# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _audit_creation_date 02-14-01 _journal_coden_Cambridge 440 loop_ _publ_author_name 'Xavier Morise' 'P. Braunstein' 'Malcolm L. H. Green' 'Leigh H. Rees' 'I. Vei' _publ_contact_author_name 'Dr Xavier Morise' _publ_contact_author_address ; Laboratoire de Chimie de Coordn. UMR 7513 CNRS Universite Louis Pasteur 4 rue Blaise Pascal Strasbourg cedex 67070 FRANCE ; _publ_contact_author_phone '(+33) (0)390241316' _publ_contact_author_fax '(+33) (0)390245001' _publ_contact_author_email morise@chimie.u-strasbg.fr _publ_requested_journal 'New J. Chem.' _publ_requested_category FM _publ_section_title ; Moncocyclopentadienyl Complexes of Niobium, Tantalum and tungsten containing Heterodoifunctionl P,O Ligands. ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. ; data_CRYSTALS_cif_1 _database_code_CSD 190864 _audit_creation_method CRYSTALS_ver_12-03-99 #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 42.5519(5) _cell_angle_alpha 90 _cell_length_b 42.5519(5) _cell_angle_beta 90 _cell_length_c 8.7407(5) _cell_angle_gamma 120 _cell_volume 13706.1 _symmetry_cell_setting 'Trigonal ' _symmetry_space_group_name_H-M 'R -3 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/3,y+2/3,z+2/3' '-x+1/3,-y+2/3,-z+2/3' 'x+2/3,y+1/3,z+1/3' '-x+2/3,-y+1/3,-z+1/3' '-y,x-y,z' 'y,-x+y,-z' '-y+1/3,x-y+2/3,z+2/3' 'y+1/3,-x+y+2/3,-z+2/3' '-y+2/3,x-y+1/3,z+1/3' 'y+2/3,-x+y+1/3,-z+1/3' '-x+y,-x,z' 'x-y,x,-z' '-x+y+1/3,-x+2/3,z+2/3' 'x-y+1/3,x+2/3,-z+2/3' '-x+y+2/3,-x+1/3,z+1/3' 'x-y+2/3,x+1/3,-z+1/3' 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' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Ta ' -1.2580 6.5230 29.2024 1.7733 15.2293 9.3705 14.5135 0.2960 4.7649 63.3644 9.2435 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C30 H31 Cl3 O1 P1 Ta1 ' _chemical_formula_moiety ' C30 H31 Cl3 O1 P1 Ta1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 725.86 _cell_measurement_reflns_used 6889 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 18 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_max 0.10 _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 6431.330 _exptl_absorpt_coefficient_mu 3.945 # Sheldrick geometric definitions 0.79 0.85 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.85 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 6943 _reflns_number_total 6943 _diffrn_reflns_av_R_equivalents 0.00 # Number of reflections with Friedels Law is 6943 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6987 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_gt 5794 _diffrn_reflns_theta_min 5.16 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_h_max 55 _diffrn_reflns_limit_k_min -55 _diffrn_reflns_limit_k_max 55 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _reflns_limit_h_min -55 _reflns_limit_h_max 26 _reflns_limit_k_min 0 _reflns_limit_k_max 55 _reflns_limit_l_min 0 _reflns_limit_l_max 11 _refine_diff_density_min -0.67 _refine_diff_density_max 2.34 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 5794 _refine_ls_number_parameters 325 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0298 _refine_ls_goodness_of_fit_ref 1.0695 _refine_ls_shift/su_max 0.007337 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 1.81 -.961 1.15 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _refine_special_details ; Examination of the structure shows a considerable void. Difference Fourier maps show no significant electron density to be present in this region, suggesting it to be genuinely vacant. ; ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 COLLECT Software, Nonius BV 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type TA1 TA 0.638603(4) 0.114287(4) 0.333868(14) 0.0182 1.0000 Uani CL1 CL 0.67402(2) 0.12793(2) 0.10143(9) 0.0266 1.0000 Uani CL2 CL 0.65163(3) 0.06700(3) 0.3886(1) 0.0323 1.0000 Uani CL3 CL 0.58220(2) 0.08191(2) 0.4681(1) 0.0293 1.0000 Uani O1 O 0.61319(6) 0.13561(7) 0.2127(3) 0.0234 1.0000 Uani P1 P 0.59500(2) 0.06208(2) 0.1418(1) 0.0216 1.0000 Uani C1 C 0.57593(9) 0.0861(1) 0.0525(4) 0.0253 1.0000 Uani C2 C 0.58924(9) 0.12081(9) 0.0979(4) 0.0221 1.0000 Uani C3 C 0.5789(1) 0.1459(1) 0.0235(4) 0.0257 1.0000 Uani C4 C 0.55185(12) 0.13395(12) -0.0869(5) 0.0370 1.0000 Uani C5 C 0.54374(13) 0.15783(15) -0.1610(5) 0.0438 1.0000 Uani C6 C 0.56249(15) 0.19400(15) -0.1257(6) 0.0504 1.0000 Uani C7 C 0.58946(18) 0.20664(15) -0.0160(7) 0.0626 1.0000 Uani C8 C 0.59771(14) 0.18273(12) 0.0585(5) 0.0459 1.0000 Uani C9 C 0.6108(1) 0.0441(1) -0.0117(4) 0.0269 1.0000 Uani C10 C 0.64336(11) 0.04371(11) -0.0050(5) 0.0317 1.0000 Uani C11 C 0.65281(12) 0.02842(11) -0.1245(6) 0.0402 1.0000 Uani C12 C 0.63079(14) 0.01439(12) -0.2521(5) 0.0443 1.0000 Uani C13 C 0.59838(15) 0.01474(14) -0.2597(5) 0.0491 1.0000 Uani C14 C 0.58848(13) 0.02930(13) -0.1394(5) 0.0421 1.0000 Uani C15 C 0.55806(9) 0.02009(9) 0.2185(4) 0.0249 1.0000 Uani C16 C 