# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 186/1542 data_CRYSTALS_cif _audit_creation_date 99-04-09 _audit_creation_method CRYSTALS # VA288A #**************************************************************************** # The contents of this file between this point and the next #***** line # are held in the file CRYSTALS\SCRIPT\CIF.REF. # This is a character file which you may edit to reflect local # conditions # # 1. SUBMISSION DETAILS _publ_contact_author ; Pr L. G. Hubert-Pfalzgraf ; _publ_contact_author_phone ' 33 04 72 43 15 70 ' _publ_contact_author_fax ' 33 04 72 43 15 68 ' _publ_contact_author_email ' hubert@cismsun.univ-lyon1.fr ' _publ_requested_journal ' Dalton Trans. ' _publ_requested_coeditor_name ' ? ' _publ_contact_letter ; ; #============================================================================= # 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 ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? # Title of paper ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Other, Anthony N.' #<--'Last name, first name' ; ? # Address ; 'Else, S. O.' ; ? # Address ; #============================================================================== # 4. TEXT _publ_section_abstract ; ? #Text of the abstract ; _publ_section_comment ; ? #Text of the paper ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; # Add your own references - in alphabetic order Carruthers, J.R. and Watkin, D.J. (1979), (Chebychev Weighting) Acta Cryst, A35, 698-699 Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Walker, N., and Stuart, D. DIFABS. Acta Cryst, A39, 158-166 Watkin, D.J., Prout, C.K. Carruthers, R.J. & Betteridge, P. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_figure_captions ; ? #Captions to figures ; _publ_section_acknowledgements ; ? ; #========================================================================== # Now, all the strucure specific goodies #========================================================================== _computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 software (Enraf-Nonius, 1989)' _computing_data_reduction ; RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994) ; _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; # _computing_structure_solution 'SHELXS86 (Sheldrick, 1986)' #========================================================================== # NOW THE GOODIES TO BE ENTERED BY HAND #========================================================================== _chemical_melting_point ? _diffrn_radiation_monochromator ' graphite' _diffrn_measurement_device ' Enraf-nonius CAD4 ' _refine_ls_matrix_type ' full' _refine_ls_weighting_scheme ; Chebychev polynomial (Carruthers & Watkin, 1979) ; _atom_sites_solution_primary ' Direct_Methods' _atom_sites_solution_hydrogens ' Geometric' _refine_ls_hydrogen_treatment ; H atoms placed geometrically after each cycle, one overall isotropic thermal parameter refined ; #**************************************************************************** _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 17.938(5) _cell_angle_alpha 78.86(3) _cell_length_b 17.960(5) _cell_angle_beta 74.24(3) _cell_length_c 9.335(5) _cell_angle_gamma 78.84(2) _cell_volume 2807(4) _symmetry_cell_setting ' triclinic ' _symmetry_space_group_name_H-M 'P -1 ' 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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'Nb ' -2.1970 0.6210 