0.4180 0.5540 0.1063 0.035 Uiso 1 1 calc R . . H84 -0.1493 0.8974 0.1651 0.046 Uiso 1 1 calc R . . H16A 0.3523 0.1477 0.2550 0.056 Uiso 1 1 calc R . . H16B 0.3301 0.0973 0.1839 0.056 Uiso 1 1 calc R . . H16C 0.1999 0.0549 0.2201 0.056 Uiso 1 1 calc R . . H17A -0.0912 0.2921 0.0729 0.050 Uiso 1 1 calc R . . H17B 0.0774 0.3299 0.0590 0.050 Uiso 1 1 calc R . . H17C 0.0286 0.4001 0.1088 0.050 Uiso 1 1 calc R . . H26A 0.2807 0.2029 0.4274 0.063 Uiso 1 1 calc R . . H26B 0.4619 0.2618 0.4576 0.063 Uiso 1 1 calc R . . H26C 0.4064 0.1986 0.3876 0.063 Uiso 1 1 calc R . . H27A 0.5233 0.6154 0.3655 0.054 Uiso 1 1 calc R . . H27B 0.4553 0.6345 0.4251 0.054 Uiso 1 1 calc R . . H27C 0.3458 0.6142 0.3566 0.054 Uiso 1 1 calc R . . H36A -0.0936 0.0207 0.2889 0.061 Uiso 1 1 calc R . . H36B -0.2145 0.0024 0.3320 0.061 Uiso 1 1 calc R . . H36C -0.0332 0.0603 0.3627 0.061 Uiso 1 1 calc R . . H37A -0.3633 0.3559 0.3542 0.053 Uiso 1 1 calc R . . H37B -0.4349 0.3150 0.2810 0.053 Uiso 1 1 calc R . . H37C -0.2793 0.4096 0.3060 0.053 Uiso 1 1 calc R . . H42A 0.0680 0.7522 0.3502 0.035 Uiso 1 1 calc R . . H42B 0.2232 0.7337 0.3859 0.035 Uiso 1 1 calc R . . H43A -0.1966 0.6464 0.3583 0.037 Uiso 1 1 calc R . . H43B -0.2071 0.5616 0.3996 0.037 Uiso 1 1 calc R . . H44A 0.2020 0.5977 0.4504 0.038 Uiso 1 1 calc R . . H44B 0.0331 0.5323 0.4551 0.038 Uiso 1 1 calc R . . H46A -0.0859 0.8322 0.4111 0.044 Uiso 1 1 calc R . . H46B -0.0292 0.8634 0.4856 0.044 Uiso 1 1 calc R . . H48A -0.1206 0.6130 0.5170 0.047 Uiso 1 1 calc R . . H48B -0.0503 0.7303 0.5497 0.047 Uiso 1 1 calc R . . H4A1 0.3111 0.7823 0.5028 0.048 Uiso 1 1 calc R . . H4A2 0.2126 0.8327 0.5416 0.048 Uiso 1 1 calc R . . H66A -0.3093 0.6420 0.0717 0.056 Uiso 1 1 calc R . . H66B -0.3368 0.5592 0.0106 0.056 Uiso 1 1 calc R . . H66C -0.1631 0.6259 0.0479 0.056 Uiso 1 1 calc R . . H67A -0.3072 0.2733 0.1863 0.060 Uiso 1 1 calc R . . H67B -0.3807 0.2258 0.1137 0.060 Uiso 1 1 calc R . . H67C -0.4799 0.2713 0.1544 0.060 Uiso 1 1 calc R . . H76A 0.0491 0.5808 0.0384 0.055 Uiso 1 1 calc R . . H76B 0.2185 0.6009 0.0249 0.055 Uiso 1 1 calc R . . H76C 0.1741 0.6913 0.0604 0.055 Uiso 1 1 calc R . . H77A 0.5275 0.5407 0.2605 0.053 Uiso 1 1 calc R . . H77B 0.5138 0.4640 0.1983 0.053 Uiso 1 1 calc R . . H77C 0.3938 0.4335 0.2407 0.053 Uiso 1 1 calc R . . H86A -0.3112 0.6799 0.2025 0.056 Uiso 1 1 calc R . . H86B -0.2281 0.7832 0.2527 0.056 Uiso 1 1 calc R . . H86C -0.1597 0.6908 0.2557 0.056 Uiso 1 1 calc R . . H87A 0.1840 0.9363 0.0899 0.072 Uiso 1 1 calc R . . H87B 0.0427 0.9808 0.0926 0.072 Uiso 1 1 calc R . . H87C 0.0211 0.8865 0.0391 0.072 Uiso 1 1 calc R . . H912 0.5569 -0.0199 0.5819 0.053 Uiso 1 1 calc R . . H913 0.7427 0.0026 0.6732 0.066 Uiso 1 1 calc R . . H914 0.7664 0.1249 0.7593 0.077 Uiso 1 1 calc R . . H915 0.6013 0.2254 0.7527 0.074 Uiso 1 1 calc R . . H916 0.4172 0.2039 0.6607 0.061 Uiso 1 1 calc R . . H91A 0.3852 0.0448 0.5172 0.091 Uiso 1 1 calc R . . H91B 0.3427 0.1414 0.5454 0.091 Uiso 1 1 calc R . . H91C 0.2496 0.0317 0.5535 0.091 Uiso 1 1 calc R . . H922 -0.5486 0.8125 0.0429 0.061 Uiso 1 1 calc R . . H923 -0.5984 0.8468 0.1403 0.065 Uiso 1 1 calc R . . H924 -0.4420 0.9943 0.2123 0.061 Uiso 1 1 calc R . . H925 -0.2410 1.1068 0.1843 0.055 Uiso 1 1 calc R . . H926 -0.1935 1.0736 0.0869 0.053 Uiso 1 1 calc R . . H92A -0.3437 0.8450 -0.0189 0.092 Uiso 1 1 calc R . . H92B -0.2322 0.9585 -0.0088 0.092 Uiso 1 1 calc R . . H92C -0.4146 0.9300 -0.0404 0.092 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 U1 0.02162(9) 0.02223(12) 0.02040(9) 0.00889(7) 0.00841(6) 0.00612(6) N4 0.0304(18) 0.026(2) 0.0209(16) 0.0105(15) 0.0104(13) -0.0002(13) N11 0.0321(18) 0.024(2) 0.0233(16) 0.0124(15) 0.0082(14) 0.0059(14) N12 0.0243(16) 0.024(2) 0.0276(17) 0.0108(14) 0.0105(13) 0.0080(14) N21 0.0260(17) 0.028(2) 0.0260(17) 0.0104(15) 0.0057(14) 0.0046(14) N22 0.0278(17) 0.031(2) 0.0199(15) 0.0137(15) 0.0067(13) 0.0084(14) N31 0.0242(16) 0.026(2) 0.0284(17) 0.0078(15) 0.0129(14) 0.0086(14) N32 0.0270(18) 0.025(2) 0.0257(17) 0.0075(15) 0.0090(14) 0.0083(14) N61 0.0234(16) 0.026(2) 0.0259(16) 0.0089(15) 0.0082(13) 0.0051(14) N62 0.0292(17) 0.0185(19) 0.0222(16) 0.0070(14) 0.0077(13) 0.0050(13) N71 0.0216(15) 0.023(2) 0.0296(17) 0.0093(14) 0.0085(13) 0.0088(14) N72 0.0237(16) 0.0202(19) 0.0260(16) 0.0079(14) 0.0099(13) 0.0080(13) N81 0.036(2) 0.025(2) 0.0339(19) 0.0072(16) 0.0126(16) 0.0092(15) N82 0.0291(17) 0.020(2) 0.0301(17) 0.0074(15) 0.0115(14) 0.0096(14) C13 0.027(2) 0.024(2) 0.034(2) 0.0090(18) 0.0118(17) 0.0048(17) C14 0.035(2) 0.028(3) 0.031(2) 0.0119(19) 0.0181(18) 0.0064(17) C15 0.029(2) 0.023(2) 0.0244(19) 0.0064(18) 0.0107(16) 0.0041(16) C16 0.045(3) 0.037(3) 0.040(2) 0.025(2) 0.016(2) 0.010(2) C17 0.046(3) 0.031(3) 0.029(2) 0.017(2) 0.015(2) 0.0087(19) C23 0.027(2) 0.047(3) 0.026(2) 0.020(2) 0.0100(16) 0.0079(19) C24 0.026(2) 0.052(3) 0.0241(19) 0.017(2) 0.0082(16) 0.0023(19) C25 0.0228(19) 0.043(3) 0.027(2) 0.0139(19) 0.0079(16) 0.0025(18) C26 0.049(3) 0.055(4) 0.034(2) 0.030(3) 0.008(2) 0.020(2) C27 0.026(2) 0.031(3) 0.044(3) 0.003(2) 0.0092(19) -0.004(2) C33 0.033(2) 0.031(3) 0.026(2) 0.0074(19) 0.0124(17) 0.0113(18) C34 0.025(2) 0.038(3) 0.031(2) 0.0055(19) 0.0138(17) 0.0089(18) C35 0.026(2) 0.028(3) 0.028(2) 0.0065(18) 0.0108(16) 0.0081(17) C36 0.043(3) 0.032(3) 0.053(3) 0.012(2) 0.018(2) 0.019(2) C37 0.027(2) 0.034(3) 0.048(3) 0.009(2) 0.015(2) 0.006(2) C41 0.027(2) 0.030(3) 0.0231(19) 0.0093(18) 0.0113(16) 0.0081(17) C42 0.033(2) 0.029(3) 0.027(2) 0.0089(19) 0.0098(17) 0.0056(17) C43 0.026(2) 0.036(3) 0.029(2) 0.0066(19) 0.0103(17) 0.0019(18) C44 0.039(2) 0.038(3) 0.027(2) 0.019(2) 0.0135(18) 0.0135(19) C45 0.037(2) 0.026(3) 0.039(2) 0.006(2) 0.0142(19) 0.0047(19) C46 0.043(3) 0.037(3) 0.034(2) 0.021(2) 0.0118(19) 0.0011(19) C47 0.030(2) 0.044(3) 0.036(2) 0.014(2) 0.0148(18) 0.000(2) C48 0.044(3) 0.045(3) 0.030(2) 0.012(2) 0.021(2) 0.003(2) C49 0.044(3) 0.048(3) 0.025(2) 0.020(2) 0.012(2) 0.007(2) C4A 0.031(2) 0.051(3) 0.032(2) 0.012(2) 0.0057(18) -0.004(2) C63 0.026(2) 0.038(3) 0.026(2) 0.0159(19) 0.0080(16) 0.0075(18) C64 0.0244(19) 0.032(3) 0.029(2) 0.0080(18) 0.0036(16) 0.0006(17) C65 0.0249(19) 0.029(3) 0.0255(19) 0.0095(18) 0.0052(16) 0.0034(17) C66 0.036(2) 0.049(3) 0.028(2) 0.017(2) 0.0024(18) 0.015(2) C67 0.035(2) 0.033(3) 0.047(3) 0.006(2) 0.004(2) 0.011(2) C73 0.031(2) 0.029(3) 0.027(2) 0.0115(18) 0.0111(17) 0.0061(17) C74 0.027(2) 0.036(3) 0.031(2) 0.0119(19) 0.0149(17) 0.0112(18) C75 0.0227(19) 0.031(3) 0.030(2) 0.0092(18) 0.0128(16) 0.0077(17) C76 0.042(3) 0.050(3) 0.030(2) 0.022(2) 0.016(2) 0.015(2) C77 0.029(2) 0.046(3) 0.041(2) 0.021(2) 0.0143(19) 0.016(2) C83 0.029(2) 0.031(3) 0.037(2) 0.0146(19) 0.0118(18) 0.0074(19) C84 0.043(3) 0.035(3) 0.045(3) 0.022(2) 0.012(2) 0.011(2) C85 0.042(3) 0.029(3) 0.039(2) 0.014(2) 0.011(2) 0.013(2) C86 0.038(2) 0.042(3) 0.042(3) 0.019(2) 0.019(2) 0.016(2) C87 0.060(3) 0.037(3) 0.056(3) 0.019(3) 0.020(3) 0.022(3) C911 0.046(3) 0.033(3) 0.038(3) 0.001(2) 0.016(2) 0.010(2) C912 0.052(3) 0.033(3) 0.051(3) 0.009(2) 0.025(2) 0.013(2) C913 0.049(3) 0.056(4) 0.062(4) 0.009(3) 0.018(3) 0.027(3) C914 0.065(4) 0.056(4) 0.054(4) -0.005(3) 0.006(3) 0.018(3) C915 0.084(5) 0.040(4) 0.039(3) -0.015(3) 0.019(3) -0.002(2) C916 0.068(4) 0.030(3) 0.059(3) 0.008(3) 0.032(3) 0.013(2) C917 0.067(4) 0.067(5) 0.054(3) 0.030(3) 0.012(3) 0.016(3) C921 0.041(3) 0.040(3) 0.042(3) 0.012(2) 0.014(2) 0.007(2) C922 0.045(3) 0.048(4) 0.051(3) 0.002(3) 0.014(2) 0.005(3) C923 0.046(3) 0.068(4) 0.053(3) 0.016(3) 0.023(3) 0.019(3) C924 0.058(3) 0.062(4) 0.045(3) 0.035(3) 0.019(3) 0.011(3) C925 0.056(3) 0.038(3) 0.044(3) 0.023(3) 0.004(2) 0.005(2) C926 0.041(3) 0.037(3) 0.056(3) 0.013(2) 0.010(2) 0.018(2) C927 0.059(4) 0.073(5) 0.047(3) 0.008(3) 0.023(3) 0.007(3) B1 0.028(2) 0.028(3) 0.032(2) 0.014(2) 0.0125(19) 0.011(2) B2 0.024(2) 0.028(3) 0.027(2) 0.013(2) 0.0068(17) 0.0081(18) # 10. MOLECULAR GEOMETRY _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_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N4 1.953(3) . . ? U1 N31 2.533(4) . . ? U1 N21 2.560(3) . . ? U1 N71 2.587(3) . . ? U1 N61 2.590(3) . . ? U1 N11 2.682(4) . . ? U1 H2 2.37(5) . . ? N4 C41 1.454(5) . . ? N11 C15 1.342(5) . . ? N11 N12 1.380(5) . . ? N12 C13 1.347(5) . . ? N12 B1 1.547(6) . . ? N21 C25 1.342(6) . . ? N21 N22 1.364(5) . . ? N22 C23 1.359(5) . . ? N22 B1 1.534(6) . . ? N31 C35 1.345(5) . . ? N31 N32 1.367(5) . . ? N32 C33 1.352(6) . . ? N32 B1 1.552(6) . . ? N61 C65 1.341(6) . . ? N61 N62 1.378(5) . . ? N62 C63 1.354(5) . . ? N62 B2 1.576(6) . . ? N71 C75 1.350(5) . . ? N71 N72 1.394(5) . . ? N72 C73 1.353(5) . . ? N72 B2 1.544(5) . . ? N81 C85 1.329(6) . . ? N81 N82 1.385(5) . . ? N82 C83 1.358(6) . . ? N82 B2 1.514(6) . . ? C13 C14 1.379(6) . . ? C13 C16 1.502(6) . . ? C14 C15 1.392(6) . . ? C14 H14 0.9500 . . ? C15 C17 1.503(6) . . ? C16 H16A 0.9800 . . ? C16 H16B 0.9800 . . ? C16 H16C 0.9800 . . ? C17 H17A 0.9800 . . ? C17 H17B 0.9800 . . ? C17 H17C 0.9800 . . ? C23 C24 1.361(7) . . ? C23 C26 1.494(7) . . ? C24 C25 1.390(7) . . ? C24 H24 0.9500 . . ? C25 C27 1.495(8) . . ? C26 H26A 0.9800 . . ? C26 H26B 0.9800 . . ? C26 H26C 0.9800 . . ? C27 H27A 0.9800 . . ? C27 H27B 0.9800 . . ? C27 H27C 0.9800 . . ? C33 C34 1.377(6) . . ? C33 C36 1.503(7) . . ? C34 C35 1.394(7) . . ? C34 H34 0.9500 . . ? C35 C37 1.497(6) . . ? C36 H36A 0.9800 . . ? C36 H36B 0.9800 . . ? C36 H36C 0.9800 . . ? C37 H37A 0.9800 . . ? C37 H37B 0.9800 . . ? C37 H37C 0.9800 . . ? C41 C42 1.528(7) . . ? C41 C44 1.540(6) . . ? C41 C43 1.544(6) . . ? C42 C45 1.536(6) . . ? C42 H42A 0.9900 . . ? C42 H42B 0.9900 . . ? C43 C47 1.539(6) . . ? C43 H43A 0.9900 . . ? C43 H43B 0.9900 . . ? C44 C49 1.540(7) . . ? C44 H44A 0.9900 . . ? C44 H44B 0.9900 . . ? C45 C46 1.522(6) . . ? C45 C4A 1.532(7) . . ? C45 H45 1.0000 . . ? C46 C47 1.541(8) . . ? C46 H46A 0.9900 . . ? C46 H46B 0.9900 . . ? C47 C48 1.525(7) . . ? C47 H47 1.0000 . . ? C48 C49 1.538(7) . . ? C48 H48A 0.9900 . . ? C48 H48B 0.9900 . . ? C49 C4A 1.528(8) . . ? C49 H49 1.0000 . . ? C4A H4A1 0.9900 . . ? C4A H4A2 0.9900 . . ? C63 C64 1.379(7) . . ? C63 C66 1.498(6) . . ? C64 C65 1.386(6) . . ? C64 H64 0.9500 . . ? C65 C67 1.485(7) . . ? C66 H66A 0.9800 . . ? C66 H66B 0.9800 . . ? C66 H66C 0.9800 . . ? C67 H67A 0.9800 . . ? C67 H67B 0.9800 . . ? C67 H67C 0.9800 . . ? C73 C74 1.379(6) . . ? C73 C76 1.493(6) . . ? C74 C75 1.392(6) . . ? C74 H74 0.9500 . . ? C75 C77 1.495(6) . . ? C76 H76A 0.9800 . . ? C76 H76B 0.9800 . . ? C76 H76C 0.9800 . . ? C77 H77A 0.9800 . . ? C77 H77B 0.9800 . . ? C77 H77C 0.9800 . . ? C83 C84 1.383(7) . . ? C83 C86 1.500(6) . . ? C84 C85 1.406(7) . . ? C84 H84 0.9500 . . ? C85 C87 1.517(7) . . ? C86 H86A 0.9800 . . ? C86 H86B 0.9800 . . ? C86 H86C 0.9800 . . ? C87 H87A 0.9800 . . ? C87 H87B 0.9800 . . ? C87 H87C 0.9800 . . ? C911 C912 1.381(8) . . ? C911 C916 1.400(8) . . ? C911 C917 1.494(8) . . ? C912 C913 1.375(9) . . ? C912 H912 0.9500 . . ? C913 C914 1.380(10) . . ? C913 H913 0.9500 . . ? C914 C915 1.392(11) . . ? C914 H914 0.9500 . . ? C915 C916 1.374(9) . . ? C915 H915 0.9500 . . ? C916 H916 0.9500 . . ? C917 H91A 0.9800 . . ? C917 H91B 0.9800 . . ? C917 H91C 0.9800 . . ? C921 C922 1.382(8) . . ? C921 C926 1.387(8) . . ? C921 C927 1.513(8) . . ? C922 C923 1.386(8) . . ? C922 H922 0.9500 . . ? C923 C924 1.387(9) . . ? C923 H923 0.9500 . . ? C924 C925 1.378(9) . . ? C924 H924 0.9500 . . ? C925 C926 1.377(8) . . ? C925 H925 0.9500 . . ? C926 H926 0.9500 . . ? C927 H92A 0.9800 . . ? C927 H92B 0.9800 . . ? C927 H92C 0.9800 . . ? B1 H1 1.05(6) . . ? B2 H2 1.23(5) . . ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 U1 N31 94.11(14) . . . ? N4 U1 N21 92.68(13) . . . ? N31 U1 N21 75.73(12) . . . ? N4 U1 N71 112.21(14) . . . ? N31 U1 N71 150.38(11) . . . ? N21 U1 N71 89.22(11) . . . ? N4 U1 N61 109.24(13) . . . ? N31 U1 N61 98.53(11) . . . ? N21 U1 N61 157.80(12) . . . ? N71 U1 N61 85.78(10) . . . ? N4 U1 N11 162.05(13) . . . ? N31 U1 N11 70.58(11) . . . ? N21 U1 N11 74.83(11) . . . ? N71 U1 N11 80.99(11) . . . ? N61 U1 N11 83.02(11) . . . ? N4 U1 H2 72.7(12) . . . ? N31 U1 H2 148.6(12) . . . ? N21 U1 H2 131.8(12) . . . ? N71 U1 H2 57.7(12) . . . ? N61 U1 H2 61.6(12) . . . ? N11 U1 H2 125.2(12) . . . ? C41 N4 U1 173.0(3) . . . ? C15 N11 N12 106.3(3) . . . ? C15 N11 U1 132.5(3) . . . ? N12 N11 U1 116.7(2) . . . ? C13 N12 N11 109.9(3) . . . ? C13 N12 B1 127.5(4) . . . ? N11 N12 B1 122.5(3) . . . ? C25 N21 N22 107.6(3) . . . ? C25 N21 U1 128.4(3) . . . ? N22 N21 U1 121.6(2) . . . ? C23 N22 N21 108.6(4) . . . ? C23 N22 B1 129.5(4) . . . ? N21 N22 B1 121.8(3) . . . ? C35 N31 N32 106.4(4) . . . ? C35 N31 U1 129.2(3) . . . ? N32 N31 U1 123.7(2) . . . ? C33 N32 N31 110.0(3) . . . ? C33 N32 B1 128.7(4) . . . ? N31 N32 B1 121.2(3) . . . ? C65 N61 N62 106.9(3) . . . ? C65 N61 U1 140.1(3) . . . ? N62 N61 U1 112.8(2) . . . ? C63 N62 N61 109.5(3) . . . ? C63 N62 B2 135.4(4) . . . ? N61 N62 B2 115.0(3) . . . ? C75 N71 N72 106.2(3) . . . ? C75 N71 U1 133.5(3) . . . ? N72 N71 U1 109.8(2) . . . ? C73 N72 N71 109.4(3) . . . ? C73 N72 B2 136.8(3) . . . ? N71 N72 B2 113.7(3) . . . ? C85 N81 N82 105.5(4) . . . ? C83 N82 N81 110.1(4) . . . ? C83 N82 B2 127.6(4) . . . ? N81 N82 B2 121.7(3) . . . ? N12 C13 C14 107.9(4) . . . ? N12 C13 C16 123.4(4) . . . ? C14 C13 C16 128.8(4) . . . ? C13 C14 C15 106.1(4) . . . ? C13 C14 H14 127.00 . . . ? C15 C14 H14 127.00 . . . ? N11 C15 C14 109.9(4) . . . ? N11 C15 C17 122.8(4) . . . ? C14 C15 C17 127.3(4) . . . ? C13 C16 H16A 109.50 . . . ? C13 C16 H16B 109.50 . . . ? H16A C16 H16B 109.50 . . . ? C13 C16 H16C 109.50 . . . ? H16A C16 H16C 109.50 . . . ? H16B C16 H16C 109.50 . . . ? C15 C17 H17A 109.50 . . . ? C15 C17 H17B 109.50 . . . ? H17A C17 H17B 109.50 . . . ? C15 C17 H17C 109.50 . . . ? H17A C17 H17C 109.50 . . . ? H17B C17 H17C 109.50 . . . ? N22 C23 C24 108.5(4) . . . ? N22 C23 C26 122.7(4) . . . ? C24 C23 C26 128.8(4) . . . ? C23 C24 C25 106.3(4) . . . ? C23 C24 H24 126.90 . . . ? C25 C24 H24 126.90 . . . ? N21 C25 C24 109.1(4) . . . ? N21 C25 C27 120.7(4) . . . ? C24 C25 C27 130.2(4) . . . ? C23 C26 H26A 109.50 . . . ? C23 C26 H26B 109.50 . . . ? H26A C26 H26B 109.50 . . . ? C23 C26 H26C 109.50 . . . ? H26A C26 H26C 109.50 . . . ? H26B C26 H26C 109.50 . . . ? C25 C27 H27A 109.50 . . . ? C25 C27 H27B 109.50 . . . ? H27A C27 H27B 109.50 . . . ? C25 C27 H27C 109.50 . . . ? H27A C27 H27C 109.50 . . . ? H27B C27 H27C 109.50 . . . ? N32 C33 C34 107.8(4) . . . ? N32 C33 C36 123.7(4) . . . ? C34 C33 C36 128.5(4) . . . ? C33 C34 C35 105.8(4) . . . ? C33 C34 H34 127.10 . . . ? C35 C34 H34 127.10 . . . ? N31 C35 C34 109.9(4) . . . ? N31 C35 C37 120.3(4) . . . ? C34 C35 C37 129.8(4) . . . ? C33 C36 H36A 109.50 . . . ? C33 C36 H36B 109.50 . . . ? H36A C36 H36B 109.50 . . . ? C33 C36 H36C 109.50 . . . ? H36A C36 H36C 109.50 . . . ? H36B C36 H36C 109.50 . . . ? C35 C37 H37A 109.50 . . . ? C35 C37 H37B 109.50 . . . ? H37A C37 H37B 109.50 . . . ? C35 C37 H37C 109.50 . . . ? H37A C37 H37C 109.50 . . . ? H37B C37 H37C 109.50 . . . ? N4 C41 C42 110.1(3) . . . ? N4 C41 C44 109.7(4) . . . ? C42 C41 C44 109.1(4) . . . ? N4 C41 C43 111.8(4) . . . ? C42 C41 C43 108.7(4) . . . ? C44 C41 C43 107.4(4) . . . ? C41 C42 C45 110.9(4) . . . ? C41 C42 H42A 109.50 . . . ? C45 C42 H42A 109.50 . . . ? C41 C42 H42B 109.50 . . . ? C45 C42 H42B 109.50 . . . ? H42A C42 H42B 108.00 . . . ? C47 C43 C41 110.3(4) . . . ? C47 C43 H43A 109.60 . . . ? C41 C43 H43A 109.60 . . . ? C47 C43 H43B 109.60 . . . ? C41 C43 H43B 109.60 . . . ? H43A C43 H43B 108.10 . . . ? C41 C44 C49 110.6(4) . . . ? C41 C44 H44A 109.50 . . . ? C49 C44 H44A 109.50 . . . ? C41 C44 H44B 109.50 . . . ? C49 C44 H44B 109.50 . . . ? H44A C44 H44B 108.10 . . . ? C46 C45 C4A 109.4(4) . . . ? C46 C45 C42 109.7(4) . . . ? C4A C45 C42 109.1(4) . . . ? C46 C45 H45 109.50 . . . ? C4A C45 H45 109.50 . . . ? C42 C45 H45 109.50 . . . ? C45 C46 C47 109.1(4) . . . ? C45 C46 H46A 109.90 . . . ? C47 C46 H46A 109.90 . . . ? C45 C46 H46B 109.90 . . . ? C47 C46 H46B 109.90 . . . ? H46A C46 H46B 108.30 . . . ? C48 C47 C43 110.0(4) . . . ? C48 C47 C46 109.3(4) . . . ? C43 C47 C46 109.8(4) . . . ? C48 C47 H47 109.20 . . . ? C43 C47 H47 109.20 . . . ? C46 C47 H47 109.20 . . . ? C47 C48 C49 109.0(4) . . . ? C47 C48 H48A 109.90 . . . ? C49 C48 H48A 109.90 . . . ? C47 C48 H48B 109.90 . . . ? C49 C48 H48B 109.90 . . . ? H48A C48 H48B 108.30 . . . ? C4A C49 C48 109.0(4) . . . ? C4A C49 C44 109.4(4) . . . ? C48 C49 C44 109.6(4) . . . ? C4A C49 H49 109.60 . . . ? C48 C49 H49 109.60 . . . ? C44 C49 H49 109.60 . . . ? C49 C4A C45 109.9(4) . . . ? C49 C4A H4A1 109.70 . . . ? C45 C4A H4A1 109.70 . . . ? C49 C4A H4A2 109.70 . . . ? C45 C4A H4A2 109.70 . . . ? H4A1 C4A H4A2 108.20 . . . ? N62 C63 C64 107.4(4) . . . ? N62 C63 C66 123.5(4) . . . ? C64 C63 C66 129.0(4) . . . ? C63 C64 C65 106.8(4) . . . ? C63 C64 H64 126.60 . . . ? C65 C64 H64 126.60 . . . ? N61 C65 C64 109.5(4) . . . ? N61 C65 C67 120.9(4) . . . ? C64 C65 C67 129.7(4) . . . ? C63 C66 H66A 109.50 . . . ? C63 C66 H66B 109.50 . . . ? H66A C66 H66B 109.50 . . . ? C63 C66 H66C 109.50 . . . ? H66A C66 H66C 109.50 . . . ? H66B C66 H66C 109.50 . . . ? C65 C67 H67A 109.50 . . . ? C65 C67 H67B 109.50 . . . ? H67A C67 H67B 109.50 . . . ? C65 C67 H67C 109.50 . . . ? H67A C67 H67C 109.50 . . . ? H67B C67 H67C 109.50 . . . ? N72 C73 C74 107.9(4) . . . ? N72 C73 C76 125.5(4) . . . ? C74 C73 C76 126.4(4) . . . ? C73 C74 C75 106.6(4) . . . ? C73 C74 H74 126.70 . . . ? C75 C74 H74 126.70 . . . ? N71 C75 C74 109.7(4) . . . ? N71 C75 C77 121.9(4) . . . ? C74 C75 C77 128.4(4) . . . ? C73 C76 H76A 109.50 . . . ? C73 C76 H76B 109.50 . . . ? H76A C76 H76B 109.50 . . . ? C73 C76 H76C 109.50 . . . ? H76A C76 H76C 109.50 . . . ? H76B C76 H76C 109.50 . . . ? C75 C77 H77A 109.50 . . . ? C75 C77 