0.56475(11) -0.00794(11) 0.2544(5) 0.0346 1.0000 Uani C17 C 0.53776(13) -0.03975(12) 0.3206(5) 0.0413 1.0000 Uani C18 C 0.50389(11) -0.04375(11) 0.3507(5) 0.0362 1.0000 Uani C19 C 0.4972(1) -0.01590(11) 0.3156(4) 0.0326 1.0000 Uani C20 C 0.5241(1) 0.01580(11) 0.2483(4) 0.0293 1.0000 Uani C21 C 0.6997(1) 0.16101(12) 0.4258(5) 0.0351 1.0000 Uani C22 C 0.68306(11) 0.13887(12) 0.5552(5) 0.0352 1.0000 Uani C23 C 0.6527(1) 0.14226(11) 0.5944(4) 0.0306 1.0000 Uani C24 C 0.6505(1) 0.1665(1) 0.4904(4) 0.0281 1.0000 Uani C25 C 0.6800(1) 0.1784(1) 0.3854(4) 0.0310 1.0000 Uani C26 C 0.73496(12) 0.16782(17) 0.3584(6) 0.0623 1.0000 Uani C27 C 0.69713(16) 0.11881(16) 0.6475(6) 0.0586 1.0000 Uani C29 C 0.62390(13) 0.17972(14) 0.4999(6) 0.0463 1.0000 Uani C28 C 0.63040(13) 0.12747(14) 0.7360(5) 0.0470 1.0000 Uani C30 C 0.69028(15) 0.20703(13) 0.2644(5) 0.0508 1.0000 Uani H11 H 0.5565 0.0747 -0.0268 0.0312 1.0000 Uiso H41 H 0.5379 0.1076 -0.1136 0.0460 1.0000 Uiso H51 H 0.5242 0.1486 -0.2402 0.0582 1.0000 Uiso H61 H 0.5567 0.2113 -0.1792 0.0678 1.0000 Uiso H71 H 0.6031 0.2331 0.0101 0.0780 1.0000 Uiso H81 H 0.6173 0.1921 0.1377 0.0572 1.0000 Uiso H101 H 0.6598 0.0543 0.0852 0.0386 1.0000 Uiso H111 H 0.6758 0.0275 -0.1181 0.0492 1.0000 Uiso H121 H 0.6382 0.0041 -0.3384 0.0523 1.0000 Uiso H131 H 0.5823 0.0046 -0.3512 0.0593 1.0000 Uiso H141 H 0.5649 0.0292 -0.1444 0.0524 1.0000 Uiso H161 H 0.5891 -0.0051 0.2325 0.0429 1.0000 Uiso H171 H 0.5427 -0.0598 0.3465 0.0505 1.0000 Uiso H181 H 0.4844 -0.0667 0.3976 0.0384 1.0000 Uiso H191 H 0.4729 -0.0186 0.3387 0.0350 1.0000 Uiso H201 H 0.5189 0.0356 0.2211 0.0348 1.0000 Uiso H261 H 0.7411 0.1843 0.2679 0.0667 1.0000 Uiso H262 H 0.7546 0.1795 0.4368 0.0667 1.0000 Uiso H263 H 0.7327 0.1443 0.3254 0.0667 1.0000 Uiso H271 H 0.6798 0.1054 0.7323 0.0751 1.0000 Uiso H272 H 0.7213 0.1365 0.6916 0.0751 1.0000 Uiso H273 H 0.6997 0.1012 0.5802 0.0751 1.0000 Uiso H291 H 0.6280 0.1966 0.4127 0.0602 1.0000 Uiso H292 H 0.6273 0.1928 0.5988 0.0602 1.0000 Uiso H293 H 0.5986 0.1586 0.4944 0.0602 1.0000 Uiso H281 H 0.6105 0.1336 0.7362 0.0479 1.0000 Uiso H282 H 0.6461 0.1384 0.8279 0.0479 1.0000 Uiso H283 H 0.6196 0.1005 0.7386 0.0479 1.0000 Uiso H301 H 0.6715 0.2146 0.2597 0.0521 1.0000 Uiso H302 H 0.7144 0.2285 0.2902 0.0521 1.0000 Uiso H303 H 0.6918 0.1970 0.1630 0.0521 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 Ta1 0.01421(7) 0.02363(8) 0.01560(7) 0.00281(5) 0.00120(5) 0.00870(5) Cl1 0.0211(4) 0.0324(4) 0.0216(4) 0.0024(3) 0.0051(3) 0.0099(3) Cl2 0.0360(5) 0.0372(5) 0.0302(4) 0.0029(4) -0.0057(4) 0.0231(4) Cl3 0.0208(4) 0.0341(4) 0.0240(4) 0.0007(3) 0.0052(3) 0.0069(3) O1 0.0228(11) 0.0275(12) 0.0208(11) 0.0009(9) -0.0015(9) 0.013(1) P1 0.0195(4) 0.0248(4) 0.0207(4) 0.0026(3) 0.0015(3) 0.0112(3) C1 0.0248(16) 0.0321(18) 0.0211(16) 0.0033(13) 0.0002(13) 0.0158(15) C2 0.0182(15) 0.0290(17) 0.0201(15) 0.0057(12) 0.0045(12) 0.0125(13) C3 0.0259(16) 0.0320(18) 0.0229(16) 0.0055(13) 0.0056(13) 0.0172(15) C4 0.037(2) 0.043(2) 0.035(2) 0.0013(17) -0.0059(16) 0.0231(19) C5 0.045(2) 0.064(3) 0.036(2) 0.011(2) -0.0041(18) 0.038(2) C6 0.066(3) 0.060(3) 0.044(3) 0.017(2) 0.000(2) 0.045(3) C7 0.084(4) 0.039(3) 0.071(4) 0.004(2) -0.023(3) 0.036(3) C8 0.062(3) 0.037(2) 0.044(2) -0.0006(18) -0.016(2) 0.029(2) C9 0.0255(17) 0.0239(16) 0.0301(18) 0.0050(14) 0.0074(14) 0.0115(14) C10 0.0299(18) 0.0309(19) 0.036(2) 0.0009(15) 0.0068(15) 0.0163(16) C11 0.038(2) 0.0285(19) 0.056(3) 0.0048(18) 0.0179(19) 0.0184(17) C12 0.058(3) 0.034(2) 0.038(2) -0.0008(17) 0.017(2) 0.021(2) C13 0.064(3) 0.050(3) 0.034(2) -0.0105(19) -0.002(2) 0.029(2) C14 0.045(2) 0.052(3) 0.034(2) -0.0089(19) -0.0030(18) 0.028(2) C15 0.0239(16) 0.0249(16) 0.0221(16) 0.0021(13) 0.0018(12) 0.0093(14) C16 0.034(2) 0.035(2) 0.039(2) 0.0085(16) 0.0114(16) 0.0198(17) C17 0.050(3) 0.031(2) 0.046(2) 0.0097(17) 0.0093(19) 0.0217(19) C18 0.034(2) 0.0284(19) 0.034(2) 0.0043(15) 0.0046(16) 0.0062(16) C19 0.0181(16) 0.038(2) 0.0317(19) 0.0025(16) 0.0004(14) 0.0061(15) C20 0.0233(17) 0.0339(19) 0.0297(18) 0.0040(15) 0.0011(14) 0.0134(15) C21 0.0213(17) 0.042(2) 0.036(2) -0.0112(17) -0.0025(15) 0.0107(16) C22 0.0270(18) 0.041(2) 0.034(2) -0.0074(16) -0.0117(15) 0.0145(17) C23 0.0285(18) 0.0355(19) 0.0175(16) -0.0005(14) -0.0035(13) 0.0083(15) C24 0.0244(17) 0.0340(19) 0.0230(16) -0.0050(14) -0.0031(13) 0.0125(15) C25 0.0300(18) 0.0272(18) 0.0234(17) -0.0013(14) 0.0017(14) 0.0050(15) C26 0.0186(19) 0.087(4) 0.061(3) -0.039(3) -0.0019(19) 0.011(2) C27 0.067(3) 0.064(3) 0.057(3) -0.019(3) -0.041(3) 0.042(3) C29 0.045(2) 0.058(3) 0.047(3) -0.017(2) -0.012(2) 0.035(2) C28 0.039(2) 0.058(3) 0.0230(19) 0.0007(18) 0.0015(16) 0.008(2) C30 0.064(3) 0.033(2) 0.033(2) 0.0041(17) 0.007(2) 0.008(2) _refine_ls_extinction_method '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 Ta1 . Cl1 . 2.4209(8) yes Ta1 . Cl2 . 2.3873(9) yes Ta1 . Cl3 . 2.3934(8) yes Ta1 . O1 . 2.024(2) yes Ta1 . P1 . 