17.6142 1.1887 12.0144 11.7660 4.0418 0.2048 3.5335 69.7957 3.7559 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C40 H90 Nb4 O20 ' _chemical_formula_moiety ' C40 H90 Nb4 O20 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1262.77 _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 161K _cell_formula_units_Z 2 _exptl_crystal_description ' ' _exptl_crystal_colour ' ' _exptl_crystal_size_min ? _exptl_crystal_size_mid ? _exptl_crystal_size_max ? _exptl_crystal_density_diffrn 1.49 _exptl_crystal_density_meas ? _exptl_crystal_F_000 1290.48 _exptl_absorpt_coefficient_mu 0.82 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_process_details 'refined from delta-F' _exptl_absorpt_correction_T_min 0.96 _exptl_absorpt_correction_T_max 1.00 _diffrn_standards_interval_time 3600s _diffrn_standards_number 2 _diffrn_standards_decay_% 6.56 _diffrn_ambient_temperature 161K _diffrn_reflns_number 3433 _reflns_number_total 3267 _diffrn_reflns_av_R_equivalents 0.03 _reflns_number_observed 2703 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 17 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _reflns_limit_h_min -13 _reflns_limit_h_max 14 _reflns_limit_k_min -13 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 7 _reflns_observed_criterion >2.00\s(I) _refine_diff_density_min -0.82 _refine_diff_density_max 1.95 _refine_ls_number_reflns 2703 _refine_ls_number_parameters 279 _refine_ls_R_factor_obs 0.0692 _refine_ls_wR_factor_obs 0.0801 _refine_ls_goodness_of_fit_obs 1.1257 _refine_ls_shift/esd_max 1.086399 _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method 2\q/\w loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type NB1 0.69765(9) 0.80049(8) 0.4057(2) 0.0204 1.0000 Uani NB2 0.69737(8) 0.99925(8) 0.3649(2) 0.0152 1.0000 Uani NB3 0.79390(8) 1.14639(8) 0.1089(2) 0.0166 1.0000 Uani NB4 0.76867(9) 1.34853(8) 0.0348(2) 0.0218 1.0000 Uani O1 0.6201(6) 0.8156(6) 0.300(1) 0.035(3) 1.0000 Uiso O2 0.7753(6) 0.7848(6) 0.508(1) 0.038(3) 1.0000 Uiso O3 0.6384(7) 0.7402(6) 0.569(1) 0.039(3) 1.0000 Uiso O4 0.7588(6) 0.7329(6) 0.271(1) 0.038(3) 1.0000 Uiso O5 0.7468(6) 0.8979(6) 0.277(1) 0.025(3) 1.0000 Uiso O6 0.6454(5) 0.9042(5) 0.488(1) 0.017(3) 1.0000 Uiso O7 0.7945(5) 1.0281(5) 0.172(1) 0.017(3) 1.0000 Uiso O8 0.6112(6) 1.0412(6) 0.517(1) 0.036(3) 1.0000 Uiso O9 0.7712(6) 0.9827(6) 0.481(1) 0.032(3) 1.0000 Uiso O10 0.6347(6) 1.0258(6) 0.224(1) 0.026(3) 1.0000 Uiso O11 0.7099(6) 1.1503(6) 0.021(1) 0.029(3) 1.0000 Uiso O12 0.7135(5) 1.1155(5) 0.321(1) 0.018(3) 1.0000 Uiso O13 0.7374(6) 1.2514(6) 0.187(1) 0.023(3) 1.0000 Uiso O14 0.8698(6) 1.1458(6) 0.211(1) 0.029(3) 1.0000 Uiso O15 0.8694(6) 1.1081(6) -0.060(1) 0.032(3) 1.0000 Uiso O16 0.8282(6) 1.2448(5) -0.040(1) 0.021(3) 1.0000 Uiso O17 0.8491(6) 1.3531(6) 0.129(1) 0.028(3) 1.0000 Uiso O18 0.7057(6) 1.4201(6) 0.161(1) 0.029(3) 1.0000 Uiso O19 0.8215(6) 1.4062(6) -0.142(1) 0.034(3) 1.0000 Uiso O20 0.6871(6) 1.3480(6) -0.053(1) 0.037(3) 1.0000 Uiso C1 0.592(2) 0.811(2) 0.177(3) 0.11(1) 1.0000 Uiso C2 0.605(2) 0.871(2) 0.055(3) 0.109(9) 1.0000 Uiso C3 0.519(2) 0.780(2) 0.219(3) 0.12(1) 1.0000 Uiso C4 0.812(2) 0.775(2) 0.620(4) 0.14(1) 1.0000 Uiso C5 0.760(3) 0.773(3) 0.760(6) 0.21(2) 1.0000 Uiso C6 0.889(2) 0.736(2) 0.604(4) 0.14(1) 1.0000 Uiso C7 0.567(1) 0.711(1) 0.615(2) 0.054(6) 1.0000 Uiso C8 0.541(1) 0.697(1) 0.782(3) 0.079(7) 1.0000 Uiso C9 0.582(2) 0.639(2) 0.550(3) 0.100(9) 1.0000 Uiso C10 0.828(1) 