H77B 109.50 . . . ? H77A C77 H77B 109.50 . . . ? C75 C77 H77C 109.50 . . . ? H77A C77 H77C 109.50 . . . ? H77B C77 H77C 109.50 . . . ? N82 C83 C84 108.1(4) . . . ? N82 C83 C86 123.2(4) . . . ? C84 C83 C86 128.7(4) . . . ? C83 C84 C85 104.6(4) . . . ? C83 C84 H84 127.70 . . . ? C85 C84 H84 127.70 . . . ? N81 C85 C84 111.7(4) . . . ? N81 C85 C87 119.3(5) . . . ? C84 C85 C87 129.0(5) . . . ? C83 C86 H86A 109.50 . . . ? C83 C86 H86B 109.50 . . . ? H86A C86 H86B 109.50 . . . ? C83 C86 H86C 109.50 . . . ? H86A C86 H86C 109.50 . . . ? H86B C86 H86C 109.50 . . . ? C85 C87 H87A 109.50 . . . ? C85 C87 H87B 109.50 . . . ? H87A C87 H87B 109.50 . . . ? C85 C87 H87C 109.50 . . . ? H87A C87 H87C 109.50 . . . ? H87B C87 H87C 109.50 . . . ? C912 C911 C916 118.3(5) . . . ? C912 C911 C917 120.6(5) . . . ? C916 C911 C917 121.1(6) . . . ? C913 C912 C911 121.2(6) . . . ? C913 C912 H912 119.40 . . . ? C911 C912 H912 119.40 . . . ? C912 C913 C914 120.2(6) . . . ? C912 C913 H913 119.90 . . . ? C914 C913 H913 119.90 . . . ? C913 C914 C915 119.5(6) . . . ? C913 C914 H914 120.20 . . . ? C915 C914 H914 120.20 . . . ? C916 C915 C914 120.0(6) . . . ? C916 C915 H915 120.00 . . . ? C914 C915 H915 120.00 . . . ? C915 C916 C911 120.7(6) . . . ? C915 C916 H916 119.60 . . . ? C911 C916 H916 119.60 . . . ? C911 C917 H91A 109.50 . . . ? C911 C917 H91B 109.50 . . . ? H91A C917 H91B 109.50 . . . ? C911 C917 H91C 109.50 . . . ? H91A C917 H91C 109.50 . . . ? H91B C917 H91C 109.50 . . . ? C922 C921 C926 118.4(5) . . . ? C922 C921 C927 120.2(5) . . . ? C926 C921 C927 121.4(5) . . . ? C921 C922 C923 121.1(6) . . . ? C921 C922 H922 119.50 . . . ? C923 C922 H922 119.50 . . . ? C922 C923 C924 120.0(6) . . . ? C922 C923 H923 120.00 . . . ? C924 C923 H923 120.00 . . . ? C925 C924 C923 118.9(5) . . . ? C925 C924 H924 120.50 . . . ? C923 C924 H924 120.50 . . . ? C926 C925 C924 121.0(5) . . . ? C926 C925 H925 119.50 . . . ? C924 C925 H925 119.50 . . . ? C925 C926 C921 120.7(5) . . . ? C925 C926 H926 119.70 . . . ? C921 C926 H926 119.70 . . . ? C921 C927 H92A 109.50 . . . ? C921 C927 H92B 109.50 . . . ? H92A C927 H92B 109.50 . . . ? C921 C927 H92C 109.50 . . . ? H92A C927 H92C 109.50 . . . ? H92B C927 H92C 109.50 . . . ? N22 B1 N12 110.4(4) . . . ? N22 B1 N32 110.1(3) . . . ? N12 B1 N32 109.7(3) . . . ? N22 B1 H1 109(3) . . . ? N12 B1 H1 108(3) . . . ? N32 B1 H1 110(3) . . . ? N82 B2 N72 116.2(4) . . . ? N82 B2 N62 109.9(3) . . . ? N72 B2 N62 111.5(3) . . . ? N82 B2 H2 111(2) . . . ? N72 B2 H2 103(2) . . . ? N62 B2 H2 104(2) . . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N31 U1 N4 C41 119(3) . . . . ? N21 U1 N4 C41 43(3) . . . . ? N71 U1 N4 C41 -47(3) . . . . ? N61 U1 N4 C41 -140(3) . . . . ? N11 U1 N4 C41 88(3) . . . . ? N4 U1 N11 C15 -175.3(4) . . . . ? N31 U1 N11 C15 152.0(4) . . . . ? N21 U1 N11 C15 -128.1(4) . . . . ? N71 U1 N11 C15 -36.5(4) . . . . ? N61 U1 N11 C15 50.4(4) . . . . ? N4 U1 N11 N12 -22.9(6) . . . . ? N31 U1 N11 N12 -55.6(3) . . . . ? N21 U1 N11 N12 24.3(3) . . . . ? N71 U1 N11 N12 115.9(3) . . . . ? N61 U1 N11 N12 -157.3(3) . . . . ? C15 N11 N12 C13 1.1(5) . . . . ? U1 N11 N12 C13 -158.0(3) . . . . ? C15 N11 N12 B1 -174.9(4) . . . . ? U1 N11 N12 B1 26.0(5) . . . . ? N4 U1 N21 C25 -41.4(4) . . . . ? N31 U1 N21 C25 -135.0(4) . . . . ? N71 U1 N21 C25 70.8(4) . . . . ? N61 U1 N21 C25 147.6(3) . . . . ? N11 U1 N21 C25 151.6(4) . . . . ? N4 U1 N21 N22 118.3(3) . . . . ? N31 U1 N21 N22 24.7(3) . . . . ? N71 U1 N21 N22 -129.5(3) . . . . ? N61 U1 N21 N22 -52.7(5) . . . . ? N11 U1 N21 N22 -48.6(3) . . . . ? C25 N21 N22 C23 0.7(4) . . . . ? U1 N21 N22 C23 -162.7(3) . . . . ? C25 N21 N22 B1 -175.1(4) . . . . ? U1 N21 N22 B1 21.4(5) . . . . ? N4 U1 N31 C35 58.0(4) . . . . ? N21 U1 N31 C35 149.7(4) . . . . ? N71 U1 N31 C35 -148.7(3) . . . . ? N61 U1 N31 C35 -52.2(4) . . . . ? N11 U1 N31 C35 -131.6(4) . . . . ? N4 U1 N31 N32 -132.2(3) . . . . ? N21 U1 N31 N32 -40.5(3) . . . . ? N71 U1 N31 N32 21.1(4) . . . . ? N61 U1 N31 N32 117.6(3) . . . . ? N11 U1 N31 N32 38.1(3) . . . . ? C35 N31 N32 C33 0.1(5) . . . . ? U1 N31 N32 C33 -171.6(3) . . . . ? C35 N31 N32 B1 -178.4(4) . . . . ? U1 N31 N32 B1 9.9(5) . . . . ? N4 U1 N61 C65 -111.9(4) . . . . ? N31 U1 N61 C65 -14.5(4) . . . . ? N21 U1 N61 C65 58.5(6) . . . . ? N71 U1 N61 C65 136.0(4) . . . . ? N11 U1 N61 C65 54.6(4) . . . . ? N4 U1 N61 N62 75.7(3) . . . . ? N31 U1 N61 N62 173.1(2) . . . . ? N21 U1 N61 N62 -113.9(3) . . . . ? N71 U1 N61 N62 -36.4(2) . . . . ? N11 U1 N61 N62 -117.8(3) . . . . ? C65 N61 N62 C63 1.3(4) . . . . ? U1 N61 N62 C63 176.2(2) . . . . ? C65 N61 N62 B2 -175.9(3) . . . . ? U1 N61 N62 B2 -1.0(4) . . . . ? N4 U1 N71 C75 133.6(4) . . . . ? N31 U1 N71 C75 -17.5(5) . . . . ? N21 U1 N71 C75 41.0(4) . . . . ? N61 U1 N71 C75 -117.3(4) . . . . ? N11 U1 N71 C75 -33.7(4) . . . . ? N4 U1 N71 N72 -87.6(3) . . . . ? N31 U1 N71 N72 121.3(3) . . . . ? N21 U1 N71 N72 179.8(3) . . . . ? N61 U1 N71 N72 21.5(2) . . . . ? N11 U1 N71 N72 105.1(3) . . . . ? C75 N71 N72 C73 0.9(5) . . . . ? U1 N71 N72 C73 -149.3(3) . . . . ? C75 N71 N72 B2 178.2(4) . . . . ? U1 N71 N72 B2 28.0(4) . . . . ? C85 N81 N82 C83 0.2(5) . . . . ? C85 N81 N82 B2 172.5(4) . . . . ? N11 N12 C13 C14 -0.6(5) . . . . ? B1 N12 C13 C14 175.1(4) . . . . ? N11 N12 C13 C16 179.3(4) . . . . ? B1 N12 C13 C16 -5.0(7) . . . . ? N12 C13 C14 C15 -0.1(5) . . . . ? C16 C13 C14 C15 180.0(5) . . . . ? N12 N11 C15 C14 -1.2(5) . . . . ? U1 N11 C15 C14 153.3(3) . . . . ? N12 N11 C15 C17 177.0(4) . . . . ? U1 N11 C15 C17 -28.6(6) . . . . ? C13 C14 C15 N11 0.8(5) . . . . ? C13 C14 C15 C17 -177.2(5) . . . . ? N21 N22 C23 C24 -0.3(4) . . . . ? B1 N22 C23 C24 175.1(4) . . . . ? N21 N22 C23 C26 179.8(4) . . . . ? B1 N22 C23 C26 -4.8(7) . . . . ? N22 C23 C24 C25 -0.2(5) . . . . ? C26 C23 C24 C25 179.7(4) . . . . ? N22 N21 C25 C24 -0.8(5) . . . . ? U1 N21 C25 C24 161.1(3) . . . . ? N22 N21 C25 C27 176.9(4) . . . . ? U1 N21 C25 C27 -21.1(6) . . . . ? C23 C24 C25 N21 0.6(5) . . . . ? C23 C24 C25 C27 -176.9(4) . . . . ? N31 N32 C33 C34 0.1(5) . . . . ? B1 N32 C33 C34 178.5(4) . . . . ? N31 N32 C33 C36 -179.9(4) . . . . ? B1 N32 C33 C36 -1.5(7) . . . . ? N32 C33 C34 C35 -0.3(5) . . . . ? C36 C33 C34 C35 179.7(5) . . . . ? N32 N31 C35 C34 -0.3(5) . . . . ? U1 N31 C35 C34 170.8(3) . . . . ? N32 N31 C35 C37 179.4(4) . . . . ? U1 N31 C35 C37 -9.5(6) . . . . ? C33 C34 C35 N31 0.4(5) . . . . ? C33 C34 C35 C37 -179.3(5) . . . . ? U1 N4 C41 C42 54(3) . . . . ? U1 N4 C41 C44 -66(3) . . . . ? U1 N4 C41 C43 175(2) . . . . ? N4 C41 C42 C45 -178.7(4) . . . . ? C44 C41 C42 C45 -58.3(5) . . . . ? C43 C41 C42 C45 58.5(5) . . . . ? N4 C41 C43 C47 -179.9(4) . . . . ? C42 C41 C43 C47 -58.1(5) . . . . ? C44 C41 C43 C47 59.7(5) . . . . ? N4 C41 C44 C49 178.5(4) . . . . ? C42 C41 C44 C49 57.8(5) . . . . ? C43 C41 C44 C49 -59.8(5) . . . . ? C41 C42 C45 C46 -60.3(5) . . . . ? C41 C42 C45 C4A 59.6(5) . . . . ? C4A C45 C46 C47 -59.9(5) . . . . ? C42 C45 C46 C47 59.8(5) . . . . ? C41 C43 C47 C48 -61.0(5) . . . . ? C41 C43 C47 C46 59.4(5) . . . . ? C45 C46 C47 C48 61.0(5) . . . . ? C45 C46 C47 C43 -59.8(5) . . . . ? C43 C47 C48 C49 59.6(5) . . . . ? C46 C47 C48 C49 -61.1(5) . . . . ? C47 C48 C49 C4A 60.6(5) . . . . ? C47 C48 C49 C44 -59.1(6) . . . . ? C41 C44 C49 C4A -58.9(5) . . . . ? C41 C44 C49 C48 60.5(6) . . . . ? C48 C49 C4A C45 -60.1(5) . . . . ? C44 C49 C4A C45 59.8(5) . . . . ? C46 C45 C4A C49 60.2(5) . . . . ? C42 C45 C4A C49 -59.9(5) . . . . ? N61 N62 C63 C64 -0.9(4) . . . . ? B2 N62 C63 C64 175.4(4) . . . . ? N61 N62 C63 C66 176.7(4) . . . . ? B2 N62 C63 C66 -6.9(7) . . . . ? N62 C63 C64 C65 0.2(5) . . . . ? C66 C63 C64 C65 -177.3(4) . . . . ? N62 N61 C65 C64 -1.1(5) . . . . ? U1 N61 C65 C64 -173.8(3) . . . . ? N62 N61 C65 C67 178.9(4) . . . . ? U1 N61 C65 C67 6.3(7) . . . . ? C63 C64 C65 N61 0.6(5) . . . . ? C63 C64 C65 C67 -179.5(5) . . . . ? N71 N72 C73 C74 -1.8(5) . . . . ? B2 N72 C73 C74 -178.1(5) . . . . ? N71 N72 C73 C76 173.3(4) . . . . ? B2 N72 C73 C76 -3.0(8) . . . . ? N72 C73 C74 C75 2.0(5) . . . . ? C76 C73 C74 C75 -173.1(5) . . . . ? N72 N71 C75 C74 0.4(5) . . . . ? U1 N71 C75 C74 140.2(3) . . . . ? N72 N71 C75 C77 -177.8(4) . . . . ? U1 N71 C75 C77 -38.0(6) . . . . ? C73 C74 C75 N71 -1.5(5) . . . . ? C73 C74 C75 C77 176.6(5) . . . . ? N81 N82 C83 C84 -1.0(5) . . . . ? B2 N82 C83 C84 -172.8(4) . . . . ? N81 N82 C83 C86 179.0(4) . . . . ? B2 N82 C83 C86 7.3(7) . . . . ? N82 C83 C84 C85 1.4(6) . . . . ? C86 C83 C84 C85 -178.7(5) . . . . ? N82 N81 C85 C84 0.7(5) . . . . ? N82 N81 C85 C87 -178.2(4) . . . . ? C83 C84 C85 N81 -1.4(6) . . . . ? C83 C84 C85 C87 177.4(5) . . . . ? C916 C911 C912 C913 -0.2(8) . . . . ? C917 C911 C912 C913 178.6(5) . . . . ? C911 C912 C913 C914 0.3(9) . . . . ? C912 C913 C914 C915 -0.1(9) . . . . ? C913 C914 C915 C916 -0.3(10) . . . . ? C914 C915 C916 C911 0.4(9) . . . . ? C912 C911 C916 C915 -0.2(8) . . . . ? C917 C911 C916 C915 -179.0(6) . . . . ? C926 