2.6596(9) yes Ta1 . C21 . 2.488(4) yes Ta1 . C24 . 2.437(4) yes Ta1 . C25 . 2.437(4) yes O1 . C2 . 1.342(4) yes P1 . C1 . 1.773(4) yes P1 . C9 . 1.831(4) yes P1 . C15 . 1.818(3) yes C1 . C2 . 1.349(5) yes C1 . H11 . 1.000 no C2 . C3 . 1.493(5) yes C3 . C4 . 1.388(5) yes C3 . C8 . 1.391(6) yes C4 . C5 . 1.386(6) yes C4 . H41 . 1.000 no C5 . C6 . 1.368(8) yes C5 . H51 . 1.000 no C6 . C7 . 1.382(8) yes C6 . H61 . 1.000 no C7 . C8 . 1.393(6) yes C7 . H71 . 1.000 no C8 . H81 . 1.000 no C9 . C10 . 1.395(5) yes C9 . C14 . 1.396(6) yes C10 . C11 . 1.392(6) yes C10 . H101 . 1.000 no C11 . C12 . 1.386(7) yes C11 . H111 . 1.000 no C12 . C13 . 1.388(7) yes C12 . H121 . 1.000 no C13 . C14 . 1.388(6) yes C13 . H131 . 1.000 no C14 . H141 . 1.000 no C15 . C16 . 1.393(5) yes C15 . C20 . 1.389(5) yes C16 . C17 . 1.390(6) yes C16 . H161 . 1.000 no C17 . C18 . 1.389(6) yes C17 . H171 . 1.000 no C18 . C19 . 1.386(6) yes C18 . H181 . 1.000 no C19 . C20 . 1.390(5) yes C19 . H191 . 1.000 no C20 . H201 . 1.000 no C21 . C22 . 1.415(6) yes C21 . C25 . 1.414(6) yes C21 . C26 . 1.499(6) yes C22 . C23 . 1.412(6) yes C22 . C27 . 1.500(6) yes C23 . C24 . 1.412(5) yes C23 . C28 . 1.494(5) yes C24 . C25 . 1.428(5) yes C24 . C29 . 1.497(6) yes C25 . C30 . 1.503(6) yes C26 . H261 . 1.000 no C26 . H262 . 1.000 no C26 . H263 . 1.000 no C27 . H271 . 1.000 no C27 . H272 . 1.000 no C27 . H273 . 1.000 no C29 . H291 . 1.000 no C29 . H292 . 1.000 no C29 . H293 . 1.000 no C28 . H281 . 1.000 no C28 . H282 . 1.000 no C28 . H283 . 1.000 no C30 . H301 . 1.000 no C30 . H302 . 1.000 no C30 . H303 . 1.000 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 Cl1 . Ta1 . Cl2 . 89.49(3) yes Cl1 . Ta1 . Cl3 . 150.95(3) yes Cl2 . Ta1 . Cl3 . 90.31(3) yes Cl1 . Ta1 . O1 . 82.04(7) yes Cl2 . Ta1 . O1 . 152.12(7) yes Cl3 . Ta1 . O1 . 84.70(7) yes Cl1 . Ta1 . P1 . 76.19(3) yes Cl2 . Ta1 . P1 . 77.37(3) yes Cl3 . Ta1 . P1 . 75.43(3) yes O1 . Ta1 . P1 . 74.83(7) yes Cl1 . Ta1 . C21 . 78.63(9) yes Cl2 . Ta1 . C21 . 91.07(11) yes Cl3 . Ta1 . C21 . 130.42(9) yes O1 . Ta1 . C21 . 112.95(13) yes P1 . Ta1 . C21 . 152.28(9) yes Cl1 . Ta1 . C24 . 115.61(9) yes Cl2 . Ta1 . C24 . 128.75(9) yes Cl3 . Ta1 . C24 . 86.60(9) yes O1 . Ta1 . C24 . 78.40(11) yes P1 . Ta1 . C24 . 148.85(9) yes Cl1 . Ta1 . C25 . 82.65(9) yes Cl2 . Ta1 . C25 . 124.4(1) yes Cl3 . Ta1 . C25 . 120.58(9) yes O1 . Ta1 . C25 . 80.99(12) yes P1 . Ta1 . C25 . 149.68(9) yes C21 . Ta1 . C24 . 55.44(13) yes C21 . Ta1 . C25 . 33.35(14) yes C24 . Ta1 . C25 . 34.06(12) yes Ta1 . O1 . C2 . 129.2(2) yes Ta1 . P1 . C1 . 97.19(12) yes Ta1 . P1 . C9 . 124.24(12) yes C1 . P1 . C9 . 106.72(17) yes Ta1 . P1 . C15 . 119.18(11) yes C1 . P1 . C15 . 108.01(17) yes C9 . P1 . C15 . 100.25(16) yes P1 . C1 . C2 . 116.0(3) yes P1 . C1 . H11 . 121.987 no C2 . C1 . H11 . 121.986 no O1 . C2 . C1 . 122.6(3) yes O1 . C2 . C3 . 114.6(3) yes C1 . C2 . C3 . 122.8(3) yes C2 . C3 . C4 . 121.9(3) yes C2 . C3 . C8 . 120.0(3) yes C4 . C3 . C8 . 118.1(4) yes C3 . C4 . C5 . 121.4(4) yes C3 . C4 . H41 . 119.324 no C5 . C4 . H41 . 119.324 no C4 . C5 . C6 . 120.0(4) yes C4 . C5 . H51 . 119.978 no C6 . C5 . H51 . 119.979 no C5 . C6 . C7 . 119.8(4) yes C5 . C6 . H61 . 120.075 no C7 . C6 . H61 . 120.076 no C6 . C7 . C8 . 120.3(5) yes C6 . C7 . H71 . 119.871 no C8 . C7 . H71 . 119.871 no C3 . C8 . C7 . 120.4(4) yes C3 . C8 . H81 . 119.789 no C7 . C8 . H81 . 119.790 no P1 . C9 . C10 . 123.3(3) yes P1 . C9 . C14 . 117.7(3) yes C10 . C9 . C14 . 119.0(4) yes C9 . C10 . C11 . 119.7(4) yes C9 . C10 . H101 . 120.169 no C11 . C10 . H101 . 120.169 no C10 . C11 . C12 . 120.9(4) yes C10 . C11 . H111 . 119.525 no C12 . C11 . H111 . 119.525 no C11 . C12 . C13 . 119.7(4) yes C11 . C12 . H121 . 120.156 no C13 . C12 . H121 . 120.156 no C12 . C13 . C14 . 119.6(4) yes C12 . C13 . H131 . 120.208 no C14 . C13 . H131 . 120.209 no C9 . C14 . C13 . 121.1(4) yes C9 . C14 . H141 . 119.433 no C13 . C14 . H141 . 119.432 no P1 . C15 . C16 . 118.6(3) yes P1 . C15 . C20 . 122.0(3) yes C16 . C15 . C20 . 119.4(3) yes C15 . C16 . C17 . 120.3(4) yes C15 . C16 . H161 . 119.847 no C17 . C16 . H161 . 119.848 no C16 . C17 . C18 . 120.0(4) yes C16 . C17 . H171 . 120.017 no C18 . C17 . H171 . 120.017 no C17 . C18 . C19 . 119.9(4) yes C17 . C18 . H181 . 120.038 no C19 . C18 . H181 . 120.037 no C18 . C19 . C20 . 120.1(4) yes C18 . C19 . H191 . 119.964 no C20 . C19 . H191 . 119.964 no C15 . C20 . C19 . 120.4(4) yes C15 . C20 . H201 . 119.819 no C19 . C20 . H201 . 119.819 no Ta1 . C21 . C22 . 75.6(2) yes Ta1 . C21 . C25 . 71.4(2) yes C22 . C21 . C25 . 108.5(3) yes Ta1 . C21 . C26 . 124.9(3) yes C22 . C21 . C26 . 124.2(4) yes C25 . C21 . C26 . 126.9(5) yes C21 . C22 . C23 . 107.8(4) yes C21 . C22 . C27 . 126.8(4) yes C23 . C22 . C27 . 125.0(4) yes C22 . C23 . C24 . 108.5(3) yes C22 . C23 . C28 . 125.4(4) yes C24 . C23 . C28 . 125.5(4) yes Ta1 . C24 . C23 . 75.8(2) yes Ta1 . C24 . C25 . 73.0(2) yes C23 . C24 . C25 . 