0.681(1) 0.262(2) 0.056(6) 1.0000 Uiso C11 0.867(1) 0.672(1) 0.101(3) 0.091(8) 1.0000 Uiso C12 0.810(1) 0.606(1) 0.359(3) 0.092(8) 1.0000 Uiso C13 0.824(1) 0.895(1) 0.178(2) 0.033(5) 1.0000 Uiso C14 0.8255(9) 0.9694(9) 0.079(2) 0.026(5) 1.0000 Uiso C15 0.571(1) 0.919(1) 0.594(2) 0.050(6) 1.0000 Uiso C16 0.577(1) 0.991(1) 0.650(2) 0.068(7) 1.0000 Uiso C17 0.799(1) 1.0291(9) 0.576(2) 0.14(1) 1.0000 Uiso C18 0.728(2) 1.054(2) 0.703(3) 0.16(1) 1.0000 Uiso C19 0.858(1) 0.981(2) 0.641(3) 0.13(1) 1.0000 Uiso C20 0.607(1) 1.071(1) 0.112(2) 0.061(6) 1.0000 Uiso C21 0.639(2) 1.134(2) 0.032(4) 0.14(1) 1.0000 Uiso C22 0.676(1) 1.175(1) 0.409(2) 0.052(6) 1.0000 Uiso C23 0.677(2) 1.247(2) 0.318(3) 0.106(9) 1.0000 Uiso C24 0.943(1) 1.1281(9) 0.255(2) 0.16(1) 1.0000 Uiso C25 1.006(1) 1.158(1) 0.126(2) 0.079(7) 1.0000 Uiso C26 0.935(2) 1.168(2) 0.392(3) 0.18(2) 1.0000 Uiso C27 0.891(1) 1.157(1) -0.201(2) 0.043(5) 1.0000 Uiso C28 0.887(1) 1.236(1) -0.175(2) 0.053(6) 1.0000 Uiso C29 0.859(1) 1.392(1) 0.239(3) 0.085(8) 1.0000 Uiso C30 0.939(1) 1.409(1) 0.210(2) 0.066(7) 1.0000 Uiso C31 0.842(3) 1.340(3) 0.378(6) 0.23(2) 1.0000 Uiso C32 0.632(1) 1.466(1) 0.183(2) 0.039(5) 1.0000 Uiso C33 0.600(1) 1.474(1) 0.345(2) 0.055(6) 1.0000 Uiso C34 0.641(1) 1.545(1) 0.087(2) 0.069(7) 1.0000 Uiso C35 0.886(1) 1.445(1) -0.180(2) 0.045(5) 1.0000 Uiso C36 0.932(2) 1.439(2) -0.342(3) 0.106(9) 1.0000 Uiso C37 0.860(2) 1.525(2) -0.157(3) 0.111(9) 1.0000 Uiso C38 0.640(1) 1.348(1) -0.151(3) 0.087(8) 1.0000 Uiso C39 0.602(2) 1.427(2) -0.191(3) 0.12(1) 1.0000 Uiso C40 0.678(1) 1.300(1) -0.264(3) 0.074(7) 1.0000 Uiso H11 0.6334 0.7702 0.1215 0.119(8) 1.0000 Uiso H21 0.5850 0.8650 -0.0297 0.119(8) 1.0000 Uiso H22 0.6620 0.8778 0.0186 0.119(8) 1.0000 Uiso H23 0.5756 0.9219 0.0931 0.119(8) 1.0000 Uiso H31 0.4994 0.7803 0.1273 0.119(8) 1.0000 Uiso H32 0.4773 0.8208 0.2788 0.119(8) 1.0000 Uiso H33 0.5205 0.7319 0.2820 0.119(8) 1.0000 Uiso H41 0.8208 0.8253 0.6448 0.119(8) 1.0000 Uiso H51 0.7904 0.7620 0.8447 0.119(8) 1.0000 Uiso H52 0.7212 0.8162 0.7731 0.119(8) 1.0000 Uiso H53 0.7336 0.7232 0.7796 0.119(8) 1.0000 Uiso H61 0.9145 0.7306 0.6828 0.119(8) 1.0000 Uiso H62 0.9243 0.7662 0.5051 0.119(8) 1.0000 Uiso H63 0.8931 0.6836 0.5696 0.119(8) 1.0000 Uiso H71 0.5276 0.7503 0.5710 0.119(8) 1.0000 Uiso H81 0.4904 0.6776 0.8215 0.119(8) 1.0000 Uiso H82 0.5347 0.7479 0.8268 0.119(8) 1.0000 Uiso H83 0.5821 0.6605 0.8294 0.119(8) 1.0000 Uiso H91 0.5330 0.6132 0.5778 0.119(8) 1.0000 Uiso H92 0.6240 0.6000 0.5893 0.119(8) 1.0000 Uiso H93 0.5999 0.6471 0.4363 0.119(8) 1.0000 Uiso H101 0.8669 0.7033 0.3005 0.119(8) 1.0000 Uiso H111 0.9183 0.6352 0.0915 0.119(8) 1.0000 Uiso H112 0.8786 0.7224 0.0383 0.119(8) 1.0000 Uiso H113 0.8316 0.6504 0.0574 0.119(8) 1.0000 Uiso H121 0.8576 0.5663 0.3566 0.119(8) 1.0000 Uiso H122 0.7838 0.6136 0.4651 0.119(8) 1.0000 Uiso H123 0.7717 0.5852 0.3180 0.119(8) 1.0000 Uiso H131 0.8648 0.8855 0.2369 0.119(8) 1.0000 Uiso H132 0.8342 0.8514 0.1167 0.119(8) 1.0000 Uiso H141 0.8813 0.9763 0.0211 0.119(8) 1.0000 Uiso H142 0.7939 0.9739 0.0026 0.119(8) 1.0000 Uiso H151 0.5635 0.8744 0.6798 0.119(8) 1.0000 Uiso H152 0.5259 0.9267 0.5455 0.119(8) 1.0000 Uiso H161 0.6119 0.9785 0.7219 0.119(8) 1.0000 Uiso H162 0.5244 1.0161 0.7006 0.119(8) 1.0000 Uiso H171 0.8205 1.0759 0.4954 0.119(8) 1.0000 Uiso H181 0.7505 1.0860 0.7652 0.119(8) 1.0000 Uiso H182 0.6847 1.0835 0.6755 0.119(8) 1.0000 Uiso H183 0.7167 1.0061 