C921 C922 C923 1.2(9) . . . . ? C927 C921 C922 C923 179.4(6) . . . . ? C921 C922 C923 C924 -1.1(10) . . . . ? C922 C923 C924 C925 0.6(9) . . . . ? C923 C924 C925 C926 -0.2(8) . . . . ? C924 C925 C926 C921 0.3(8) . . . . ? C922 C921 C926 C925 -0.8(8) . . . . ? C927 C921 C926 C925 -178.9(6) . . . . ? C23 N22 B1 N12 -126.7(4) . . . . ? N21 N22 B1 N12 48.2(5) . . . . ? C23 N22 B1 N32 112.1(4) . . . . ? N21 N22 B1 N32 -73.1(5) . . . . ? C13 N12 B1 N22 106.9(5) . . . . ? N11 N12 B1 N22 -77.8(5) . . . . ? C13 N12 B1 N32 -131.6(4) . . . . ? N11 N12 B1 N32 43.7(5) . . . . ? C33 N32 B1 N22 -124.6(4) . . . . ? N31 N32 B1 N22 53.6(5) . . . . ? C33 N32 B1 N12 113.7(5) . . . . ? N31 N32 B1 N12 -68.1(5) . . . . ? C83 N82 B2 N72 -168.5(4) . . . . ? N81 N82 B2 N72 20.6(6) . . . . ? C83 N82 B2 N62 63.7(5) . . . . ? N81 N82 B2 N62 -107.2(4) . . . . ? C73 N72 B2 N82 -50.2(7) . . . . ? N71 N72 B2 N82 133.6(4) . . . . ? C73 N72 B2 N62 76.8(6) . . . . ? N71 N72 B2 N62 -99.4(4) . . . . ? C63 N62 B2 N82 32.3(6) . . . . ? N61 N62 B2 N82 -151.5(3) . . . . ? C63 N62 B2 N72 -98.0(5) . . . . ? N61 N62 B2 N72 78.1(4) . . . . ? _iucr_refine_instruction_details ; TITL xl in P-1 CELL 1.54178 9.19930 14.09540 22.37660 97.92990 101.25540 106.14170 ZERR 2 0.00040 0.00060 0.00070 0.00260 0.00320 0.00300 LATT 1 SFAC C H B N U UNIT 156 232 8 52 4 OMIT 1 0 0 OMIT -1 1 0 OMIT 0 1 0 OMIT 1 1 0 OMIT 3 -3 1 OMIT 0 0 1 OMIT -4 5 1 OMIT -2 -3 2 OMIT -2 -2 2 OMIT -1 -2 2 OMIT -2 -1 2 OMIT -1 0 2 OMIT 0 0 2 OMIT 2 0 2 OMIT 0 1 2 OMIT 0 3 2 OMIT 0 4 2 OMIT -1 -4 3 OMIT 1 -2 3 OMIT 2 -1 3 OMIT -2 -1 4 OMIT -2 1 4 OMIT -1 1 4 OMIT 1 1 4 OMIT -1 -4 5 OMIT 2 -3 5 OMIT 2 -2 5 OMIT 1 -1 5 OMIT 2 -1 5 OMIT -2 2 5 OMIT -4 -11 6 OMIT 0 2 6 OMIT 2 -4 7 OMIT -1 -3 7 OMIT 0 -3 7 OMIT 1 -3 7 OMIT -3 2 10 OMIT 0 -2 11 OMIT -2 -14 12 OMIT -2 -14 13 TEMP -123.15 SIZE 0.15 0.18 0.20 L.S. 10 ACTA 130.0 BOND $H CONF PLAN -20 WGHT 0.070200 4.301600 FVAR 0.52796 U1 5 0.035105 0.463187 0.268637 11.00000 0.02162 0.02223 = 0.02040 0.00612 0.00841 0.00889 N4 4 0.014951 0.554831 0.338147 11.00000 0.03040 0.02552 = 0.02093 -0.00021 0.01037 0.01046 N11 4 0.067134 0.301909 0.200152 11.00000 0.03215 0.02356 = 0.02330 0.00589 0.00822 0.01237 N12 4 0.134095 0.241540 0.232207 11.00000 0.02432 0.02401 = 0.02765 0.00803 0.01052 0.01082 N21 4 0.259141 0.422985 0.336733 11.00000 0.02595 0.02846 = 0.02602 0.00464 0.00570 0.01036 N22 4 0.246242 0.327479 0.345567 11.00000 0.02783 0.03095 = 0.01993 0.00836 0.00666 0.01365 N31 4 -0.097954 0.305429 0.303951 11.00000 0.02416 0.02592 = 0.02839 0.00856 0.01289 0.00782 N32 4 -0.040043 0.226388 0.307538 11.00000 0.02703 0.02477 = 0.02574 0.00829 0.00905 0.00746 N61 4 -0.180530 0.447321 0.170734 11.00000 0.02336 0.02631 = 0.02585 0.00508 0.00824 0.00894 N62 4 -0.149586 0.530708 0.143892 11.00000 0.02917 0.01848 = 0.02222 0.00504 0.00770 0.00700 N71 4 0.228708 0.555152 0.209738 11.00000 0.02156 0.02281 = 0.02959 0.00875 0.00849 0.00931 N72 4 0.150473 0.592920 0.163546 11.00000 0.02366 0.02025 = 0.02597 0.00797 0.00986 0.00791 N81 4 0.067725 0.770197 0.128688 11.00000 0.03572 0.02548 = 0.03385 0.00925 0.01264 0.00724 N82 4 -0.008874 0.718438 0.167668 11.00000 0.02910 0.02047 = 0.03008 0.00961 0.01148 0.00736 C13 1 0.193442 0.187977 0.194450 11.00000 0.02685 0.02395 = 0.03384 0.00481 0.01185 0.00898 C14 1 0.163787 0.212547 0.136733 11.00000 0.03549 0.02755 = 0.03054 0.00643 0.01806 0.01189 AFIX 43 H14 2 0.192026 0.186733 0.100724 11.00000 -1.20000 AFIX 0 C15 1 0.084084 0.282841 0.141901 11.00000 0.02869 0.02334 = 0.02437 0.00408 0.01071 0.00642 C16 1 0.276115 0.115698 0.215163 11.00000 0.04461 0.03713 = 0.04034 0.01017 0.01595 0.02464 AFIX 137 H16A 2 0.352346 0.147742 0.255040 11.00000 -1.50000 H16B 2 0.330093 0.097288 0.183901 11.00000 -1.50000 H16C 2 0.199863 0.054891 0.220066 11.00000 -1.50000 AFIX 0 C17 1 0.019087 0.330373 0.091225 11.00000 0.04618 0.03095 = 0.02900 0.00873 0.01455 0.01743 AFIX 137 H17A 2 -0.091184 0.292128 0.072891 11.00000 -1.50000 H17B 2 0.077433 0.329852 0.058987 11.00000 -1.50000 H17C 2 0.028639 0.400126 0.108760 11.00000 -1.50000 AFIX 0 C23 1 0.359542 0.332514 0.396090 11.00000 0.02658 0.04678 = 0.02601 0.00787 0.00997 0.02042 C24 1 0.445187 0.431092 0.419253 11.00000 0.02648 0.05215 = 0.02414 0.00231 0.00819 0.01679 AFIX 43 H24 2 0.531724 0.456938 0.454486 11.00000 -1.20000 AFIX 0 C25 1 0.380715 0.486391 0.381051 11.00000 0.02277 0.04271 = 0.02746 0.00255 0.00789 0.01395 C26 1 0.378762 0.241087 0.419160 11.00000 0.04887 0.05526 = 0.03359 0.02025 0.00791 0.03030 AFIX 137 H26A 2 0.280663 0.202899 0.427401 11.00000 -1.50000 H26B 2 0.461869 0.261813 0.457630 11.00000 -1.50000 H26C 2 0.406356 0.198594 0.387578 11.00000 -1.50000 AFIX 0 C27 1 0.430567 0.597169 0.382156 11.00000 0.02630 0.03087 = 0.04414 -0.00420 0.00922 0.00334 AFIX 137 H27A 2 0.523265 0.615387 0.365515 11.00000 -1.50000 H27B 2 0.455274 0.634521 0.425088 11.00000 -1.50000 H27C 2 0.345835 0.614204 0.356591 11.00000 -1.50000 AFIX 0 C33 1 -0.146238 0.148065 0.319459 11.00000 0.03261 0.03126 = 0.02647 0.01127 0.01245 0.00738 C34 1 -0.276068 0.176516 0.323601 11.00000 0.02549 0.03816 = 0.03113 0.00887 0.01385 0.00554 AFIX 43 H34 2 -0.369799 0.137077 0.331429 11.00000 -1.20000 AFIX 0 C35 1 -0.241680 0.275112 0.313945 11.00000 0.02641 0.02764 = 0.02752 0.00813 0.01084 0.00653 C36 1 -0.119534 0.049246 0.326363 11.00000 0.04334 0.03205 = 0.05271 0.01881 0.01779 0.01197 AFIX 137 H36A 2 -0.093576 0.020656 0.288906 11.00000 -1.50000 H36B 2 -0.214463 0.002364 0.332004 11.00000 -1.50000 H36C 2 -0.033151 0.060288 0.362682 11.00000 -1.50000 AFIX 0 C37 1 -0.338119 0.344905 0.313768 11.00000 0.02663 0.03419 = 0.04762 0.00565 0.01497 0.00914 AFIX 137 H37A 2 -0.363290 0.355855 0.354232 11.00000 -1.50000 H37B 2 -0.434914 0.314972 0.280957 11.00000 -1.50000 H37C 2 -0.279300 0.409589 0.306001 11.00000 -1.50000 AFIX 0 C41 1 0.020693 0.627797 0.391941 11.00000 0.02685 0.03014 = 0.02306 0.00808 0.01126 0.00932 C42 1 0.116837 0.733499 0.388373 11.00000 0.03255 0.02914 = 0.02653 0.00561 0.00985 0.00892 AFIX 23 H42A 2 0.067957 0.752212 0.350186 11.00000 -1.20000 H42B 2 0.223230 0.733702 0.385947 11.00000 -1.20000 AFIX 0 C43 1 -0.144085 0.629309 0.396406 11.00000 0.02603 0.03637 = 0.02926 0.00186 0.01033 0.00658 AFIX 23 H43A 2 -0.196600 0.646406 0.358273 11.00000 -1.20000 H43B 2 -0.207141 0.561586 0.399610 11.00000 -1.20000 AFIX 0 C44 1 0.096257 0.600013 0.451943 11.00000 0.03903 0.03828 = 0.02676 0.01347 0.01355 0.01902 AFIX 23 H44A 2 0.202040 0.597653 0.450397 11.00000 -1.20000 H44B 2 0.033141 0.532266 0.455085 11.00000 -1.20000 AFIX 0 C45 1 0.127351 0.811413 0.445603 11.00000 0.03659 0.02637 = 0.03933 0.00471 0.01422 0.00641 AFIX 13 H45 2 0.191478 0.879759 0.442455 11.00000 -1.20000 AFIX 0 C46 1 -0.035677 0.813035 0.448863 11.00000 0.04272 0.03718 = 0.03394 0.00115 0.01183 0.02070 AFIX 23 H46A 2 -0.085888 0.832205 0.411110 11.00000 -1.20000 H46B 2 -0.029156 0.863424 0.485610 11.00000 -1.20000 AFIX 0 C47 1 -0.133356 0.707434 0.453715 11.00000 0.02978 0.04351 = 0.03586 0.00050 0.01482 0.01385 AFIX 13 H47 2 -0.240810 0.708150 0.455530 11.00000 -1.20000 AFIX 0 C48 1 -0.057020 0.679966 0.512909 11.00000 0.04434 0.04544 = 0.02972 0.00290 0.02069 0.01232 AFIX 23 H48A 2 -0.120632 0.612975 0.517009 11.00000 -1.20000 H48B 2 -0.050253 0.730303 0.549725 11.00000 -1.20000 AFIX 0 C49 1 0.107508 0.677928 0.509554 11.00000 0.04423 0.04800 = 0.02492 0.00746 0.01160 0.01973 AFIX 13 H49 2 0.158214 0.659364 0.548015 11.00000 -1.20000 AFIX 0 C4A 1 0.204353 0.782449 0.504463 11.00000 0.03103 0.05110 = 0.03190 -0.00353 0.00574 0.01153 AFIX 23 H4A1 2 0.311054 0.782284 0.502827 11.00000 -1.20000 H4A2 2 0.212567 0.832690 0.541569 11.00000 -1.20000 AFIX 0 C63 1 -0.261669 0.514567 0.091000 11.00000 0.02558 0.03751 = 0.02642 0.00755 0.00799 0.01590 C64 1 -0.364334 0.419052 0.083364 11.00000 0.02437 0.03194 = 0.02867 0.00064 0.00355 0.00800 AFIX 43 H64 2 -0.454664 0.386751 0.050274 11.00000 -1.20000 AFIX 0 C65 1 -0.310308 0.379234 0.133300 11.00000 0.02495 0.02873 = 0.02555 0.00343 0.00523 0.00946 C66 1 -0.268296 0.592108 0.051919 11.00000 0.03594 0.04910 = 0.02843 0.01522 0.00244 0.01734 AFIX 137 H66A 2 -0.309282 0.642011 0.071744 11.00000 -1.50000 H66B 2 -0.336804 0.559184 0.010556 11.00000 -1.50000 H66C 2 -0.163137 0.625868 0.047886 11.00000 -1.50000 AFIX 0 C67 1 -0.375055 0.278875 0.148204 11.00000 0.03521 0.03320 = 0.04704 0.01107 0.00366 0.00556 AFIX 137 H67A 2 -0.307233 0.273266 0.186294 11.00000 -1.50000 H67B 2 -0.380745 0.225809 0.113736 11.00000 -1.50000 H67C 2 -0.479905 0.271337 0.154417 11.00000 -1.50000 AFIX 0 C73 1 0.219579 0.593787 0.115437 11.00000 0.03082 0.02900 = 0.02711 0.00610 0.01113 0.01155 C74 1 0.345908 0.559557 0.130747 11.00000 0.02725 0.03567 = 0.03086 0.01122 0.01488 0.01187 AFIX 43 H74 2 0.417982 0.553967 0.106344 11.00000 -1.20000 AFIX 0 C75 1 0.347224 0.534802 0.188910 11.00000 0.02273 