107.8(3) yes Ta1 . C24 . C29 . 121.5(3) yes C23 . C24 . C29 . 125.3(4) yes C25 . C24 . C29 . 126.7(4) yes Ta1 . C25 . C21 . 75.3(2) yes Ta1 . C25 . C24 . 72.9(2) yes C21 . C25 . C24 . 107.5(3) yes Ta1 . C25 . C30 . 122.2(3) yes C21 . C25 . C30 . 126.2(4) yes C24 . C25 . C30 . 126.1(4) yes C21 . C26 . H261 . 109.467 no C21 . C26 . H262 . 109.468 no H261 . C26 . H262 . 109.475 no C21 . C26 . H263 . 109.467 no H261 . C26 . H263 . 109.475 no H262 . C26 . H263 . 109.476 no C22 . C27 . H271 . 109.467 no C22 . C27 . H272 . 109.466 no H271 . C27 . H272 . 109.476 no C22 . C27 . H273 . 109.466 no H271 . C27 . H273 . 109.476 no H272 . C27 . H273 . 109.476 no C24 . C29 . H291 . 109.467 no C24 . C29 . H292 . 109.467 no H291 . C29 . H292 . 109.475 no C24 . C29 . H293 . 109.467 no H291 . C29 . H293 . 109.476 no H292 . C29 . H293 . 109.476 no C23 . C28 . H281 . 109.468 no C23 . C28 . H282 . 109.466 no H281 . C28 . H282 . 109.480 no C23 . C28 . H283 . 109.464 no H281 . C28 . H283 . 109.476 no H282 . C28 . H283 . 109.474 no C25 . C30 . H301 . 109.468 no C25 . C30 . H302 . 109.466 no H301 . C30 . H302 . 109.477 no C25 . C30 . H303 . 109.465 no H301 . C30 . H303 . 109.477 no H302 . C30 . H303 . 109.474 no data_cristal _database_code_CSD 190865 _audit_creation_date 02-14-01 _audit_creation_method CRYSTALS_ver_12-03-99 _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 8.4611(1) _cell_angle_alpha 92.6314(8) _cell_length_b 16.6441(3) _cell_angle_beta 99.3326(9) _cell_length_c 16.8443(3) _cell_angle_gamma 94.1166(11) _cell_volume 2330.7 _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' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'Ta ' -1.2580 6.5230 29.2024 1.7733 15.2293 9.3705 14.5135 0.2960 4.7649 63.3644 9.2435 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C50 H42 Cl6 O2 P2 Ta2 ' _chemical_formula_moiety ' C50 H42 Cl6 O2 P2 Ta2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1311.44 _cell_measurement_reflns_used 9682 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_max 0.16 _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1269.198 _exptl_absorpt_coefficient_mu 5.145 # Sheldrick geometric definitions 0.66 0.73 _diffrn_measurement_device_type ; Enraf Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.73 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 19271 _reflns_number_total 10582 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 10582 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 10729 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_gt 8244 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min -21 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _refine_diff_density_min -1.53 _refine_diff_density_max 1.39 _reflns_threshold_expression >2.00\s(I) _refine_ls_number_reflns 8244 _refine_ls_number_parameters 560 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0366 _refine_ls_goodness_of_fit_ref 1.0798 _refine_ls_shift/su_max 0.003071 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 0.754 0.396 0.575 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type TA1 TA 0.479172(19) 0.338151(9) 1.377072(9) 0.0186 1.0000 Uani TA101 TA 0.558154(18) 0.084692(9) 0.734416(9) 0.0183 1.0000 Uani CL1 CL 0.70807(13) 0.43449(7) 1.41949(6) 0.0288 1.0000 Uani CL2 CL 0.34013(14) 0.44499(7) 1.31157(7) 0.0309 1.0000 Uani CL3 CL 0.31514(13) 0.24553(6) 1.27645(6) 0.0268 1.0000 Uani CL101 CL 0.50870(13) 0.12546(7) 0.86676(6) 0.0285 1.0000 Uani CL102 CL 0.42868(13) 0.20118(7) 0.68668(7) 0.0282 1.0000 Uani CL103 CL 0.70683(14) 0.09482(7) 0.62408(6) 0.0286 1.0000 Uani O1 O 0.6389(4) 0.25609(17) 1.38608(17) 0.0221 1.0000 Uani O101 O 0.7416(4) 0.03135(17) 0.79205(18) 0.0232 1.0000 Uani P1 P 0.62120(13) 0.34927(6) 1.24711(6) 0.0197 1.0000 Uani P101 P 0.78870(12) 0.20280(6) 0.78502(6) 0.0192 1.0000 Uani C1 C 0.7570(5) 0.2735(3) 1.2699(3) 0.0266 1.0000 Uani C2 C 0.7492(5) 0.2380(2) 1.3399(2) 0.0200 1.0000 Uani C3 C 0.8640(5) 0.1800(2) 1.3745(2) 0.0205 1.0000 Uani C4 C 0.8828(5) 0.1679(3) 1.4573(3) 0.0251 1.0000 Uani C5 C 0.9935(6) 0.1163(3) 1.4900(3) 0.0295 1.0000 Uani C6 C 1.0836(5) 0.0754(3) 1.4418(3) 0.0282 1.0000 Uani C7 C 1.0629(5) 0.0865(3) 1.3592(3) 0.0261 1.0000 Uani C8 C 0.9542(5) 0.1388(3) 1.3262(2) 0.0237 1.0000 Uani C9 C 0.5041(5) 0.3214(3) 1.1478(2) 0.0228 1.0000 Uani C10 C 0.5109(6) 0.2446(3) 1.1119(3) 0.0333 1.0000 Uani C11 C 0.4203(7) 0.2232(3) 1.0366(3) 0.0414 1.0000 Uani C12 C 0.3251(6) 0.2780(4) 0.9967(3) 0.0437 1.0000 Uani C13 C 0.3158(7) 0.3533(4) 1.0323(3) 0.0410 1.0000 Uani C14 C 0.4042(6) 0.3756(3) 1.1079(3) 0.0320 1.0000 Uani C15 C 0.7418(5) 0.4383(3) 1.2260(2) 0.0249 1.0000 Uani C16 C 0.8936(6) 0.4317(3) 1.2044(3) 0.0347 1.0000 Uani C17 C 0.9758(7) 0.4969(4) 1.1785(3) 0.0434 1.0000 Uani C18 C 0.9093(7) 0.5707(3) 1.1734(3) 0.0433 1.0000 Uani C19 C 0.7626(7) 0.5791(3) 1.1971(4) 0.0453 1.0000 Uani C20 C 0.6790(6) 0.5134(3) 1.2234(3) 0.0380 1.0000 Uani C21 C 0.4985(7) 0.2998(3) 