0.7789 0.119(8) 1.0000 Uiso H191 0.8818 1.0077 0.6912 0.119(8) 1.0000 Uiso H192 0.9040 0.9587 0.5511 0.119(8) 1.0000 Uiso H193 0.8368 0.9352 0.7022 0.119(8) 1.0000 Uiso H201 0.5502 1.0901 0.1561 0.119(8) 1.0000 Uiso H202 0.6092 1.0377 0.0345 0.119(8) 1.0000 Uiso H211 0.6002 1.1805 0.0674 0.119(8) 1.0000 Uiso H212 0.6363 1.1355 -0.0783 0.119(8) 1.0000 Uiso H221 0.7030 1.1732 0.4910 0.119(8) 1.0000 Uiso H222 0.6195 1.1668 0.4593 0.119(8) 1.0000 Uiso H231 0.6801 1.2877 0.3766 0.119(8) 1.0000 Uiso H232 0.6255 1.2635 0.2841 0.119(8) 1.0000 Uiso H241 0.9517 1.0699 0.2942 0.119(8) 1.0000 Uiso H251 1.0578 1.1483 0.1479 0.119(8) 1.0000 Uiso H252 0.9904 1.2143 0.0936 0.119(8) 1.0000 Uiso H253 1.0092 1.1307 0.0365 0.119(8) 1.0000 Uiso H261 0.9833 1.1557 0.4486 0.119(8) 1.0000 Uiso H262 0.9224 1.2266 0.3867 0.119(8) 1.0000 Uiso H263 0.8894 1.1520 0.4987 0.119(8) 1.0000 Uiso H271 0.9451 1.1374 -0.2588 0.119(8) 1.0000 Uiso H272 0.8532 1.1563 -0.2656 0.119(8) 1.0000 Uiso H281 0.9382 1.2440 -0.1599 0.119(8) 1.0000 Uiso H282 0.8729 1.2752 -0.2585 0.119(8) 1.0000 Uiso H291 0.8225 1.4443 0.2407 0.119(8) 1.0000 Uiso H301 0.9466 1.4374 0.2834 0.119(8) 1.0000 Uiso H302 0.9537 1.4408 0.1042 0.119(8) 1.0000 Uiso H303 0.9769 1.3593 0.2063 0.119(8) 1.0000 Uiso H311 0.8466 1.3644 0.4709 0.119(8) 1.0000 Uiso H312 0.8796 1.2912 0.3792 0.119(8) 1.0000 Uiso H313 0.7869 1.3277 0.4092 0.119(8) 1.0000 Uiso H321 0.5964 1.4364 0.1508 0.119(8) 1.0000 Uiso H331 0.5467 1.5065 0.3646 0.119(8) 1.0000 Uiso H332 0.6365 1.5007 0.3787 0.119(8) 1.0000 Uiso H333 0.5961 1.4231 0.4117 0.119(8) 1.0000 Uiso H341 0.5891 1.5802 0.0983 0.119(8) 1.0000 Uiso H342 0.6776 1.5701 0.1221 0.119(8) 1.0000 Uiso H343 0.6633 1.5409 -0.0223 0.119(8) 1.0000 Uiso H351 0.9203 1.4177 -0.1080 0.119(8) 1.0000 Uiso H361 0.9809 1.4662 -0.3685 0.119(8) 1.0000 Uiso H362 0.9000 1.4629 -0.4141 0.119(8) 1.0000 Uiso H363 0.9525 1.3836 -0.3561 0.119(8) 1.0000 Uiso H371 0.9047 1.5570 -0.1839 0.119(8) 1.0000 Uiso H372 0.8301 1.5314 -0.0505 0.119(8) 1.0000 Uiso H373 0.8229 1.5526 -0.2249 0.119(8) 1.0000 Uiso H381 0.5964 1.3157 -0.0874 0.119(8) 1.0000 Uiso H391 0.5662 1.4277 -0.2594 0.119(8) 1.0000 Uiso H392 0.6428 1.4601 -0.2468 0.119(8) 1.0000 Uiso H393 0.5693 1.4501 -0.0999 0.119(8) 1.0000 Uiso H401 0.6429 1.3000 -0.3338 0.119(8) 1.0000 Uiso H402 0.7265 1.3229 -0.3322 0.119(8) 1.0000 Uiso H403 0.6958 1.2462 -0.2245 0.119(8) 1.0000 Uiso 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 NB1 0.023(1) 0.016(1) 0.024(1) -0.0006(8) -0.0057(8) -0.0043(8) NB2 0.015(1) 0.017(1) 0.013(1) -0.0016(8) -0.0035(8) -0.0018(8) NB3 0.017(1) 0.018(1) 0.015(1) -0.0042(8) -0.0008(8) -0.0035(8) NB4 0.028(1) 0.017(1) 0.025(1) -0.0021(8) -0.0107(9) -0.0046(8) _refine_ls_extinction_coef 'none' 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 NB1 . O1 . 1.86(1) yes NB1 . O2 . 1.84(1) yes NB1 . O3 . 1.88(1) yes NB1 . O4 . 1.89(1) yes NB1 . O5 . 2.12(1) yes NB1 . O6 . 2.104(9) yes NB2 . O5 . 2.08(1) yes NB2 . O6 . 2.094(9) yes NB2 . O7 . 2.196(9) yes NB2 . O8 . 1.94(1) yes NB2 . O9 . 1.87(1) yes NB2 . O10 . 1.89(1) yes NB2 . O12 . 2.11(1) yes NB3 . O7 . 2.09(1) yes NB3 . O11 . 1.89(1) yes NB3 . O12 . 2.157(9) yes NB3 . O13 . 2.12(1) yes NB3 . O14 . 1.86(1) yes NB3 . O15 . 1.92(1) yes NB3 . O16 . 2.11(1) yes NB4 . O13 . 2.09(1) yes NB4 . O16 . 2.11(1) yes NB4 . O17 . 1.91(1) yes NB4 . O18 . 1.90(1) yes NB4 . O19 . 1.89(1) yes NB4 . O20 . 1.86(1) yes O1 . C1 . 