0.03124 = 0.02994 0.00774 0.01284 0.00922 C76 1 0.160221 0.618851 0.054538 11.00000 0.04162 0.04963 = 0.02988 0.01450 0.01588 0.02244 AFIX 137 H76A 2 0.049117 0.580830 0.038354 11.00000 -1.50000 H76B 2 0.218499 0.600871 0.024871 11.00000 -1.50000 H76C 2 0.174090 0.691301 0.060421 11.00000 -1.50000 AFIX 0 C77 1 0.454826 0.489308 0.225222 11.00000 0.02902 0.04608 = 0.04107 0.01623 0.01434 0.02069 AFIX 137 H77A 2 0.527469 0.540669 0.260467 11.00000 -1.50000 H77B 2 0.513753 0.463961 0.198294 11.00000 -1.50000 H77C 2 0.393805 0.433467 0.240714 11.00000 -1.50000 AFIX 0 C83 1 -0.108476 0.764789 0.186142 11.00000 0.02935 0.03120 = 0.03713 0.00744 0.01178 0.01458 C84 1 -0.095906 0.849202 0.160002 11.00000 0.04283 0.03465 = 0.04498 0.01052 0.01187 0.02156 AFIX 43 H84 2 -0.149304 0.897426 0.165098 11.00000 -1.20000 AFIX 0 C85 1 0.013527 0.847730 0.124203 11.00000 0.04190 0.02943 = 0.03885 0.01257 0.01064 0.01353 C86 1 -0.210737 0.726340 0.227878 11.00000 0.03795 0.04242 = 0.04230 0.01600 0.01940 0.01869 AFIX 137 H86A 2 -0.311154 0.679888 0.202534 11.00000 -1.50000 H86B 2 -0.228131 0.783224 0.252713 11.00000 -1.50000 H86C 2 -0.159739 0.690789 0.255656 11.00000 -1.50000 AFIX 0 C87 1 0.070375 0.919159 0.082773 11.00000 0.06006 0.03736 = 0.05599 0.02249 0.02005 0.01902 AFIX 137 H87A 2 0.184002 0.936258 0.089896 11.00000 -1.50000 H87B 2 0.042737 0.980824 0.092591 11.00000 -1.50000 H87C 2 0.021116 0.886544 0.039063 11.00000 -1.50000 AFIX 0 C911 1 0.468104 0.089164 0.611510 11.00000 0.04622 0.03328 = 0.03849 0.00990 0.01618 0.00132 C912 1 0.565923 0.030465 0.616551 11.00000 0.05156 0.03347 = 0.05097 0.01338 0.02544 0.00925 AFIX 43 H912 2 0.556886 -0.019870 0.581874 11.00000 -1.20000 AFIX 0 C913 1 0.676126 0.043503 0.670805 11.00000 0.04894 0.05572 = 0.06238 0.02683 0.01846 0.00887 AFIX 43 H913 2 0.742654 0.002566 0.673235 11.00000 -1.20000 AFIX 0 C914 1 0.690366 0.115905 0.721748 11.00000 0.06456 0.05611 = 0.05413 0.01792 0.00577 -0.00459 AFIX 43 H914 2 0.766400 0.124914 0.759278 11.00000 -1.20000 AFIX 0 C915 1 0.592514 0.175652 0.717754 11.00000 0.08393 0.03986 = 0.03928 -0.00165 0.01893 -0.01498 AFIX 43 H915 2 0.601322 0.225433 0.752694 11.00000 -1.20000 AFIX 0 C916 1 0.483245 0.162619 0.663294 11.00000 0.06806 0.03035 = 0.05923 0.01331 0.03198 0.00847 AFIX 43 H916 2 0.417237 0.203892 0.660740 11.00000 -1.20000 AFIX 0 C917 1 0.351366 0.075585 0.551783 11.00000 0.06718 0.06656 = 0.05365 0.01593 0.01181 0.02995 AFIX 137 H91A 2 0.385217 0.044771 0.517218 11.00000 -1.50000 H91B 2 0.342721 0.141399 0.545406 11.00000 -1.50000 H91C 2 0.249566 0.031675 0.553538 11.00000 -1.50000 AFIX 0 C921 1 -0.367733 0.939995 0.054493 11.00000 0.04116 0.04010 = 0.04196 0.00664 0.01403 0.01180 C922 1 -0.486179 0.873114 0.071513 11.00000 0.04465 0.04840 = 0.05053 0.00474 0.01415 0.00224 AFIX 43 H922 2 -0.548601 0.812509 0.042886 11.00000 -1.20000 AFIX 0 C923 1 -0.515363 0.893012 0.129640 11.00000 0.04634 0.06808 = 0.05320 0.01931 0.02289 0.01578 AFIX 43 H923 2 -0.598428 0.846804 0.140309 11.00000 -1.20000 AFIX 0 C924 1 -0.423341 0.980362 0.172238 11.00000 0.05836 0.06235 = 0.04450 0.01066 0.01903 0.03537 AFIX 43 H924 2 -0.441964 0.994269 0.212324 11.00000 -1.20000 AFIX 0 C925 1 -0.304464 1.046653 0.155484 11.00000 0.05586 0.03803 = 0.04449 0.00459 0.00373 0.02281 AFIX 43 H925 2 -0.240972 1.106777 0.184322 11.00000 -1.20000 AFIX 0 C926 1 -0.276347 1.027019 0.097538 11.00000 0.04104 0.03670 = 0.05588 0.01845 0.00979 0.01257 AFIX 43 H926 2 -0.193523 1.073550 0.086941 11.00000 -1.20000 AFIX 0 C927 1 -0.336843 0.916278 -0.008975 11.00000 0.05863 0.07328 = 0.04696 0.00711 0.02345 0.00850 AFIX 137 H92A 2 -0.343719 0.844997 -0.018891 11.00000 -1.50000 H92B 2 -0.232183 0.958521 -0.008777 11.00000 -1.50000 H92C 2 -0.414619 0.929953 -0.040369 11.00000 -1.50000 AFIX 0 B1 3 0.126908 0.234620 0.300035 11.00000 0.02776 0.02758 = 0.03159 0.01120 0.01253 0.01444 B2 3 0.006396 0.617573 0.178403 11.00000 0.02362 0.02797 = 0.02711 0.00809 0.00682 0.01259 H2 2 0.019991 0.612170 0.233517 11.00000 -1.20000 H1 2 0.153968 0.169721 0.309358 11.00000 0.03513 HKLF 4 REM xl in P-1 REM R1 = 0.0365 for 9373 Fo > 4sig(Fo) and 0.0365 for all 9387 data REM 652 parameters refined using 0 restraints END WGHT 0.0702 4.3018 REM Highest difference peak 2.393, deepest hole -1.462, 1-sigma level 0.133 Q1 1 0.0658 0.5362 0.2828 11.00000 0.05 2.39 Q2 1 0.0234 0.3996 0.2553 11.00000 0.05 2.36 Q3 1 -0.0493 0.4436 0.2798 11.00000 0.05 2.17 Q4 1 0.1282 0.4791 0.2693 11.00000 0.05 2.02 Q5 1 -0.0002 0.4376 0.2291 11.00000 0.05 1.17 Q6 1 0.0288 0.3359 0.2101 11.00000 0.05 0.76 Q7 1 -0.1117 0.4438 0.1878 11.00000 0.05 0.65 Q8 1 0.0224 0.6018 0.3639 11.00000 0.05 0.63 Q9 1 0.0813 0.5958 0.1573 11.00000 0.05 0.58 Q10 1 -0.1414 0.4594 0.2011 11.00000 0.05 0.57 Q11 1 0.2277 0.4577 0.3312 11.00000 0.05 0.54 Q12 1 0.2771 0.5450 0.2082 11.00000 0.05 0.49 Q13 1 -0.0283 0.6234 0.2288 11.00000 0.05 0.49 Q14 1 0.1903 0.4924 0.2095 11.00000 0.05 0.49 Q15 1 -0.1559 0.7560 0.2048 11.00000 0.05 0.47 Q16 1 -0.0096 0.4825 0.3519 11.00000 0.05 0.47 Q17 1 0.1808 0.5657 0.1787 11.00000 0.05 0.46 Q18 1 0.2311 0.4743 0.2422 11.00000 0.05 0.46 Q19 1 -0.0563 0.2863 0.1773 11.00000 0.05 0.46 Q20 1 0.0482 0.2375 0.3083 11.00000 0.05 0.46 ; # Attachment '- sbmg01full.cif' #============================================================================ data_SBMG01 _database_code_depnum_ccdc_archive 'CCDC 859612' #TrackingRef '- sbmg01full.cif' # 5. CRYSTAL DATA _database_code_CSD SBMG01 _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _chemical_name_systematic ; ? ; _chemical_formula_sum 'C39 H55 B2 N13 U1' _chemical_formula_moiety 'C39 H55 B2 N13 U1' _chemical_formula_structural ? _chemical_formula_weight 965.61 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.3252(5) _cell_length_b 14.1075(4) _cell_length_c 19.9873(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.487(2) _cell_angle_gamma 90.00 _cell_volume 4143.6(2) _cell_measurement_reflns_used 8260 _cell_measurement_theta_min 2 _cell_measurement_theta_max 72 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' loop_ _atom_type_symbol _atom_type_radius_bond U 1.42 N 0.75 C 0.77 B 0.82 H 0.32 _diffrn_radiation_type CU-K\a _diffrn_radiation_wavelength 1.54184 _exptl_absorpt_coefficient_mu 12.207 _cell_measurement_temperature 150(2) _exptl_crystal_F_000 1928 # 6. DATA COLLECTION _diffrn_ambient_temperature 150(2) _diffrn_measurement_device_type Rigaku_Rapid_II _diffrn_radiation_monochromator 'confocal optics' _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.1867 _exptl_absorpt_correction_T_max 0.5432 _diffrn_reflns_number 49215 _diffrn_measured_fraction_theta_max 0.9640 _diffrn_reflns_theta_full 72.2 _diffrn_measured_fraction_theta_full 0.9640 _reflns_number_total 7883 _reflns_number_gt 7558 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 72.18 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_max 23 _diffrn_special_details 'mosaicity from Denzo/Scalepack is 0.44' _diffrn_standards_number 0 _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_measurement_details ; Data were collected on a Rigaku Rapid which has a quarter chi circle and a 200 degree curved image plate at a fixed distance of 127.4mm. Strategy was optimized using the CrystalClear software. The completeness is the best that can be obtained with this geometry. Also the use of HKL2000/SCALEPACK lowers the number of observed data as inconsistent equivalents are removed from the data set and not included in the collected total ; # 7. REFINEMENT DATA _refine_special_details ; Outlier data were removed using a local program based on the method of Prince and Nicholson. Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_all 0.030 _refine_ls_R_factor_gt 0.030 _refine_ls_wR_factor_ref 0.082 _refine_ls_wR_factor_gt 0.081 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 7883 _refine_ls_number_parameters 518 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+6.9090P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.49 _refine_diff_density_min -1.53 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection 'CrystalClear(Rigaku, 2001)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1996)' _computing_structure_solution ; PATTY (DIRDIF, Beurskins, 2008) ; _computing_structure_refinement 'SHELX97 (Sheldrick, 2008)' _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLATON (Spek, 1997) ; _computing_publication_material 'SHELX97(Sheldrick, 2008) and local programs' # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _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 U1 0.254614(7) 0.202141(7) 0.485497(5) 0.01621(6) Uani 1 1 d . . . N11 0.3345(2) 0.3660(2) 0.54823(15) 0.0215(6) Uani 1 1 d . . . N12 0.3263(2) 0.3871(2) 0.61348(15) 0.0202(6) Uani 1 1 d . . . N21 0.1657(2) 0.2395(2) 0.56989(16) 0.0221(6) Uani 1 1 d . . . N22 0.1978(2) 0.2861(2) 0.63235(17) 0.0213(7) Uani 1 1 d . . . N31 0.3673(2) 0.1736(2) 0.60980(16) 0.0210(6) Uani 1 1 d . . . N32 0.3611(2) 0.2247(2) 0.66752(16) 0.0215(6) Uani 1 1 d . . . N41 0.24481(18) 0.0642(2) 0.49858(16) 0.0199(6) Uani 1 1 d . . . N61 0.1539(2) 0.1539(2) 0.35768(15) 0.0199(6) Uani 1 1 d . . . N62 0.1651(2) 0.20121(19) 0.29946(17) 0.0203(7) Uani 1 1 d . . . N71 0.1756(2) 0.3508(2) 0.40947(15) 0.0202(6) Uani 1 1 d . . . N72 0.1944(2) 0.3672(2) 0.34684(15) 0.0202(6) Uani 1 1 d . . . N81 0.3603(2) 0.2318(2) 0.40908(16) 0.0228(6) Uani 1 1 d . . . N82 0.3287(2) 0.2612(2) 0.34067(15) 0.0199(6) Uani 1 1 d . . . C13 0.3534(2) 0.4777(3) 0.63128(19) 0.0232(7) Uani 1 1 d . . . C14 0.3810(3) 0.5148(3) 0.5771(2) 0.0260(8) Uani 1 1 d . . . C15 0.3681(2) 0.4440(3) 0.52659(19) 0.0225(7) Uani 1 1 d . . . C16 0.3477(3) 0.5250(3) 0.6968(2) 0.0315(9) Uani 1 1 d . . . C17 0.3873(3) 0.4522(3) 0.45765(19) 0.0274(8) Uani 1 1 d . . . C23 0.1280(3) 0.2998(3) 0.6607(2) 0.0297(10) Uani 1 1 d . . . C24 0.0505(3) 0.2614(3) 0.6162(2) 0.0305(9) Uani 1 1 d . . . C25 0.0765(3) 0.2236(3) 0.5608(2) 0.0241(8) Uani 1 1 d . . . C26 0.1385(3) 0.3489(5) 0.7291(3) 0.0522(14) Uani 1 1 d . . . C27 0.0222(3) 0.1718(4) 0.4977(2) 0.0363(10) Uani 1 1 d . . . C33 0.4126(3) 0.1835(3) 0.7265(2) 0.0266(8) Uani 1 1 d . . . C34 0.4532(3) 0.1048(3) 0.7078(2) 0.0292(8) Uani 1 1 d . . . C35 0.4236(2) 0.1001(3) 0.6355(2) 0.0252(8) Uani 1 1 d . . . C36 0.4220(4) 0.2203(4) 0.7982(2) 0.0376(10) Uani 1 1 d . . . C37 0.4472(3) 0.0253(3) 0.5909(2) 0.0305(9) Uani 1 1 d . . . C41 0.2396(2) -0.0322(3) 0.51205(16) 0.0190(7) Uani 1 1 d . . . C42 0.2556(2) -0.1002(3) 0.4655(2) 0.0228(7) Uani 1 1 d . . . C43 0.2427(3) -0.1952(3) 0.4760(2) 0.0274(9) Uani 1 1 d . . . C44 0.2170(3) -0.2288(3) 0.5330(2) 0.0310(9) Uani 1 1 d . . . C45 0.2072(2) -0.1611(3) 0.5815(2) 0.0276(8) Uani 1 1 d . . . C46 0.2173(2) -0.0642(3) 0.5724(2) 0.0240(8) Uani 1 1 d . . . C47 0.2855(3) -0.0676(3) 0.4035(2) 0.0275(8) Uani 1 1 d . . . C48 0.1946(3) -0.3309(3) 0.5407(3) 0.0476(12) Uani 1 1 d . . . C49 0.2032(3) 0.0052(3) 0.6258(2) 0.0299(8) Uani 1 1 d . . . C63 0.1151(2) 0.1597(3) 0.24048(19) 0.0248(8) Uani 1 1 d . . . C64 0.0702(3) 0.0850(3) 0.2588(2) 0.0262(8) Uani 1 1 d . . . C65 0.0947(2) 0.0831(3) 0.33114(19) 0.0219(7) Uani 1 1 d . . . C66 0.1098(4) 0.1946(3) 0.1684(2) 0.0347(11) Uani 1 1 d . . . C67 0.0583(3) 0.0168(3) 0.3750(2) 0.0264(8) Uani 1 1 d . . . C73 0.1710(2) 0.4572(3) 0.32515(19) 0.0238(7) Uani 1 1 d . . . C74 0.1361(3) 0.4992(3) 0.3742(2) 0.0256(8) Uani 1 1 d . . . C75 0.1394(2) 0.4310(3) 0.42522(19) 0.0210(7) Uani 1 1 d . . . C76 0.1850(3) 0.4994(3) 0.2603(2) 0.0301(8) Uani 1 1 d . . . C77 0.1082(3) 0.4415(3) 0.4897(2) 0.0301(9) Uani 1 1 d . . . C83 0.3995(3) 0.2703(3) 0.3135(2) 0.0239(7) Uani 1 1 d . . . C84 0.4781(2) 0.2465(3) 0.3640(2) 0.0259(8) Uani 1 1 d . . . C85 0.4519(3) 0.2236(3) 0.4233(2) 0.0236(8) Uani 1 1 d . . . C86 0.3900(3) 0.3021(3) 0.2402(3) 0.0386(12) Uani 1 1 d . . . C87 0.5105(3) 0.2004(3) 0.4942(2) 0.0356(11) Uani 1 1 d . . . B1 0.2992(3) 0.3128(3) 0.6607(2) 0.0217(9) Uani 1 1 d . . . B2 0.2276(3) 0.2879(3) 0.3064(2) 0.0195(8) Uani 1 1 d . . . H1 0.311(3) 0.346(3) 0.715(2) 0.025(11) Uiso 1 1 d . . . H2 0.225(3) 0.311(3) 0.254(3) 0.025(12) Uiso 1 1 d . . . H14 0.4043 0.5767 0.5745 0.031 Uiso 1 1 calc R . . H24 -0.0088 0.2609 0.6222 0.037 Uiso 1 1 calc R . . H34 0.4935 0.0622 0.7383 0.035 Uiso 1 1 calc R . . H43 0.2517 -0.2396 0.4428 0.033 Uiso 1 1 calc R . . H45 0.1930 -0.1821 0.6223 0.033 Uiso 1 1 calc R . . H64 0.0300 0.0425 0.2280 0.031 Uiso 1 1 calc R . . H74 0.1140 0.5623 0.3734 0.031 Uiso 1 1 calc R . . H84 0.5382 0.2459 0.3595 0.031 Uiso 1 1 calc R . . H16A 0.2839 0.5284 0.6971 0.047 Uiso 1 1 calc R . . H16B 0.3728 0.5893 0.6990 0.047 Uiso 1 1 calc R . . H16C 0.3826 0.4885 0.7372 0.047 Uiso 1 1 calc R . . H17A 0.4350 0.4069 0.4556 0.041 Uiso 1 1 calc R . . H17B 0.4078 0.5167 0.4519 0.041 Uiso 1 1 calc R . . H17C 0.3318 0.4383 0.4202 0.041 Uiso 1 1 calc R . . H26A 0.1779 0.3110 0.7668 0.078 Uiso 1 1 calc R . . H26B 0.0786 0.3562 0.7370 0.078 Uiso 1 1 calc R . . H26C 0.1659 0.4114 0.7281 0.078 Uiso 1 1 calc R . . H27A 0.0273 0.2044 0.4557 0.055 Uiso 1 1 calc R . . H27B -0.0418 0.1700 0.4976 0.055 Uiso 1 1 calc R . . H27C 0.0453 0.1069 0.4984 0.055 Uiso 1 1 calc R . . H36A 0.4400 0.2872 0.8008 0.056 Uiso 1 1 calc R . . H36B 0.4684 0.1836 0.8322 0.056 Uiso 1 1 calc R . . H36C 0.3636 0.2144 0.8089 0.056 Uiso 1 1 calc R . . H37A 0.4151 0.0377 0.5418 0.046 Uiso 1 1 calc R . . H37B 0.4291 -0.0369 0.6043 0.046 Uiso 1 1 calc R . . H37C 0.5130 0.0258 0.5972 0.046 Uiso 1 1 calc R . . H47A 0.3011 -0.1228 0.3794 0.041 Uiso 1 1 calc R . . H47B 0.3389 -0.0264 0.4194 0.041 Uiso 1 1 calc R . . H47C 0.2359 -0.0324 0.3713 0.041 Uiso 1 1 calc R . . H48A 0.2164 -0.3491 0.5900 0.071 Uiso 1 1 calc R . . H48B 0.2244 -0.3704 0.5133 0.071 Uiso 1 1 calc R . . H48C 0.1286 -0.3399 0.5239 0.071 Uiso 1 1 calc R . . H49A 0.1542 0.0492 0.6034 0.045 Uiso 1 1 calc R . . H49B 0.2595 0.0408 0.6456 0.045 Uiso 1 1 calc R . . H49C 0.1869 -0.0294 0.6630 0.045 Uiso 1 1 calc R . . H66A 0.0893 0.2607 0.1637 0.052 Uiso 1 1 calc R . . H66B 0.0666 0.1554 0.1339 0.052 Uiso 1 1 calc R . . H66C 0.1701 0.1904 0.1607 0.052 Uiso 1 1 calc R . . H67A 0.0991 0.0163 0.4226 0.040 Uiso 1 1 calc R . . H67B 0.0542 -0.0472 0.3553 0.040 Uiso 1 1 calc R . . H67C -0.0023 0.0379 0.3758 0.040 Uiso 1 1 calc R . . H76A 0.2502 0.5007 0.2642 0.045 Uiso 1 1 calc R . . H76B 0.1609 0.5641 0.2544 0.045 Uiso 1 1 calc R . . H76C 0.1532 0.4610 0.2199 0.045 Uiso 1 1 calc R . . H77A 0.0662 0.3899 0.4917 0.045 Uiso 1 1 calc R . . H77B 0.0771 0.5025 0.4884 0.045 Uiso 1 1 calc R . . H77C 0.1610 0.4390 0.5311 0.045 Uiso 1 1 calc R . . H86A 0.3516 0.2571 0.2074 0.058 Uiso 1 1 calc R . . H86B 0.4503 0.3049 0.2324 0.058 Uiso 1 1 calc R . . H86C 0.3620 0.3651 0.2329 0.058 Uiso 1 1 calc R . . H87A 0.4752 0.2070 0.5279 0.053 Uiso 1 1 calc R . . H87B 0.5625 0.2437 0.5067 0.053 Uiso 1 1 calc R . . H87C 0.5323 0.1350 0.4949 0.053 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 U1 0.01666(9) 0.01759(9) 0.01522(9) -0.00086(3) 0.00588(5) -0.00080(3) N11 0.0203(14) 0.0242(16) 0.0198(14) -0.0029(12) 0.0052(11) -0.0012(12) N12 0.0207(14) 0.0227(16) 0.0173(14) -0.0014(12) 0.0055(11) -0.0028(12) N21 0.0188(14) 0.0245(17) 0.0241(15) -0.0027(12) 0.0078(12) -0.0054(13) N22 0.0212(16) 0.0239(16) 0.0198(15) -0.0013(11) 0.0074(13) -0.0033(11) N31 0.0220(15) 0.0230(16) 0.0181(14) -0.0015(13) 0.0059(12) -0.0041(12) N32 0.0195(15) 0.0262(16) 0.0172(14) -0.0014(13) 0.0029(12) -0.0022(13) N41 0.0229(15) 0.0195(16) 0.0175(12) -0.0024(11) 0.0063(11) -0.0011(12) N61 0.0200(14) 0.0207(16) 0.0182(14) -0.0001(11) 0.0043(11) 0.0025(12) N62 0.0230(17) 0.0192(17) 0.0171(15) 0.0012(10) 0.0029(13) 0.0008(10) N71 0.0206(14) 0.0226(16) 0.0183(14) -0.0024(12) 0.0074(11) 0.0004(12) N72 0.0190(14) 0.0212(16) 0.0195(14) 0.0004(11) 0.0038(11) 0.0003(12) N81 0.0207(15) 0.0260(16) 0.0208(15) 0.0029(13) 0.0047(12) 0.0008(13) N82 0.0230(15) 0.0205(16) 0.0170(14) -0.0009(12) 0.0070(11) 0.0005(12) C13 0.0185(17) 0.026(2) 0.0243(18) 0.0008(14) 0.0042(14) -0.0041(15) C14 0.0269(18) 0.0197(18) 0.032(2) -0.0029(14) 0.0096(15) -0.0012(15) C15 0.0180(16) 0.026(2) 0.0245(18) 0.0019(14) 0.0081(14) -0.0003(15) C16 0.039(2) 0.025(2) 0.033(2) -0.0023(17) 0.0134(17) -0.0085(16) C17 0.0308(19) 0.030(2) 0.0227(18) -0.0096(16) 0.0092(15) -0.0029(15) C23 0.027(2) 0.042(3) 0.026(2) -0.0030(15) 0.0170(18) -0.0058(15) C24 0.0220(19) 0.046(3) 0.029(2) -0.0027(17) 0.0151(16) -0.0050(18) C25 0.0234(18) 0.0229(18) 0.0266(19) 0.0013(15) 0.0079(15) -0.0019(16) C26 0.039(3) 0.085(4) 0.039(3) -0.007(3) 0.022(2) -0.026(3) C27 0.023(2) 0.045(3) 0.039(2) -0.0023(18) 0.0058(17) -0.014(2) C33 0.0240(19) 0.036(2) 0.0195(18) -0.0017(16) 0.0048(15) 0.0018(16) C34 0.0240(18) 0.034(2) 0.0270(19) 0.0013(16) 0.0035(15) 0.0063(16) C35 0.0184(17) 0.025(2) 0.0299(19) 0.0000(14) 0.0029(14) 0.0013(15) C36 0.044(3) 0.045(3) 0.021(2) 0.004(2) 0.0046(18) 0.0001(18) C37 0.0252(19) 0.029(2) 0.036(2) 0.0071(16) 0.0073(16) -0.0024(17) C41 0.0192(17) 0.019(2) 0.0181(17) -0.0001(12) 0.0032(14) 0.0000(12) C42 0.0218(17) 0.020(2) 0.0244(17) 0.0004(13) 0.0037(13) -0.0017(15) C43 0.0211(19) 0.030(3) 0.031(2) 0.0040(14) 0.0062(16) -0.0006(15) C44 0.0234(19) 0.026(2) 0.041(2) 0.0008(16) 0.0040(17) 0.0058(18) C45 0.0225(18) 0.028(2) 0.031(2) -0.0007(15) 0.0069(15) 0.0098(16) C46 0.0186(17) 0.029(2) 0.0234(18) -0.0009(14) 0.0036(14) 0.0028(15) C47 0.032(2) 0.027(2) 0.0243(18) 0.0038(16) 0.0099(15) -0.0009(15) C48 0.044(3) 0.021(2) 0.078(4) 0.0053(19) 0.017(2) 0.009(2) C49 0.033(2) 0.035(2) 0.0235(18) -0.0018(17) 0.0107(15) 0.0035(16) C63 0.0252(18) 0.028(2) 0.0211(17) 0.0021(15) 0.0061(14) -0.0017(15) C64 0.0235(18) 0.028(2) 0.0252(18) -0.0014(15) 0.0036(14) -0.0066(15) C65 0.0178(16) 0.0186(18) 0.0273(18) 0.0018(13) 0.0032(14) -0.0008(14) C66 0.048(3) 0.033(2) 0.020(2) -0.0064(18) 