1.5149(3) 0.0346 1.0000 Uani C22 C 0.4487(6) 0.3781(3) 1.5165(3) 0.0299 1.0000 Uani C23 C 0.2964(6) 0.3791(3) 1.4703(3) 0.0357 1.0000 Uani C24 C 0.2494(6) 0.2984(4) 1.4404(3) 0.0396 1.0000 Uani C25 C 0.3739(7) 0.2501(3) 1.4678(3) 0.0351 1.0000 Uani C101 C 0.9397(5) 0.1398(2) 0.8276(2) 0.0216 1.0000 Uani C102 C 0.8885(5) 0.0618(3) 0.8296(2) 0.0203 1.0000 Uani C103 C 0.9870(5) -0.0001(2) 0.8716(2) 0.0221 1.0000 Uani C104 C 1.1295(5) 0.0225(3) 0.9224(3) 0.0282 1.0000 Uani C105 C 1.2189(6) -0.0349(3) 0.9617(3) 0.0358 1.0000 Uani C106 C 1.1649(6) -0.1146(3) 0.9510(3) 0.0344 1.0000 Uani C107 C 1.0203(6) -0.1379(3) 0.9020(3) 0.0341 1.0000 Uani C108 C 0.9327(6) -0.0806(2) 0.8625(3) 0.0269 1.0000 Uani C109 C 0.8728(5) 0.2648(2) 0.7135(2) 0.0202 1.0000 Uani C110 C 1.0109(6) 0.2448(3) 0.6846(3) 0.0310 1.0000 Uani C111 C 1.0741(6) 0.2931(3) 0.6304(3) 0.0326 1.0000 Uani C112 C 1.0019(6) 0.3619(3) 0.6053(3) 0.0303 1.0000 Uani C113 C 0.8657(5) 0.3814(3) 0.6337(3) 0.0270 1.0000 Uani C114 C 0.8009(5) 0.3340(3) 0.6871(3) 0.0261 1.0000 Uani C115 C 0.7677(5) 0.2763(2) 0.8660(2) 0.0211 1.0000 Uani C116 C 0.8784(5) 0.2842(3) 0.9372(3) 0.0263 1.0000 Uani C117 C 0.8676(6) 0.3433(3) 0.9977(3) 0.0322 1.0000 Uani C118 C 0.7425(6) 0.3936(3) 0.9879(3) 0.0316 1.0000 Uani C119 C 0.6301(6) 0.3855(3) 0.9180(3) 0.0322 1.0000 Uani C120 C 0.6414(6) 0.3267(3) 0.8574(3) 0.0277 1.0000 Uani C121 C 0.4040(8) -0.0347(4) 0.7619(4) 0.0604 1.0000 Uani C122 C 0.4850(7) -0.0587(3) 0.6999(4) 0.0584 1.0000 Uani C123 C 0.4197(7) -0.0196(3) 0.6322(3) 0.0502 1.0000 Uani C124 C 0.3039(7) 0.0262(3) 0.6531(3) 0.0496 1.0000 Uani C125 C 0.2919(7) 0.0177(4) 0.7331(4) 0.0542 1.0000 Uani H11 H 0.8337 0.2583 1.2335 0.0326 1.0000 Uiso H41 H 0.8168 0.1963 1.4922 0.0307 1.0000 Uiso H51 H 1.0089 0.1083 1.5491 0.0354 1.0000 Uiso H61 H 1.1631 0.0381 1.4662 0.0336 1.0000 Uiso H71 H 1.1265 0.0567 1.3240 0.0313 1.0000 Uiso H81 H 0.9401 0.1472 1.2672 0.0285 1.0000 Uiso H101 H 0.5808 0.2052 1.1403 0.0398 1.0000 Uiso H111 H 0.4237 0.1680 1.0111 0.0490 1.0000 Uiso H121 H 0.2628 0.2629 0.9417 0.0511 1.0000 Uiso H131 H 0.2451 0.3922 1.0035 0.0487 1.0000 Uiso H141 H 0.3966 0.4301 1.1338 0.0392 1.0000 Uiso H161 H 0.9428 0.3788 1.2078 0.0409 1.0000 Uiso H171 H 1.0840 0.4912 1.1633 0.0511 1.0000 Uiso H181 H 0.9676 0.6175 1.1527 0.0484 1.0000 Uiso H191 H 0.7161 0.6327 1.1953 0.0515 1.0000 Uiso H201 H 0.5728 0.5200 1.2407 0.0452 1.0000 Uiso H211 H 0.6035 0.2824 1.5422 0.0434 1.0000 Uiso H221 H 0.5128 0.4262 1.5464 0.0363 1.0000 Uiso H231 H 0.2330 0.4272 1.4602 0.0446 1.0000 Uiso H241 H 0.1450 0.2791 1.4056 0.0480 1.0000 Uiso H251 H 0.3739 0.1906 1.4560 0.0439 1.0000 Uiso H1011 H 1.0532 0.1611 0.8482 0.0253 1.0000 Uiso H1041 H 1.1688 0.0809 0.9310 0.0341 1.0000 Uiso H1051 H 1.3228 -0.0179 0.9979 0.0435 1.0000 Uiso H1061 H 1.2303 -0.1561 0.9786 0.0433 1.0000 Uiso H1071 H 0.9791 -0.1961 0.8952 0.0415 1.0000 Uiso H1081 H 0.8282 -0.0976 0.8268 0.0322 1.0000 Uiso H1101 H 1.0645 0.1957 0.7029 0.0389 1.0000 Uiso H1111 H 1.1724 0.2780 0.6092 0.0408 1.0000 Uiso H1121 H 1.0489 0.3970 0.5670 0.0378 1.0000 Uiso H1131 H 0.8127 0.4307 0.6153 0.0327 1.0000 Uiso H1141 H 0.7015 0.3492 0.7072 0.0321 1.0000 Uiso H1161 H 0.9669 0.2471 0.9454 0.0314 1.0000 Uiso H1171 H 0.9499 0.3493 1.0478 0.0375 1.0000 Uiso H1181 H 0.7338 0.4354 1.0312 0.0382 1.0000 Uiso H1191 H 0.5404 0.4219 0.9106 0.0400 1.0000 Uiso H1201 H 0.5584 0.3206 0.8075 0.0331 1.0000 Uiso H1211 H 0.4242 -0.0526 0.8182 0.0666 1.0000 Uiso H1221 H 0.5723 -0.0965 0.7034 0.0647 1.0000 Uiso H1231 H 0.4522 -0.0243 0.5778 0.0581 1.0000 Uiso H1241 H 0.2376 0.0607 0.6161 0.0544 1.0000 Uiso H1251 H 0.2167 0.0443 0.7641 0.0640 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 Ta1 0.0211(1) 0.01791(9) 0.01738(9) 0.00053(6) 0.00545(6) 0.00048(6) Ta101 0.01771(9) 0.01955(9) 0.01745(9) 0.00257(6) 0.00179(6) 0.00131(6) Cl1 0.0307(5) 0.0296(5) 0.0246(5) -0.0008(4) 0.0046(4) -0.0068(4) Cl2 0.0326(6) 0.0280(5) 0.0355(6) 0.0068(4) 0.0104(4) 0.0113(4) Cl3 0.0284(5) 0.0270(5) 0.0240(5) -0.0011(4) 0.0058(4) -0.0062(4) Cl101 0.0311(5) 0.0326(5) 0.0222(5) 0.0007(4) 0.0092(4) -0.0045(4) Cl102 0.0257(5) 0.0275(5) 0.0313(5) 0.0072(4) 0.0006(4) 0.0071(4) Cl103 0.0312(5) 0.0305(5) 0.0259(5) -0.0004(4) 0.0115(4) 0.0002(4) O1 0.0250(15) 0.0221(14) 0.0210(14) 0.0063(11) 0.0073(11) 0.0026(11) O101 0.0225(14) 0.0187(14) 0.0266(14) 0.0038(11) -0.0016(11) -0.0004(11) P1 0.0218(5) 0.0192(5) 0.0189(5) 0.0041(4) 0.0045(4) 0.0020(4) P101 0.0189(5) 0.0189(5) 0.0204(5) 0.0046(4) 0.0036(4) 0.0029(4) C1 0.029(2) 0.029(2) 0.024(2) 0.0065(17) 0.0081(17) 0.0029(17) C2 0.0188(18) 0.0190(18) 0.0220(18) 0.0006(14) 0.0030(14) 0.0006(14) C3 0.0189(18) 0.0168(18) 0.0254(19) 0.0026(15) 0.0043(15) -0.0024(14) C4 0.030(2) 0.023(2) 0.023(2) 0.0001(16) 0.0089(17) 0.0034(17) C5 0.034(2) 0.032(2) 0.022(2) 0.0060(17) 0.0012(17) 0.0073(19) C6 0.026(2) 0.024(2) 0.034(2) 0.0084(18) 0.0015(18) 0.0028(17) C7 0.026(2) 0.024(2) 