1.39(3) yes O2 . C4 . 1.34(3) yes O3 . C7 . 1.41(2) yes O4 . C10 . 1.39(2) yes O5 . C13 . 1.44(2) yes O6 . C15 . 1.44(2) yes O7 . C14 . 1.43(2) yes O8 . C16 . 1.45(2) yes O9 . C17 . 1.55(2) yes O10 . C20 . 1.34(2) yes O11 . C21 . 1.34(3) yes O12 . C22 . 1.42(2) yes O13 . C23 . 1.39(3) yes O14 . C24 . 1.43(2) yes O15 . C27 . 1.43(2) yes O16 . C28 . 1.41(2) yes O17 . C29 . 1.42(2) yes O18 . C32 . 1.40(2) yes O19 . C35 . 1.40(2) yes O20 . C38 . 1.41(2) yes C1 . C2 . 1.42(4) yes C1 . C3 . 1.45(4) yes C1 . H11 . 1.03(3) no C2 . H21 . 0.99(3) no C2 . H22 . 1.01(3) no C2 . H23 . 1.03(3) no C3 . H31 . 1.01(3) no C3 . H32 . 1.06(3) no C3 . H33 . 0.95(3) no C4 . C5 . 1.39(5) yes C4 . C6 . 1.40(4) yes C4 . H41 . 1.03(3) no C5 . H51 . 1.05(5) no C5 . H52 . 0.94(5) no C5 . H53 . 1.05(5) no C6 . H61 . 0.96(3) no C6 . H62 . 1.08(3) no C6 . H63 . 1.03(3) no C7 . C8 . 1.48(3) yes C7 . C9 . 1.49(3) yes C7 . H71 . 1.00(2) no C8 . H81 . 1.00(2) no C8 . H82 . 1.04(2) no C8 . H83 . 1.02(2) no C9 . H91 . 1.02(3) no C9 . H92 . 1.02(3) no C9 . H93 . 1.01(3) no C10 . C11 . 1.50(3) yes C10 . C12 . 1.51(3) yes C10 . H101 . 1.04(2) no C11 . H111 . 1.02(2) no C11 . H112 . 1.01(3) no C11 . H113 . 1.00(2) no C12 . H121 . 1.00(3) no C12 . H122 . 1.00(3) no C12 . H123 . 1.03(2) no C13 . C14 . 1.47(2) yes C13 . H131 . 1.00(2) no C13 . H132 . 1.01(2) no C14 . H141 . 1.02(2) no C14 . H142 . 1.01(2) no C15 . C16 . 1.51(3) yes C15 . H151 . 1.02(2) no C15 . H152 . 1.01(2) no C16 . H161 . 1.00(2) no C16 . H162 . 1.00(2) no C17 . C18 . 1.54(2) yes C17 . C19 . 1.43(2) yes C17 . H171 . 1.07(2) no C18 . H181 . 1.07(3) no C18 . H182 . 0.93(3) no C18 . H183 . 1.02(4) no C19 . H191 . 0.95(2) no C19 . H192 . 1.08(3) no C19 . H193 . 0.99(3) no C20 . C21 . 1.36(4) yes C20 . H201 . 1.00(2) no C20 . H202 . 1.02(2) no C21 . H211 . 1.03(3) no C21 . H212 . 1.03(3) no C22 . C23 . 1.41(3) yes C22 . H221 . 1.01(2) no C22 . H222 . 1.01(2) no C23 . H231 . 1.01(3) no C23 . H232 . 1.03(3) no C24 . C25 . 1.51(2) yes C24 . C26 . 1.55(2) yes C24 . H241 . 1.04(1) no C25 . H251 . 0.98(2) no C25 . H252 . 1.00(2) no C25 . H253 . 1.03(2) no C26 . H261 . 1.10(3) no C26 . H262 . 1.02(4) no C26 . H263 . 1.13(3) no C27 . C28 . 1.47(3) yes C27 . H271 . 1.01(2) no C27 . H272 . 1.02(2) no C28 . H281 . 1.01(2) no C28 . H282 . 1.00(2) no C29 . C30 . 1.47(3) yes C29 . C31 . 1.43(5) yes C29 . H291 . 1.03(2) no C30 . H301 . 0.98(2) no C30 . H302 . 1.03(2) no C30 . H303 . 1.01(2) no C31 . H311 . 1.07(5) no C31 . H312 . 1.00(5) no C31 . H313 . 1.01(5) no C32 . C33 . 1.50(3) yes C32 . C34 . 1.54(3) yes C32 . H321 . 1.04(2) no C33 . H331 . 1.01(2) no C33 . H332 . 1.02(2) no C33 . H333 . 1.01(2) no C34 . H341 . 1.01(2) no C34 . H342 . 1.01(2) no C34 . H343 . 1.00(2) no C35 . C36 . 1.53(3) yes C35 . C37 . 1.46(3) yes C35 . H351 . 1.03(2) no C36 . H361 . 1.03(3) no C36 . H362 . 0.99(3) no C36 . H363 . 1.02(3) no C37 . H371 . 1.03(3) no C37 . H372 . 1.01(3) no C37 . H373 . 1.03(3) no C38 . C39 . 1.47(3) yes C38 . C40 . 1.44(3) yes C38 . H381 . 1.04(2) no C39 . H391 . 1.01(3) no C39 . H392 . 1.01(3) no C39 . H393 . 1.00(3) no C40 . H401 . 1.02(2) no C40 . H402 . 1.03(2) no C40 . H403 . 0.99(2) 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 O1 . NB1 . O2 . 179.2(5) no O1 . NB1 . O3 . 91.4(5) no O2 . NB1 . O3 . 89.0(5) no O1 . NB1 . O4 . 88.1(5) no O2 . NB1 . O4 . 91.0(5) no O3 . NB1 . O4 . 106.7(5) no O1 . NB1 . O5 . 92.4(4) no O2 . NB1 . O5 . 87.5(4) no O3 . NB1 . O5 . 