0.0047(19) -0.0022(15) C67 0.0268(19) 0.026(2) 0.0259(18) -0.0052(15) 0.0069(15) 0.0007(15) C73 0.0240(18) 0.0208(19) 0.0251(18) 0.0005(14) 0.0048(14) 0.0015(14) C74 0.0270(18) 0.0186(19) 0.032(2) 0.0019(14) 0.0103(16) -0.0020(15) C75 0.0188(16) 0.0182(18) 0.0268(18) 0.0005(13) 0.0080(14) -0.0033(14) C76 0.038(2) 0.023(2) 0.032(2) -0.0004(16) 0.0136(17) 0.0047(16) C77 0.038(2) 0.024(2) 0.035(2) 0.0049(16) 0.0206(18) -0.0011(16) C83 0.0272(19) 0.0236(19) 0.0245(18) -0.0008(16) 0.0132(15) 0.0021(15) C84 0.0204(17) 0.032(2) 0.0297(19) 0.0017(15) 0.0143(15) 0.0019(16) C85 0.0181(17) 0.0267(19) 0.0268(19) 0.0015(15) 0.0079(15) 0.0015(16) C86 0.036(2) 0.057(3) 0.029(2) 0.0072(18) 0.020(2) 0.0119(18) C87 0.023(2) 0.055(3) 0.028(2) 0.0051(16) 0.0063(18) 0.0055(17) B1 0.023(2) 0.025(2) 0.019(2) -0.0026(16) 0.0091(16) -0.0019(16) B2 0.020(2) 0.021(2) 0.0177(19) 0.0006(14) 0.0052(16) 0.0014(14) # 10. MOLECULAR GEOMETRY _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_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N41 1.976(3) . . ? U1 N21 2.507(3) . . ? U1 N81 2.556(3) . . ? U1 N31 2.624(3) . . ? U1 N71 2.669(3) . . ? U1 N61 2.671(3) . . ? U1 N11 2.747(3) . . ? N11 C15 1.338(5) . . ? N11 N12 1.378(4) . . ? N12 C13 1.360(5) . . ? N12 B1 1.544(5) . . ? N21 C25 1.345(5) . . ? N21 N22 1.372(4) . . ? N22 C23 1.359(5) . . ? N22 B1 1.542(5) . . ? N31 C35 1.353(5) . . ? N31 N32 1.386(4) . . ? N32 C33 1.350(5) . . ? N32 B1 1.546(6) . . ? N41 C41 1.392(5) . . ? N61 C65 1.353(5) . . ? N61 N62 1.394(4) . . ? N62 C63 1.344(5) . . ? N62 B2 1.535(5) . . ? N71 C75 1.338(5) . . ? N71 N72 1.381(4) . . ? N72 C73 1.357(5) . . ? N72 B2 1.548(5) . . ? N81 C85 1.357(5) . . ? N81 N82 1.378(4) . . ? N82 C83 1.351(5) . . ? N82 B2 1.552(5) . . ? C13 C14 1.374(6) . . ? C13 C16 1.494(5) . . ? C14 C15 1.394(5) . . ? C14 H14 0.9500 . . ? C15 C17 1.493(5) . . ? C16 H16A 0.9800 . . ? C16 H16B 0.9800 . . ? C16 H16C 0.9800 . . ? C17 H17A 0.9800 . . ? C17 H17B 0.9800 . . ? C17 H17C 0.9800 . . ? C23 C24 1.378(6) . . ? C23 C26 1.498(6) . . ? C24 C25 1.385(6) . . ? C24 H24 0.9500 . . ? C25 C27 1.491(6) . . ? C26 H26A 0.9800 . . ? C26 H26B 0.9800 . . ? C26 H26C 0.9800 . . ? C27 H27A 0.9800 . . ? C27 H27B 0.9800 . . ? C27 H27C 0.9800 . . ? C33 C34 1.374(6) . . ? C33 C36 1.493(6) . . ? C34 C35 1.388(6) . . ? C34 H34 0.9500 . . ? C35 C37 1.492(5) . . ? C36 H36A 0.9800 . . ? C36 H36B 0.9800 . . ? C36 H36C 0.9800 . . ? C37 H37A 0.9800 . . ? C37 H37B 0.9800 . . ? C37 H37C 0.9800 . . ? C41 C42 1.406(5) . . ? C41 C46 1.417(5) . . ? C42 C43 1.379(5) . . ? C42 C47 1.510(5) . . ? C43 C44 1.390(7) . . ? C43 H43 0.9500 . . ? C44 C45 1.398(6) . . ? C44 C48 1.499(6) . . ? C45 C46 1.394(6) . . ? C45 H45 0.9500 . . ? C46 C49 1.508(6) . . ? C47 H47A 0.9800 . . ? C47 H47B 0.9800 . . ? C47 H47C 0.9800 . . ? C48 H48A 0.9800 . . ? C48 H48B 0.9800 . . ? C48 H48C 0.9800 . . ? C49 H49A 0.9800 . . ? C49 H49B 0.9800 . . ? C49 H49C 0.9800 . . ? C63 C64 1.365(6) . . ? C63 C66 1.502(6) . . ? C64 C65 1.387(5) . . ? C64 H64 0.9500 . . ? C65 C67 1.494(5) . . ? C66 H66A 0.9800 . . ? C66 H66B 0.9800 . . ? C66 H66C 0.9800 . . ? C67 H67A 0.9800 . . ? C67 H67B 0.9800 . . ? C67 H67C 0.9800 . . ? C73 C74 1.378(5) . . ? C73 C76 1.496(5) . . ? C74 C75 1.392(5) . . ? C74 H74 0.9500 . . ? C75 C77 1.504(5) . . ? C76 H76A 0.9800 . . ? C76 H76B 0.9800 . . ? C76 H76C 0.9800 . . ? C77 H77A 0.9800 . . ? C77 H77B 0.9800 . . ? C77 H77C 0.9800 . . ? C83 C84 1.377(5) . . ? C83 C86 1.499(6) . . ? C84 C85 1.392(5) . . ? C84 H84 0.9500 . . ? C85 C87 1.484(6) . . ? C86 H86A 0.9800 . . ? C86 H86B 0.9800 . . ? C86 H86C 0.9800 . . ? C87 H87A 0.9800 . . ? C87 H87B 0.9800 . . ? C87 H87C 0.9800 . . ? B1 H1 1.15(4) . . ? B2 H2 1.09(5) . . ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N41 U1 N21 92.40(12) . . . ? N41 U1 N81 108.98(12) . . . ? N21 U1 N81 157.69(12) . . . ? N41 U1 N31 77.18(11) . . . ? N21 U1 N31 74.50(10) . . . ? N81 U1 N31 103.44(9) . . . ? N41 U1 N71 144.10(10) . . . ? N21 U1 N71 88.43(10) . . . ? N81 U1 N71 78.05(9) . . . ? N31 U1 N71 136.87(10) . . . ? N41 U1 N61 80.24(11) . . . ? N21 U1 N61 114.85(9) . . . ? N81 U1 N61 76.24(9) . . . ? N31 U1 N61 155.95(10) . . . ? N71 U1 N61 67.06(9) . . . ? N41 U1 N11 144.08(10) . . . ? N21 U1 N11 76.87(9) . . . ? N81 U1 N11 81.91(10) . . . ? N31 U1 N11 66.94(10) . . . ? N71 U1 N11 70.73(9) . . . ? N61 U1 N11 135.46(9) . . . ? C15 N11 N12 106.0(3) . . . ? C15 N11 U1 135.0(2) . . . ? N12 N11 U1 117.8(2) . . . ? C13 N12 N11 110.3(3) . . . ? C13 N12 B1 126.4(3) . . . ? N11 N12 B1 123.0(3) . . . ? C25 N21 N22 106.9(3) . . . ? C25 N21 U1 126.8(2) . . . ? N22 N21 U1 126.1(2) . . . ? C23 N22 N21 109.0(3) . . . ? C23 N22 B1 129.9(3) . . . ? N21 N22 B1 121.0(3) . . . ? C35 N31 N32 105.6(3) . . . ? C35 N31 U1 130.9(2) . . . ? N32 N31 U1 121.8(2) . . . ? C33 N32 N31 110.0(3) . . . ? C33 N32 B1 128.0(3) . . . ? N31 N32 B1 122.0(3) . . . ? C41 N41 U1 176.6(3) . . . ? C65 N61 N62 104.7(3) . . . ? C65 N61 U1 134.8(2) . . . ? N62 N61 U1 120.1(2) . . . ? C63 N62 N61 110.4(3) . . . ? C63 N62 B2 127.8(3) . . . ? N61 N62 B2 121.8(3) . . . ? C75 N71 N72 106.2(3) . . . ? C75 N71 U1 133.0(2) . . . ? N72 N71 U1 118.0(2) . . . ? C73 N72 N71 110.0(3) . . . ? C73 N72 B2 127.3(3) . . . ? N71 N72 B2 122.4(3) . . . ? C85 N81 N82 106.5(3) . . . ? C85 N81 U1 130.9(2) . . . ? N82 N81 U1 122.6(2) . . . ? C83 N82 N81 109.4(3) . . . ? C83 N82 B2 127.9(3) . . . ? N81 N82 B2 122.4(3) . . . ? N12 C13 C14 107.0(3) . . . ? N12 C13 C16 124.1(3) . . . ? C14 C13 C16 128.9(4) . . . ? C13 C14 C15 106.6(3) . . . ? C13 C14 H14 126.70 . . . ? C15 C14 H14 126.70 . . . ? N11 C15 C14 110.1(3) . . . ? N11 C15 C17 123.8(3) . . . ? C14 C15 C17 126.0(4) . . . ? C13 C16 H16A 109.50 . . . ? C13 C16 H16B 109.50 . . . ? H16A C16 H16B 109.50 . . . ? C13 C16 H16C 109.50 . . . ? H16A C16 H16C 109.50 . . . ? H16B C16 H16C 109.50 . . . ? C15 C17 H17A 109.50 . . . ? C15 C17 H17B 109.50 . . . ? H17A C17 H17B 109.50 . . . ? C15 C17 H17C 109.50 . . . ? H17A C17 H17C 109.50 . . . ? H17B C17 H17C 109.50 . . . ? N22 C23 C24 108.1(4) . . . ? N22 C23 C26 123.6(4) . . . ? C24 C23 C26 128.4(4) . . . ? C23 C24 C25 106.0(3) . . . ? C23 C24 H24 127.00 . . . ? C25 C24 H24 127.00 . . . ? N21 C25 C24 109.9(3) . . . ? N21 C25 C27 119.9(3) . . . ? C24 C25 C27 130.2(4) . . . ? C23 C26 H26A 109.50 . . . ? C23 C26 H26B 109.50 . . . ? H26A C26 H26B 109.50 . . . ? C23 C26 H26C 109.50 . . . ? H26A C26 H26C 109.50 . . . ? H26B C26 H26C 109.50 . . . ? C25 C27 H27A 109.50 . . . ? C25 C27 H27B 109.50 . . . ? H27A C27 H27B 109.50 . . . ? C25 C27 H27C 109.50 . . . ? H27A C27 H27C 109.50 . . . ? H27B C27 H27C 109.50 . . . ? N32 C33 C34 107.9(3) . . . ? N32 C33 C36 124.2(4) . . . ? C34 C33 C36 127.9(4) . . . ? C33 C34 C35 106.4(3) . . . ? C33 C34 H34 126.80 . . . ? C35 C34 H34 126.80 . . . ? N31 C35 C34 110.1(3) . . . ? N31 C35 C37 123.5(3) . . . ? C34 C35 C37 126.4(4) . . . ? C33 C36 H36A 109.50 . . . ? C33 C36 H36B 109.50 . . . ? H36A C36 H36B 109.50 . . . ? C33 C36 H36C 109.50 . . . ? H36A C36 H36C 109.50 . . . ? H36B C36 H36C 109.50 . . . ? C35 C37 H37A 109.50 . . . ? C35 C37 H37B 109.50 . . . ? H37A C37 H37B 109.50 . . . ? C35 C37 H37C 109.50 . . . ? H37A C37 H37C 109.50 . . . ? H37B C37 H37C 109.50 . . . ? N41 C41 C42 120.5(3) . . . ? N41 C41 C46 121.1(3) . . . ? C42 C41 C46 118.4(4) . . . ? C43 C42 C41 120.2(4) . . . ? C43 C42 C47 120.7(4) . . . ? C41 C42 C47 119.1(3) . . . ? C42 C43 C44 122.8(4) . . . ? C42 C43 H43 118.60 . . . ? C44 C43 H43 118.60 . . . ? C43 C44 C45 116.6(4) . . . ? C43 C44 C48 122.6(4) . . . ? C45 C44 C48 120.7(4) . . . ? C46 C45 C44 122.8(4) . . . ? C46 C45 H45 118.60 . . . ? C44 C45 H45 118.60 . . . ? C45 C46 C41 119.1(4) . . . ? C45 C46 C49 120.1(3) . . . ? C41 C46 C49 120.9(3) . . . ? C42 C47 H47A 109.50 . . . ? C42 C47 H47B 109.50 . . . ? H47A C47 H47B 109.50 . . . ? C42 C47 H47C 109.50 . . . ? H47A C47 H47C 109.50 . . . ? H47B C47 H47C 109.50 . . . ? C44 C48 H48A 109.50 . . . ? C44 C48 H48B 109.50 . . . ? H48A C48 H48B 109.50 . . . ? C44 C48 H48C 109.50 . . . ? H48A C48 H48C 109.50 . . . ? H48B C48 H48C 109.50 . . . ? C46 C49 H49A 109.50 . . . ? C46 C49 H49B 109.50 . . . ? H49A C49 H49B 109.50 . . . ? C46 C49 H49C 109.50 . . . ? H49A C49 H49C 109.50 . . . ? H49B C49 H49C 109.50 . . . ? N62 C63 C64 107.9(3) . . . ? N62 C63 C66 124.1(4) . . . ? C64 C63 C66 128.0(4) . . . ? C63 C64 C65 106.7(3) . . . ? C63 C64 H64 126.70 . . . ? C65 C64 H64 126.70 . . . ? N61 C65 C64 110.3(3) . . . ? N61 C65 C67 123.6(3) . . . ? C64 C65 C67 126.0(3) . . . ? C63 C66 H66A 109.50 . . . ? C63 C66 H66B 109.50 . . . ? H66A C66 H66B 109.50 . . . ? C63 C66 H66C 109.50 . . . ? H66A C66 H66C 109.50 . . . ? H66B C66 H66C 109.50 . . . ? C65 C67 H67A 109.50 . . . ? C65 C67 H67B 109.50 . . . ? H67A C67 H67B 109.50 . . . ? C65 C67 H67C 109.50 . . . ? H67A C67 H67C 109.50 . . . ? H67B C67 H67C 109.50 . . . ? N72 C73 C74 107.2(3) . . . ? N72 