0.029(2) 0.0038(17) 0.0032(17) 0.0034(16) C8 0.023(2) 0.028(2) 0.0198(18) 0.0086(16) 0.0036(15) -0.0021(16) C9 0.026(2) 0.024(2) 0.0189(18) 0.0025(15) 0.0048(15) -0.0051(16) C10 0.044(3) 0.030(2) 0.025(2) -0.0032(18) 0.010(2) -0.005(2) C11 0.045(3) 0.042(3) 0.035(3) -0.011(2) 0.009(2) -0.006(2) C12 0.028(3) 0.072(4) 0.027(2) -0.009(2) 0.005(2) -0.013(3) C13 0.035(3) 0.057(3) 0.030(2) 0.011(2) 0.001(2) 0.001(2) C14 0.038(3) 0.033(2) 0.027(2) 0.0110(18) 0.0063(19) 0.008(2) C15 0.027(2) 0.026(2) 0.0199(19) 0.0085(16) -0.0007(16) -0.0069(16) C16 0.033(3) 0.042(3) 0.027(2) 0.001(2) 0.0054(19) -0.009(2) C17 0.041(3) 0.047(3) 0.039(3) -0.003(2) 0.011(2) -0.021(2) C18 0.050(3) 0.044(3) 0.027(2) 0.012(2) -0.010(2) -0.026(3) C19 0.042(3) 0.032(3) 0.055(3) 0.018(2) -0.012(3) -0.009(2) C20 0.034(3) 0.036(3) 0.043(3) 0.013(2) 0.003(2) -0.003(2) C21 0.045(3) 0.038(3) 0.026(2) 0.0109(19) 0.016(2) 0.007(2) C22 0.035(2) 0.033(2) 0.023(2) -0.0048(17) 0.0137(18) -0.0066(19) C23 0.033(3) 0.047(3) 0.031(2) 0.002(2) 0.017(2) 0.007(2) C24 0.035(3) 0.054(3) 0.032(2) -0.006(2) 0.021(2) -0.017(2) C25 0.047(3) 0.036(3) 0.027(2) 0.0040(19) 0.021(2) 0.000(2) C101 0.0162(18) 0.024(2) 0.0227(19) 0.0022(15) -0.0032(15) 0.0047(15) C102 0.0178(18) 0.027(2) 0.0172(17) 0.0032(15) 0.0027(14) 0.0053(15) C103 0.028(2) 0.0261(19) 0.0141(16) 0.0044(14) 0.0077(15) 0.0067(16) C104 0.026(2) 0.032(2) 0.028(2) 0.0124(17) 0.0026(16) 0.0031(17) C105 0.026(2) 0.046(3) 0.037(2) 0.019(2) 0.0028(19) 0.0087(19) C106 0.036(2) 0.042(2) 0.030(2) 0.0154(19) 0.0114(18) 0.015(2) C107 0.047(3) 0.028(2) 0.029(2) 0.0038(18) 0.0075(19) 0.0088(19) C108 0.033(2) 0.025(2) 0.0224(19) 0.0027(16) 0.0020(16) 0.0063(17) C109 0.024(2) 0.0174(18) 0.0188(18) 0.0025(14) 0.0028(15) 0.0000(15) C110 0.031(2) 0.031(2) 0.036(2) 0.0110(19) 0.0143(19) 0.0062(18) C111 0.029(2) 0.040(3) 0.032(2) 0.009(2) 0.0110(19) 0.013(2) C112 0.036(3) 0.033(2) 0.025(2) 0.0104(18) 0.0125(18) 0.0058(19) C113 0.031(2) 0.025(2) 0.026(2) 0.0106(17) 0.0024(17) 0.0072(17) C114 0.023(2) 0.028(2) 0.029(2) 0.0032(17) 0.0069(17) 0.0081(17) C115 0.0231(19) 0.0208(19) 0.0201(18) 0.0000(15) 0.0061(15) 0.0015(15) C116 0.028(2) 0.030(2) 0.0200(19) 0.0035(16) 0.0034(16) 0.0004(17) C117 0.031(2) 0.041(3) 0.021(2) -0.0015(18) 0.0019(18) -0.009(2) C118 0.034(3) 0.033(2) 0.028(2) 0.0012(18) 0.0077(19) 0.0023(19) C119 0.037(3) 0.029(2) 0.033(2) 0.0029(19) 0.012(2) 0.0099(19) C120 0.032(2) 0.027(2) 0.023(2) 0.0020(17) 0.0013(17) 0.0075(18) C121 0.071(4) 0.047(3) 0.049(3) 0.013(2) -0.016(3) -0.043(3) C122 0.032(3) 0.028(3) 0.102(4) -0.016(3) -0.019(3) -0.007(2) C123 0.048(3) 0.052(3) 0.045(3) -0.020(2) 0.012(2) -0.028(2) C124 0.040(3) 0.041(3) 0.055(3) 0.000(2) -0.023(2) -0.012(2) C125 0.034(3) 0.063(3) 0.063(3) -0.023(3) 0.017(2) -0.017(2) _refine_ls_extinction_coef 33.7(71) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' 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 Ta1 . Cl1 . 2.415(1) yes Ta1 . Cl2 . 2.4131(11) yes Ta1 . Cl3 . 2.422(1) yes Ta1 . O1 . 1.983(3) yes Ta1 . P1 . 2.670(1) yes Ta1 . C21 . 2.419(5) yes Ta1 . C22 . 2.470(4) yes Ta1 . C23 . 2.482(5) yes Ta1 . C24 . 2.431(4) yes Ta1 . C25 . 2.396(5) yes Ta101 . Cl101 . 2.410(1) yes Ta101 . Cl102 . 2.402(1) yes Ta101 . Cl103 . 2.413(1) yes Ta101 . O101 . 1.982(3) yes Ta101 . P101 . 2.674(1) yes Ta101 . C121 . 2.402(5) yes Ta101 . C122 . 2.442(5) yes Ta101 . C123 . 2.476(5) yes Ta101 . C124 . 2.464(5) yes Ta101 . C125 . 2.437(6) yes O1 . C2 . 1.349(5) yes O101 . C102 . 1.352(5) yes P1 . C1 . 1.779(5) yes P1 . C9 . 1.822(4) yes P1 . C15 . 1.819(4) yes P101 . C101 . 1.792(4) yes P101 . C109 . 1.820(4) yes P101 . C115 . 1.829(4) yes C1 . C2 . 1.352(6) yes C1 . H11 . 1.000 no C2 . C3 . 1.489(5) yes C3 . C4 . 1.402(6) yes C3 . C8 . 1.393(6) yes C4 . C5 . 1.382(6) yes C4 . H41 . 1.000 no C5 . C6 . 1.389(7) yes C5 . H51 . 1.000 no C6 . C7 . 1.397(6) yes C6 . H61 . 1.000 no C7 . C8 . 1.381(6) yes C7 . H71 . 1.000 no C8 . H81 . 1.000 no C9 . C10 . 1.398(6) yes C9 . C14 . 1.400(6) yes C10 . C11 . 1.389(7) yes C10 . H101 . 1.000 no C11 . C12 . 1.385(9) yes C11 . H111 . 1.000 no C12 . C13 . 1.377(9) yes C12 . H121 . 1.000 no C13 . C14 . 1.388(7) yes C13 . H131 . 1.000 no C14 . H141 . 1.000 no C15 . C16 . 1.402(7) yes C15 . C20 . 1.392(7) yes C16 . C17 . 1.372(7) yes C16 . H161 . 1.000 no C17 . C18 . 1.388(9) yes C17 . H171 . 1.000 no C18 . C19 . 1.378(9) yes C18 . H181 . 1.000 no C19 . C20 . 1.389(7) yes C19 . H191 . 1.000 no C20 . H201 . 1.000 no C21 . C22 . 1.399(7) yes C21 . C25 . 1.403(8) yes C21 . H211 . 1.000 no C22 . C23 . 1.395(7) yes C22 . H221 . 1.000 no C23 . C24 . 1.419(8) yes C23 . H231 . 1.000 no C24 . C25 . 1.403(8) yes C24 . H241 . 1.000 no C25 . H251 . 1.000 no C101 . C102 . 1.342(6) yes C101 . H1011 . 1.000 no C102 . C103 . 1.501(5) yes C103 . C104 . 1.378(5) yes C103 . C108 . 1.378(5) yes C104 . C105 . 1.386(5) yes C104 . H1041 . 1.000 no C105 . C106 . 