159.1(4) no O4 . NB1 . O5 . 94.0(4) no O1 . NB1 . O6 . 87.9(4) no O2 . NB1 . O6 . 92.9(4) no O3 . NB1 . O6 . 93.7(4) no O4 . NB1 . O6 . 159.3(4) no O5 . NB1 . O6 . 65.9(4) no O5 . NB2 . O6 . 66.8(4) no O5 . NB2 . O7 . 73.7(4) no O6 . NB2 . O7 . 140.3(4) no O5 . NB2 . O8 . 141.9(4) no O6 . NB2 . O8 . 75.4(4) no O7 . NB2 . O8 . 144.3(4) no O5 . NB2 . O9 . 90.9(4) no O6 . NB2 . O9 . 92.2(4) no O7 . NB2 . O9 . 85.6(4) no O8 . NB2 . O9 . 95.0(4) no O5 . NB2 . O10 . 89.7(4) no O6 . NB2 . O10 . 96.8(4) no O7 . NB2 . O10 . 85.4(4) no O8 . NB2 . O10 . 90.4(4) no O9 . NB2 . O10 . 170.4(4) no O5 . NB2 . O12 . 138.8(4) no O6 . NB2 . O12 . 154.4(4) no O7 . NB2 . O12 . 65.1(3) no O8 . NB2 . O12 . 79.2(4) no O9 . NB2 . O12 . 86.5(4) no O10 . NB2 . O12 . 86.7(4) no O7 . NB3 . O11 . 89.0(4) no O7 . NB3 . O12 . 66.1(4) no O11 . NB3 . O12 . 86.1(4) no O7 . NB3 . O13 . 140.1(4) no O11 . NB3 . O13 . 88.1(4) no O12 . NB3 . O13 . 74.0(4) no O7 . NB3 . O14 . 91.9(4) no O11 . NB3 . O14 . 174.7(4) no O12 . NB3 . O14 . 89.4(4) no O13 . NB3 . O14 . 87.9(4) no O7 . NB3 . O15 . 79.0(4) no O11 . NB3 . O15 . 92.3(4) no O12 . NB3 . O15 . 145.1(4) no O13 . NB3 . O15 . 140.8(4) no O14 . NB3 . O15 . 93.1(4) no O7 . NB3 . O16 . 153.7(4) no O11 . NB3 . O16 . 90.5(4) no O12 . NB3 . O16 . 140.1(4) no O13 . NB3 . O16 . 66.1(4) no O14 . NB3 . O16 . 91.0(4) no O15 . NB3 . O16 . 74.7(4) no O13 . NB4 . O16 . 66.8(4) no O13 . NB4 . O17 . 90.7(4) no O16 . NB4 . O17 . 91.2(4) no O13 . NB4 . O18 . 95.1(4) no O16 . NB4 . O18 . 161.6(4) no O17 . NB4 . O18 . 85.6(4) no O13 . NB4 . O19 . 158.1(4) no O16 . NB4 . O19 . 91.3(4) no O17 . NB4 . O19 . 89.5(4) no O18 . NB4 . O19 . 106.7(5) no O13 . NB4 . O20 . 89.9(4) no O16 . NB4 . O20 . 91.6(4) no O17 . NB4 . O20 . 177.2(5) no O18 . NB4 . O20 . 91.6(4) no O19 . NB4 . O20 . 91.0(5) no NB1 . O1 . C1 . 153.4(15) no NB1 . O2 . C4 . 161.6(18) no NB1 . O3 . C7 . 141.3(11) no NB1 . O4 . C10 . 136.4(11) no NB1 . O5 . NB2 . 113.5(5) no NB1 . O5 . C13 . 124.4(9) no NB2 . O5 . C13 . 117.7(9) no NB1 . O6 . NB2 . 113.7(4) no NB1 . O6 . C15 . 127.7(10) no NB2 . O6 . C15 . 117.2(9) no NB2 . O7 . NB3 . 112.9(4) no NB2 . O7 . C14 . 114.2(8) no NB3 . O7 . C14 . 127.6(9) no NB2 . O8 . C16 . 119.4(11) no NB2 . O9 . C17 . 137.3(8) no NB2 . O10 . C20 . 154.7(12) no NB3 . O11 . C21 . 149.8(17) no NB2 . O12 . NB3 . 113.8(4) no NB2 . O12 . C22 . 128.4(10) no NB3 . O12 . C22 . 117.7(10) no NB3 . O13 . NB4 . 113.5(5) no NB3 . O13 . C23 . 117.0(13) no NB4 . O13 . C23 . 128.6(14) no NB3 . O14 . C24 . 160.9(9) no NB3 . O15 . C27 . 121.2(10) no NB3 . O16 . NB4 . 113.5(4) no NB3 . O16 . C28 . 119.2(10) no NB4 . O16 . C28 . 127.2(10) no NB4 . O17 . C29 . 137.8(12) no NB4 . O18 . C32 . 139.9(10) no NB4 . O19 . C35 . 135.1(10) no NB4 . O20 . C38 . 166.3(13) no O1 . C1 . C2 . 115.5(25) no O1 . C1 . C3 . 113.4(25) no C2 . C1 . C3 . 119.2(27) no O1 . C1 . H11 . 104.6(24) no C2 . C1 . H11 . 94.9(25) no C3 . C1 . H11 . 105.6(26) no C1 . C2 . H21 . 112.4(27) no C1 . C2 . H22 . 111.8(26) no H21 . C2 . H22 . 109.6(27) no C1 . C2 . H23 . 108.3(26) no H21 . C2 . H23 . 107.9(26) no H22 . C2 . H23 . 106.5(26) no C1 . C3 . H31 . 110.9(29) no C1 . C3 . H32 . 105.7(26) no H31 . C3 . H32 . 104.6(27) no C1 . C3 . H33 . 113.4(29) no H31 . C3 . H33 . 112.9(30) no H32 . C3 . H33 . 108.7(29) no O2 . C4 . C5 . 112.5(35) no O2 . C4 . C6 . 120.9(32) no C5 . C4 . C6 . 120.5(38) no O2 . C4 . H41 . 113.8(30) no C5 . C4 . H41 . 