C73 C76 124.0(3) . . . ? C74 C73 C76 128.7(4) . . . ? C73 C74 C75 106.4(3) . . . ? C73 C74 H74 126.80 . . . ? C75 C74 H74 126.80 . . . ? N71 C75 C74 110.1(3) . . . ? N71 C75 C77 122.6(3) . . . ? C74 C75 C77 127.2(3) . . . ? C73 C76 H76A 109.50 . . . ? C73 C76 H76B 109.50 . . . ? H76A C76 H76B 109.50 . . . ? C73 C76 H76C 109.50 . . . ? H76A C76 H76C 109.50 . . . ? H76B C76 H76C 109.50 . . . ? C75 C77 H77A 109.50 . . . ? C75 C77 H77B 109.50 . . . ? H77A C77 H77B 109.50 . . . ? C75 C77 H77C 109.50 . . . ? H77A C77 H77C 109.50 . . . ? H77B C77 H77C 109.50 . . . ? N82 C83 C84 108.5(3) . . . ? N82 C83 C86 123.7(4) . . . ? C84 C83 C86 127.8(4) . . . ? C83 C84 C85 106.1(3) . . . ? C83 C84 H84 127.00 . . . ? C85 C84 H84 127.00 . . . ? N81 C85 C84 109.6(3) . . . ? N81 C85 C87 121.9(4) . . . ? C84 C85 C87 128.4(4) . . . ? C83 C86 H86A 109.50 . . . ? C83 C86 H86B 109.50 . . . ? H86A C86 H86B 109.50 . . . ? C83 C86 H86C 109.50 . . . ? H86A C86 H86C 109.50 . . . ? H86B C86 H86C 109.50 . . . ? C85 C87 H87A 109.50 . . . ? C85 C87 H87B 109.50 . . . ? H87A C87 H87B 109.50 . . . ? C85 C87 H87C 109.50 . . . ? H87A C87 H87C 109.50 . . . ? H87B C87 H87C 109.50 . . . ? N22 B1 N12 111.0(3) . . . ? N22 B1 N32 111.4(3) . . . ? N12 B1 N32 109.6(3) . . . ? N22 B1 H1 108(2) . . . ? N12 B1 H1 107(2) . . . ? N32 B1 H1 109(2) . . . ? N62 B2 N72 109.5(3) . . . ? N62 B2 N82 111.4(3) . . . ? N72 B2 N82 112.4(3) . . . ? N62 B2 H2 108(2) . . . ? N72 B2 H2 111(2) . . . ? N82 B2 H2 105(2) . . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N41 U1 N11 C15 142.9(3) . . . . ? N21 U1 N11 C15 -141.5(3) . . . . ? N81 U1 N11 C15 31.6(3) . . . . ? N31 U1 N11 C15 140.0(3) . . . . ? N71 U1 N11 C15 -48.5(3) . . . . ? N61 U1 N11 C15 -29.2(4) . . . . ? N41 U1 N11 N12 -51.9(3) . . . . ? N21 U1 N11 N12 23.7(2) . . . . ? N81 U1 N11 N12 -163.2(2) . . . . ? N31 U1 N11 N12 -54.8(2) . . . . ? N71 U1 N11 N12 116.6(2) . . . . ? N61 U1 N11 N12 135.9(2) . . . . ? C15 N11 N12 C13 0.9(4) . . . . ? U1 N11 N12 C13 -168.2(2) . . . . ? C15 N11 N12 B1 -173.4(3) . . . . ? U1 N11 N12 B1 17.4(4) . . . . ? N41 U1 N21 C25 -69.2(3) . . . . ? N81 U1 N21 C25 127.1(3) . . . . ? N31 U1 N21 C25 -145.2(3) . . . . ? N71 U1 N21 C25 74.9(3) . . . . ? N61 U1 N21 C25 11.1(4) . . . . ? N11 U1 N21 C25 145.5(3) . . . . ? N41 U1 N21 N22 115.5(3) . . . . ? N81 U1 N21 N22 -48.2(4) . . . . ? N31 U1 N21 N22 39.5(3) . . . . ? N71 U1 N21 N22 -100.4(3) . . . . ? N61 U1 N21 N22 -164.1(3) . . . . ? N11 U1 N21 N22 -29.8(3) . . . . ? C25 N21 N22 C23 -0.9(4) . . . . ? U1 N21 N22 C23 175.1(3) . . . . ? C25 N21 N22 B1 178.0(3) . . . . ? U1 N21 N22 B1 -6.0(5) . . . . ? N41 U1 N31 C35 36.0(3) . . . . ? N21 U1 N31 C35 132.2(3) . . . . ? N81 U1 N31 C35 -70.7(3) . . . . ? N71 U1 N31 C35 -157.5(3) . . . . ? N61 U1 N31 C35 15.6(4) . . . . ? N11 U1 N31 C35 -145.7(3) . . . . ? N41 U1 N31 N32 -126.5(3) . . . . ? N21 U1 N31 N32 -30.3(3) . . . . ? N81 U1 N31 N32 126.8(3) . . . . ? N71 U1 N31 N32 40.0(3) . . . . ? N61 U1 N31 N32 -147.0(2) . . . . ? N11 U1 N31 N32 51.8(2) . . . . ? C35 N31 N32 C33 0.4(4) . . . . ? U1 N31 N32 C33 166.7(2) . . . . ? C35 N31 N32 B1 -177.2(3) . . . . ? U1 N31 N32 B1 -10.9(4) . . . . ? N21 U1 N41 C41 -49(4) . . . . ? N81 U1 N41 C41 124(4) . . . . ? N31 U1 N41 C41 24(4) . . . . ? N71 U1 N41 C41 -140(4) . . . . ? N61 U1 N41 C41 -164(4) . . . . ? N11 U1 N41 C41 21(4) . . . . ? N41 U1 N61 C65 26.8(3) . . . . ? N21 U1 N61 C65 -61.3(3) . . . . ? N81 U1 N61 C65 139.3(3) . . . . ? N31 U1 N61 C65 47.1(4) . . . . ? N71 U1 N61 C65 -138.0(3) . . . . ? N11 U1 N61 C65 -157.8(3) . . . . ? N41 U1 N61 N62 -145.2(3) . . . . ? N21 U1 N61 N62 126.7(2) . . . . ? N81 U1 N61 N62 -32.7(2) . . . . ? N31 U1 N61 N62 -124.9(3) . . . . ? N71 U1 N61 N62 49.9(2) . . . . ? N11 U1 N61 N62 30.2(3) . . . . ? C65 N61 N62 C63 -0.6(4) . . . . ? U1 N61 N62 C63 173.6(2) . . . . ? C65 N61 N62 B2 179.7(3) . . . . ? U1 N61 N62 B2 -6.1(4) . . . . ? N41 U1 N71 C75 117.5(3) . . . . ? N21 U1 N71 C75 25.6(3) . . . . ? N81 U1 N71 C75 -136.6(3) . . . . ? N31 U1 N71 C75 -39.6(4) . . . . ? N61 U1 N71 C75 143.5(3) . . . . ? N11 U1 N71 C75 -51.1(3) . . . . ? N41 U1 N71 N72 -84.2(3) . . . . ? N21 U1 N71 N72 -176.1(2) . . . . ? N81 U1 N71 N72 21.8(2) . . . . ? N31 U1 N71 N72 118.8(2) . . . . ? N61 U1 N71 N72 -58.2(2) . . . . ? N11 U1 N71 N72 107.3(2) . . . . ? C75 N71 N72 C73 0.9(4) . . . . ? U1 N71 N72 C73 -162.7(2) . . . . ? C75 N71 N72 B2 -173.2(3) . . . . ? U1 N71 N72 B2 23.1(4) . . . . ? N41 U1 N81 C85 -72.8(4) . . . . ? N21 U1 N81 C85 89.9(4) . . . . ? N31 U1 N81 C85 8.1(4) . . . . ? N71 U1 N81 C85 143.8(4) . . . . ? N61 U1 N81 C85 -147.2(4) . . . . ? N11 U1 N81 C85 71.9(4) . . . . ? N41 U1 N81 N82 107.1(3) . . . . ? N21 U1 N81 N82 -90.2(3) . . . . ? N31 U1 N81 N82 -172.1(3) . . . . ? N71 U1 N81 N82 -36.3(3) . . . . ? N61 U1 N81 N82 32.7(3) . . . . ? N11 U1 N81 N82 -108.2(3) . . . . ? C85 N81 N82 C83 0.3(4) . . . . ? U1 N81 N82 C83 -179.6(2) . . . . ? C85 N81 N82 B2 -174.1(3) . . . . ? U1 N81 N82 B2 6.0(5) . . . . ? N11 N12 C13 C14 -1.1(4) . . . . ? B1 N12 C13 C14 173.0(3) . . . . ? N11 N12 C13 C16 176.0(3) . . . . ? B1 N12 C13 C16 -9.8(6) . . . . ? N12 C13 C14 C15 0.9(4) . . . . ? C16 C13 C14 C15 -176.1(4) . . . . ? N12 N11 C15 C14 -0.4(4) . . . . ? U1 N11 C15 C14 166.0(2) . . . . ? N12 N11 C15 C17 -179.7(3) . . . . ? U1 N11 C15 C17 -13.4(6) . . . . ? C13 C14 C15 N11 -0.3(4) . . . . ? C13 C14 C15 C17 179.0(4) . . . . ? N21 N22 C23 C24 0.2(5) . . . . ? B1 N22 C23 C24 -178.5(4) . . . . ? N21 N22 C23 C26 -179.8(4) . . . . ? B1 N22 C23 C26 1.4(7) . . . . ? N22 C23 C24 C25 0.5(5) . . . . ? C26 C23 C24 C25 -179.4(5) . . . . ? N22 N21 C25 C24 1.3(5) . . . . ? U1 N21 C25 C24 -174.7(3) . . . . ? N22 N21 C25 C27 -178.7(4) . . . . ? U1 N21 C25 C27 5.3(6) . . . . ? C23 C24 C25 N21 -1.1(5) . . . . ? C23 C24 C25 C27 178.8(5) . . . . ? N31 N32 C33 C34 0.1(4) . . . . ? B1 N32 C33 C34 177.5(4) . . . . ? N31 N32 C33 C36 179.6(4) . . . . ? B1 N32 C33 C36 -3.0(6) . . . . ? N32 C33 C34 C35 -0.4(4) . . . . ? C36 C33 C34 C35 -180.0(4) . . . . ? N32 N31 C35 C34 -0.6(4) . . . . ? U1 N31 C35 C34 -165.2(3) . . . . ? N32 N31 C35 C37 178.3(3) . . . . ? U1 N31 C35 C37 13.7(5) . . . . ? C33 C34 C35 N31 0.7(5) . . . . ? C33 C34 C35 C37 -178.2(4) . . . . ? U1 N41 C41 C42 -149(4) . . . . ? U1 N41 C41 C46 31(4) . . . . ? N41 C41 C42 C43 -174.4(3) . . . . ? C46 C41 C42 C43 5.0(5) . . . . ? N41 C41 C42 C47 4.6(5) . . . . ? C46 C41 C42 C47 -176.0(3) . . . . ? C41 C42 C43 C44 -2.4(6) . . . . ? C47 C42 C43 C44 178.7(4) . . . . ? C42 C43 C44 C45 -1.9(6) . . . . ? C42 C43 C44 C48 174.2(4) . . . . ? C43 C44 C45 C46 3.5(6) . . . . ? C48 C44 C45 C46 -172.7(4) . . . . ? C44 C45 C46 C41 -0.8(6) . . . . ? C44 C45 C46 C49 178.3(4) . . . . ? N41 C41 C46 C45 175.9(3) . . . . ? C42 C41 C46 C45 -3.5(5) . . . . ? N41 C41 C46 C49 -3.2(5) . . . . ? C42 C41 C46 C49 177.4(3) . . . . ? N61 N62 C63 C64 0.2(4) . . . . ? B2 N62 C63 C64 179.9(3) . . . . ? N61 N62 C63 C66 178.3(4) . . . . ? B2 N62 C63 C66 -2.0(6) . . . . ? N62 C63 C64 C65 0.2(4) . . . . ? C66 C63 C64 C65 -177.8(4) . . . . ? N62 N61 C65 C64 0.7(4) . . . . ? U1 N61 C65 C64 -172.2(2) . . . . ? N62 N61 C65 C67 -176.2(3) . . . . ? U1 N61 C65 C67 10.9(5) . . . . ? C63 C64 C65 N61 -0.6(4) . . . . ? C63 C64 C65 C67 176.3(4) . . . . ? N71 N72 C73 C74 -0.5(4) . . . . ? B2 N72 C73 C74 173.3(3) . . . . ? N71 N72 C73 C76 178.0(3) . . . . ? B2 N72 C73 C76 -8.2(6) . . . . ? N72 C73 C74 C75 -0.2(4) . . . . ? C76 C73 C74 C75 -178.5(4) . . . . ? N72 N71 C75 C74 -1.0(4) . . . . ? U1 N71 C75 C74 159.1(2) . . . . ? N72 N71 C75 C77 179.1(3) . . . . ? U1 N71 C75 C77 -20.7(5) . . . . ? C73 C74 C75 N71 0.8(4) . . . . ? C73 C74 C75 C77 -179.4(4) . . . . ? N81 N82 C83 C84 0.2(4) . . . . ? B2 N82 C83 C84 174.3(3) . . . . ? N81 N82 C83 C86 -179.3(4) . . . . ? B2 N82 C83 C86 -5.3(6) . . . . ? N82 C83 C84 C85 -0.6(5) . . . . ? C86 C83 C84 C85 178.9(4) . . . . ? N82 N81 C85 C84 -0.7(5) . . . . ? U1 N81 C85 C84 179.2(3) . . . . ? N82 N81 C85 C87 175.2(4) . . . . ? U1 N81 C85 C87 -4.9(6) . . . . ? C83 C84 C85 N81 0.9(5) . . . . ? C83 C84 C85 C87 -174.7(4) . . . . ? C23 N22 B1 N12 -115.5(4) . . . . ? N21 N22 B1 N12 65.9(4) . . . . ? C23 N22 B1 N32 122.1(4) . . . . ? N21 N22 B1 N32 -56.5(4) . . . . ? C13 N12 B1 N22 114.7(4) . . . . ? N11 N12 B1 N22 -71.9(4) . . . . ? C13 N12 B1 N32 -121.8(4) . . . . ? N11 N12 B1 N32 51.6(4) . . . . ? C33 N32 B1 N22 -111.5(4) . . . . ? N31 N32 B1 N22 65.6(4) . . . . ? C33 N32 B1 N12 125.2(4) . . . . ? N31 N32 B1 N12 -57.7(4) . . . . ? C63 N62 B2 N72 120.5(4) . . . . ? N61 N62 B2 N72 -59.9(4) . . . . ? C63 N62 B2 N82 -114.6(4) . . . . ? N61 N62 B2 N82 65.1(4) . . . . ? C73 N72 B2 N62 -123.5(4) . . . . ? N71 N72 B2 N62 49.7(4) . . . . ? C73 N72 B2 N82 112.2(4) . . . . ? N71 N72 B2 N82 -74.7(4) . . . . ? C83 N82 B2 N62 120.0(4) . . . . ? N81 N82 B2 N62 -66.7(4) . . . . ? C83 N82 B2 N72 -116.7(4) . . . . ? N81 N82 B2 N72 56.6(4) . . . . ?