1.366(6) yes C105 . H1051 . 1.000 no C106 . C107 . 1.380(6) yes C106 . H1061 . 1.000 no C107 . C108 . 1.380(5) yes C107 . H1071 . 1.000 no C108 . H1081 . 1.000 no C109 . C110 . 1.392(6) yes C109 . C114 . 1.398(6) yes C110 . C111 . 1.389(6) yes C110 . H1101 . 1.000 no C111 . C112 . 1.388(7) yes C111 . H1111 . 1.000 no C112 . C113 . 1.371(7) yes C112 . H1121 . 1.000 no C113 . C114 . 1.377(6) yes C113 . H1131 . 1.000 no C114 . H1141 . 1.000 no C115 . C116 . 1.392(6) yes C115 . C120 . 1.398(6) yes C116 . C117 . 1.402(7) yes C116 . H1161 . 1.000 no C117 . C118 . 1.390(7) yes C117 . H1171 . 1.000 no C118 . C119 . 1.384(7) yes C118 . H1181 . 1.000 no C119 . C120 . 1.402(6) yes C119 . H1191 . 1.000 no C120 . H1201 . 1.000 no C121 . C122 . 1.398(7) yes C121 . C125 . 1.380(7) yes C121 . H1211 . 1.000 no C122 . C123 . 1.394(7) yes C122 . H1221 . 1.000 no C123 . C124 . 1.364(7) yes C123 . H1231 . 1.000 no C124 . C125 . 1.380(7) yes C124 . H1241 . 1.000 no C125 . H1251 . 1.000 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 Cl1 . Ta1 . Cl2 . 88.25(4) yes Cl1 . Ta1 . Cl3 . 151.26(4) yes Cl2 . Ta1 . Cl3 . 87.08(4) yes Cl1 . Ta1 . O1 . 85.21(9) yes Cl2 . Ta1 . O1 . 153.56(8) yes Cl3 . Ta1 . O1 . 86.47(9) yes Cl1 . Ta1 . P1 . 75.64(3) yes Cl2 . Ta1 . P1 . 79.46(3) yes Cl3 . Ta1 . P1 . 75.62(3) yes O1 . Ta1 . P1 . 74.10(8) yes Cl1 . Ta1 . C21 . 88.79(13) yes Cl2 . Ta1 . C21 . 129.52(13) yes Cl3 . Ta1 . C21 . 115.70(13) yes O1 . Ta1 . C21 . 75.99(15) yes P1 . Ta1 . C21 . 147.19(13) yes Cl1 . Ta1 . C22 . 77.60(11) yes Cl2 . Ta1 . C22 . 97.44(12) yes Cl3 . Ta1 . C22 . 131.14(11) yes O1 . Ta1 . C22 . 106.07(15) yes P1 . Ta1 . C22 . 153.13(11) yes Cl1 . Ta1 . C23 . 101.04(13) yes Cl2 . Ta1 . C23 . 75.64(13) yes Cl3 . Ta1 . C23 . 105.21(13) yes O1 . Ta1 . C23 . 130.76(15) yes P1 . Ta1 . C23 . 154.99(13) yes Cl1 . Ta1 . C24 . 131.84(12) yes Cl2 . Ta1 . C24 . 91.36(15) yes Cl3 . Ta1 . C24 . 76.65(12) yes O1 . Ta1 . C24 . 111.96(17) yes P1 . Ta1 . C24 . 151.15(13) yes Cl1 . Ta1 . C25 . 122.61(13) yes Cl2 . Ta1 . C25 . 125.09(13) yes Cl3 . Ta1 . C25 . 82.54(13) yes O1 . Ta1 . C25 . 79.34(15) yes P1 . Ta1 . C25 . 146.34(12) yes C21 . Ta1 . C22 . 33.25(17) yes C21 . Ta1 . C23 . 55.63(17) yes C22 . Ta1 . C23 . 32.73(17) yes C21 . Ta1 . C24 . 55.81(19) yes C22 . Ta1 . C24 . 54.71(16) yes C23 . Ta1 . C24 . 33.57(18) yes C21 . Ta1 . C25 . 33.87(18) yes C22 . Ta1 . C25 . 55.24(16) yes C23 . Ta1 . C25 . 56.01(17) yes C24 . Ta1 . C25 . 33.79(19) yes Cl101 . Ta101 . Cl102 . 87.41(4) yes Cl101 . Ta101 . Cl103 . 152.35(4) yes Cl102 . Ta101 . Cl103 . 87.16(4) yes Cl101 . Ta101 . O101 . 85.50(9) yes Cl102 . Ta101 . O101 . 152.76(9) yes Cl103 . Ta101 . O101 . 87.04(9) yes Cl101 . Ta101 . P101 . 76.48(3) yes Cl102 . Ta101 . P101 . 78.55(3) yes Cl103 . Ta101 . P101 . 75.87(3) yes O101 . Ta101 . P101 . 74.23(8) yes Cl101 . Ta101 . C121 . 80.81(16) yes Cl102 . Ta101 . C121 . 121.01(17) yes Cl103 . Ta101 . C121 . 124.71(17) yes O101 . Ta101 . C121 . 83.69(18) yes P101 . Ta101 . C121 . 149.29(14) yes Cl101 . Ta101 . C122 . 112.50(18) yes Cl102 . Ta101 . C122 . 130.44(13) yes Cl103 . Ta101 . C122 . 91.40(17) yes O101 . Ta101 . C122 . 76.30(15) yes P101 . Ta101 . C122 . 148.34(13) yes Cl101 . Ta101 . C123 . 131.88(13) yes Cl102 . Ta101 . C123 . 100.09(15) yes Cl103 . Ta101 . C123 . 75.77(13) yes O101 . Ta101 . C123 . 104.20(17) yes P101 . Ta101 . C123 . 151.64(13) yes Cl101 . Ta101 . C124 . 108.76(15) yes Cl102 . Ta101 . C124 . 76.77(14) yes Cl103 . Ta101 . C124 . 96.31(15) yes O101 . Ta101 . C124 . 130.34(16) yes P101 . Ta101 . C124 . 154.45(14) yes Cl101 . Ta101 . C125 . 78.79(14) yes Cl102 . Ta101 . C125 . 87.91(16) yes Cl103 . Ta101 . C125 . 128.03(14) yes O101 . Ta101 . C125 . 116.29(18) yes P101 . Ta101 . C125 . 152.22(14) yes C121 . Ta101 . C122 . 33.52(18) yes C121 . Ta101 . C123 . 54.50(19) yes C122 . Ta101 . C123 . 32.93(17) yes C121 . Ta101 . C124 . 54.03(19) yes C122 . Ta101 . C124 . 54.14(18) yes C123 . Ta101 . C124 . 32.06(16) yes C121 . Ta101 . C125 . 33.13(18) yes C122 . Ta101 . C125 . 55.3(2) yes C123 . Ta101 . C125 . 54.39(18) yes C124 . Ta101 . C125 . 32.71(17) yes Ta1 . O1 . C2 . 131.6(2) yes Ta101 . O101 . C102 . 131.2(3) yes Ta1 . P1 . C1 . 97.28(14) yes Ta1 . P1 . C9 . 119.30(14) yes C1 . P1 . C9 . 107.3(2) yes Ta1 . P1 . C15 . 124.04(15) yes C1 . P1 . C15 . 106.3(2) yes C9 . P1 . C15 . 101.09(18) yes Ta101 . P101 . C101 . 96.97(14) yes Ta101 . P101 . C109 . 120.88(13) yes C101 . P101 . C109 . 107.92(19) yes Ta101 . P101 . C115 . 120.70(14) yes C101 . P101 . C115 . 105.84(19) yes C109 . P101 . C115 . 102.94(19) yes P1 . C1 . C2 . 115.3(3) yes P1 . C1 . H11 . 122.342 no C2 . C1 . H11 . 122.342 no O1 . C2 . C1 . 121.5(4) yes O1 . C2 . C3 . 114.6(3) yes C1 . C2 . C3 . 123.8(4) yes C2 . C3 . C4 . 119.2(4) yes C2 . C3 . C8 . 121.0(4) yes C4 . C3 . C8 . 119.8(4) yes C3 . C4 . C5 . 119.3(4) yes C3 . C4 . H41 . 120.359 no C5 . C4 . H41 . 120.360 no C4 . C5 . C6 . 