82.5(32) no C6 . C4 . H41 . 97.7(30) no C4 . C5 . H51 . 110.2(43) no C4 . C5 . H52 . 115.3(46) no H51 . C5 . H52 . 110.5(46) no C4 . C5 . H53 . 107.1(42) no H51 . C5 . H53 . 102.5(41) no H52 . C5 . H53 . 110.5(46) no C4 . C6 . H61 . 120.2(35) no C4 . C6 . H62 . 106.9(31) no H61 . C6 . H62 . 106.4(30) no C4 . C6 . H63 . 110.0(31) no H61 . C6 . H63 . 110.4(32) no H62 . C6 . H63 . 101.1(29) no O3 . C7 . C8 . 110.3(16) no O3 . C7 . C9 . 105.1(17) no C8 . C7 . C9 . 111.7(19) no O3 . C7 . H71 . 107.1(17) no C8 . C7 . H71 . 111.6(18) no C9 . C7 . H71 . 110.8(19) no C7 . C8 . H81 . 113.8(20) no C7 . C8 . H82 . 111.0(20) no H81 . C8 . H82 . 106.2(21) no C7 . C8 . H83 . 112.6(20) no H81 . C8 . H83 . 108.0(22) no H82 . C8 . H83 . 104.5(20) no C7 . C9 . H91 . 111.2(23) no C7 . C9 . H92 . 111.7(22) no H91 . C9 . H92 . 106.6(24) no C7 . C9 . H93 . 112.9(23) no H91 . C9 . H93 . 107.0(24) no H92 . C9 . H93 . 107.1(25) no O4 . C10 . C11 . 110.7(17) no O4 . C10 . C12 . 109.0(17) no C11 . C10 . C12 . 112.5(19) no O4 . C10 . H101 . 108.8(17) no C11 . C10 . H101 . 106.0(18) no C12 . C10 . H101 . 109.8(18) no C10 . C11 . H111 . 112.2(21) no C10 . C11 . H112 . 111.2(22) no H111 . C11 . H112 . 107.4(23) no C10 . C11 . H113 . 109.8(21) no H111 . C11 . H113 . 107.9(23) no H112 . C11 . H113 . 108.2(23) no C10 . C12 . H121 . 112.6(22) no C10 . C12 . H122 . 111.3(22) no H121 . C12 . H122 . 109.6(24) no C10 . C12 . H123 . 108.2(21) no H121 . C12 . H123 . 107.3(23) no H122 . C12 . H123 . 107.7(23) no O5 . C13 . C14 . 106.1(13) no O5 . C13 . H131 . 110.5(14) no C14 . C13 . H131 . 111.1(15) no O5 . C13 . H132 . 109.9(14) no C14 . C13 . H132 . 111.0(15) no H131 . C13 . H132 . 108.3(16) no O7 . C14 . C13 . 107.9(13) no O7 . C14 . H141 . 109.2(13) no C13 . C14 . H141 . 110.9(14) no O7 . C14 . H142 . 110.4(13) no C13 . C14 . H142 . 111.3(14) no H141 . C14 . H142 . 107.2(15) no O6 . C15 . C16 . 103.8(15) no O6 . C15 . H151 . 110.9(16) no C16 . C15 . H151 . 111.2(17) no O6 . C15 . H152 . 111.9(16) no C16 . C15 . H152 . 112.1(18) no H151 . C15 . H152 . 106.9(17) no O8 . C16 . C15 . 105.6(16) no O8 . C16 . H161 . 109.5(18) no C15 . C16 . H161 . 110.9(19) no O8 . C16 . H162 . 109.6(18) no C15 . C16 . H162 . 111.7(19) no H161 . C16 . H162 . 109.4(21) no O9 . C17 . C18 . 109.0(1) no O9 . C17 . C19 . 109.0(1) no C18 . C17 . C19 . 109.0(1) no O9 . C17 . H171 . 103.2(16) no C18 . C17 . H171 . 114.0(19) no C19 . C17 . H171 . 112.4(19) no C17 . C18 . H181 . 105.9(21) no C17 . C18 . H182 . 117.2(23) no H181 . C18 . H182 . 109.1(26) no C17 . C18 . H183 . 107.1(19) no H181 . C18 . H183 . 102.5(26) no H182 . C18 . H183 . 113.8(32) no C17 . C19 . H191 . 113.5(22) no C17 . C19 . H192 . 108.3(17) no H191 . C19 . H192 . 106.6(23) no C17 . C19 . H193 . 109.0(18) no H191 . C19 . H193 . 114.9(27) no H192 . C19 . H193 . 103.9(24) no O10 . C20 . C21 . 122.7(22) no O10 . C20 . H201 . 107.1(18) no C21 . C20 . H201 . 106.4(23) no O10 . C20 . H202 . 107.0(18) no C21 . C20 . H202 . 104.8(23) no H201 . C20 . H202 . 108.3(19) no O11 . C21 . C20 . 127.9(29) no O11 . C21 . H211 . 105.0(29) no C20 . C21 . H211 . 105.9(31) no O11 . C21 . H212 . 104.7(29) no C20 . C21 . H212 . 106.6(30) no H211 . C21 . H212 . 104.8(31) no O12 . C22 . C23 . 110.1(18) no O12 . C22 . H221 . 110.1(16) no C23 . C22 . H221 . 109.0(19) no O12 . C22 . H222 . 109.9(16) no C23 . C22 . H222 . 109.8(20) no H221 . C22 . H222 . 107.9(18) no O13 . C23 . C22 . 116.2(22) no O13 . C23 . H231 . 107.4(23) no C22 . C23 . H231 . 110.8(25) no O13 . C23 . H232 . 106.6(23) no C22 . C23 . H232 . 109.3(24) no H231 . C23 . H232 . 106.1(25) no O14 . C24 . C25 . 109.0(1) no O14 . C24 . C26 . 109.0(1) no C25 . C24 . C26 . 109.0(1) no O14 . C24 . H241 . 108.4(17) no C25 . C24 . H241 . 116.2(17) no C26 . C24 . H241 . 105.1(19) no C24 . C25 . H251 . 113.8(17) no C24 . C25 . H252 . 109.7(15) no H251 . C25 . H252 . 111.0(21) no C24 . C25 . H253 . 106.8(15) no H251 . C25 . H253 . 108.6(19) no H252 . C25 . H253 . 106.7(20) no C24 . C26 . H261 . 118.4(23) no C24 . C26 . H262 . 121.9(22) no H261 . C26 . H262 . 100.5(26) no C24 . C26 . H263 . 117.8(21) no H261 . C26 . H263 . 94.1(21) no H262 . C26 . H263 . 98.9(26) no O15 . C27 . C28 . 109.8(15) no O15 . C27 . H271 . 110.4(15) no C28 . C27 . H271 . 110.1(16) no O15 . C27 . H272 . 109.6(15) no C28 . C27 . H272 . 109.7(16) no H271 . C27 . H272 . 107.2(16) no O16 . C28 . C27 . 106.1(15) no O16 . C28 . H281 . 108.9(16) no C27 . C28 . H281 . 111.2(17) no O16 . C28 . H282 . 109.4(16) no C27 . C28 . H282 . 112.5(17) no H281 . C28 . H282 . 108.6(18) no O17 . C29 . C30 . 112.4(19) no O17 . C29 . C31 . 104.7(28) no C30 . C29 . C31 . 109.3(28) no O17 . C29 . H291 . 110.0(20) no C30 . C29 . H291 . 106.9(21) no C31 . C29 . H291 . 113.7(30) no C29 . C30 . H301 . 113.2(20) no C29 . C30 . H302 . 109.1(19) no H301 . C30 . H302 . 108.1(20) no C29 . C30 . H303 . 109.3(20) no H301 . C30 . H303 . 110.4(20) no H302 . C30 . H303 . 106.5(19) no C29 . C31 . H311 . 111.7(43) no C29 . C31 . H312 . 113.9(45) no H311 . C31 . H312 . 104.1(45) no C29 . C31 . H313 . 114.5(44) no H311 . C31 . H313 . 103.1(45) no H312 . C31 . H313 . 108.4(49) no O18 . C32 . C33 . 110.4(14) no O18 . C32 . C34 . 108.3(14) no C33 . C32 . C34 . 110.1(15) no O18 . C32 . H321 . 105.2(14) no C33 . C32 . H321 . 109.2(15) no C34 . C32 . H321 . 113.5(16) no C32 . C33 . H331 . 112.1(17) no C32 . C33 . H332 . 109.6(17) no H331 . C33 . H332 . 107.5(18) no C32 . C33 . H333 . 112.0(17) no H331 . C33 . H333 . 108.1(18) no H332 . C33 . H333 . 107.4(18) no C32 . C34 . H341 . 111.2(18) no C32 . C34 . H342 . 109.1(18) no H341 . C34 . H342 . 107.9(20) no C32 . C34 . H343 . 111.4(18) no H341 . C34 . H343 . 108.7(20) no H342 . C34 . H343 . 108.5(20) no O19 . C35 . C36 . 110.6(17) no O19 . C35 . C37 . 109.6(17) no C36 . C35 . C37 . 111.5(20) no O19 . C35 . H351 . 104.8(15) no C36 . C35 . H351 . 109.3(18) no C37 . C35 . H351 . 110.8(18) no C35 . C36 . H361 . 110.5(22) no C35 . C36 . H362 . 111.4(23) no H361 . C36 . H362 . 108.3(25) no C35 . C36 . H363 . 111.2(23) no H361 . C36 . H363 . 106.1(25) no H362 . C36 . H363 . 109.3(26) no C35 . C37 . H371 . 112.9(24) no C35 . C37 . H372 . 113.3(25) no H371 . C37 . H372 . 106.7(25) no C35 . C37 . H373 . 111.2(23) no H371 . C37 . H373 . 105.6(26) no H372 . C37 . H373 . 106.7(26) no O20 . C38 . C39 . 110.1(21) no O20 . C38 . C40 . 111.7(20) no C39 . C38 . C40 . 121.0(23) no O20 . C38 . H381 . 104.7(20) no C39 . C38 . H381 . 108.4(23) no C40 . C38 . H381 . 99.2(21) no C38 . C39 . H391 . 110.6(27) no C38 . C39 . H392 . 109.2(26) no H391 . C39 . H392 . 108.1(28) no C38 . C39 . H393 . 111.8(27) no H391 . C39 . H393 . 108.4(28) no H392 . C39 . H393 . 108.8(28) no C38 . C40 . H401 . 111.4(21) no C38 . C40 . H402 . 108.7(20) no H401 . C40 . H402 . 105.5(20) no C38 . C40 . H403 . 114.7(22) no H401 . C40 . H403 . 108.6(21) no H402 . C40 . H403 . 107.4(20) no