120.9(4) yes C4 . C5 . H51 . 119.574 no C6 . C5 . H51 . 119.573 no C5 . C6 . C7 . 119.8(4) yes C5 . C6 . H61 . 120.088 no C7 . C6 . H61 . 120.088 no C6 . C7 . C8 . 119.7(4) yes C6 . C7 . H71 . 120.174 no C8 . C7 . H71 . 120.174 no C3 . C8 . C7 . 120.6(4) yes C3 . C8 . H81 . 119.711 no C7 . C8 . H81 . 119.711 no P1 . C9 . C10 . 119.8(3) yes P1 . C9 . C14 . 120.6(3) yes C10 . C9 . C14 . 119.6(4) yes C9 . C10 . C11 . 119.7(5) yes C9 . C10 . H101 . 120.152 no C11 . C10 . H101 . 120.152 no C10 . C11 . C12 . 120.2(5) yes C10 . C11 . H111 . 119.905 no C12 . C11 . H111 . 119.905 no C11 . C12 . C13 . 120.4(5) yes C11 . C12 . H121 . 119.796 no C13 . C12 . H121 . 119.796 no C12 . C13 . C14 . 120.3(5) yes C12 . C13 . H131 . 119.871 no C14 . C13 . H131 . 119.871 no C9 . C14 . C13 . 119.8(5) yes C9 . C14 . H141 . 120.101 no C13 . C14 . H141 . 120.101 no P1 . C15 . C16 . 120.8(4) yes P1 . C15 . C20 . 120.6(4) yes C16 . C15 . C20 . 118.3(4) yes C15 . C16 . C17 . 120.8(5) yes C15 . C16 . H161 . 119.577 no C17 . C16 . H161 . 119.577 no C16 . C17 . C18 . 120.3(5) yes C16 . C17 . H171 . 119.857 no C18 . C17 . H171 . 119.857 no C17 . C18 . C19 . 119.8(5) yes C17 . C18 . H181 . 120.118 no C19 . C18 . H181 . 120.118 no C18 . C19 . C20 . 120.2(5) yes C18 . C19 . H191 . 119.924 no C20 . C19 . H191 . 119.924 no C15 . C20 . C19 . 120.6(5) yes C15 . C20 . H201 . 119.697 no C19 . C20 . H201 . 119.697 no Ta1 . C21 . C22 . 75.4(3) yes Ta1 . C21 . C25 . 72.2(3) yes C22 . C21 . C25 . 107.3(5) yes Ta1 . C21 . H211 . 118.088 no C22 . C21 . H211 . 126.335 no C25 . C21 . H211 . 126.335 no Ta1 . C22 . C21 . 71.3(3) yes Ta1 . C22 . C23 . 74.1(3) yes C21 . C22 . C23 . 109.9(4) yes Ta1 . C22 . H221 . 121.120 no C21 . C22 . H221 . 125.068 no C23 . C22 . H221 . 125.067 no Ta1 . C23 . C22 . 73.2(3) yes Ta1 . C23 . C24 . 71.2(3) yes C22 . C23 . C24 . 106.3(5) yes Ta1 . C23 . H231 . 120.623 no C22 . C23 . H231 . 126.863 no C24 . C23 . H231 . 126.864 no Ta1 . C24 . C23 . 75.2(3) yes Ta1 . C24 . C25 . 71.7(3) yes C23 . C24 . C25 . 108.6(5) yes Ta1 . C24 . H241 . 119.151 no C23 . C24 . H241 . 125.723 no C25 . C24 . H241 . 125.723 no Ta1 . C25 . C21 . 74.0(3) yes Ta1 . C25 . C24 . 74.5(3) yes C21 . C25 . C24 . 108.0(4) yes Ta1 . C25 . H251 . 117.566 no C21 . C25 . H251 . 126.017 no C24 . C25 . H251 . 126.017 no P101 . C101 . C102 . 114.7(3) yes P101 . C101 . H1011 . 122.629 no C102 . C101 . H1011 . 122.629 no O101 . C102 . C101 . 122.3(4) yes O101 . C102 . C103 . 113.4(3) yes C101 . C102 . C103 . 124.3(4) yes C102 . C103 . C104 . 120.9(4) yes C102 . C103 . C108 . 120.3(4) yes C104 . C103 . C108 . 118.7(4) yes C103 . C104 . C105 . 120.7(4) yes C103 . C104 . H1041 . 119.673 no C105 . C104 . H1041 . 119.673 no C104 . C105 . C106 . 120.0(4) yes C104 . C105 . H1051 . 120.001 no C106 . C105 . H1051 . 120.001 no C105 . C106 . C107 . 120.0(4) yes C105 . C106 . H1061 . 119.989 no C107 . C106 . H1061 . 119.989 no C106 . C107 . C108 . 119.6(4) yes C106 . C107 . H1071 . 120.191 no C108 . C107 . H1071 . 120.191 no C103 . C108 . C107 . 121.0(4) yes C103 . C108 . H1081 . 119.497 no C107 . C108 . H1081 . 119.497 no P101 . C109 . C110 . 120.7(3) yes P101 . C109 . C114 . 120.6(3) yes C110 . C109 . C114 . 118.7(4) yes C109 . C110 . C111 . 120.0(4) yes C109 . C110 . H1101 . 120.014 no C111 . C110 . H1101 . 120.014 no C110 . C111 . C112 . 120.6(4) yes C110 . C111 . H1111 . 119.715 no C112 . C111 . H1111 . 119.715 no C111 . C112 . C113 . 119.4(4) yes C111 . C112 . H1121 . 120.319 no C113 . C112 . H1121 . 120.319 no C112 . C113 . C114 . 120.8(4) yes C112 . C113 . H1131 . 119.580 no C114 . C113 . H1131 . 119.580 no C109 . C114 . C113 . 120.5(4) yes C109 . C114 . H1141 . 119.736 no C113 . C114 . H1141 . 119.736 no P101 . C115 . C116 . 120.8(3) yes P101 . C115 . C120 . 120.8(3) yes C116 . C115 . C120 . 118.4(4) yes C115 . C116 . C117 . 120.9(4) yes C115 . C116 . H1161 . 119.532 no C117 . C116 . H1161 . 119.532 no C116 . C117 . C118 . 120.0(4) yes C116 . C117 . H1171 . 120.002 no C118 . C117 . H1171 . 120.002 no C117 . C118 . C119 . 119.7(4) yes C117 . C118 . H1181 . 120.170 no C119 . C118 . H1181 . 120.170 no C118 . C119 . C120 . 120.3(4) yes C118 . C119 . H1191 . 119.841 no C120 . C119 . H1191 . 119.841 no C115 . C120 . C119 . 120.6(4) yes C115 . C120 . H1201 . 119.694 no C119 . C120 . H1201 . 119.694 no Ta101 . C121 . C122 . 74.8(3) yes Ta101 . C121 . C125 . 74.8(3) yes C122 . C121 . C125 . 109.3(5) yes Ta101 . C121 . H1211 . 116.904 no C122 . C121 . H1211 . 125.352 no C125 . C121 . H1211 . 125.352 no Ta101 . C122 . C121 . 71.7(3) yes Ta101 . C122 . C123 . 74.9(3) yes C121 . C122 . C123 . 106.3(5) yes Ta101 . C122 . H1221 . 118.673 no C121 . C122 . H1221 . 126.832 no C123 . C122 . H1221 . 126.832 no Ta101 . C123 . C122 . 72.2(3) yes Ta101 . C123 . C124 . 73.5(3) yes C122 . C123 . C124 . 108.1(5) yes Ta101 . C123 . H1231 . 120.154 no C122 . C123 . H1231 . 125.957 no C124 . C123 . H1231 . 125.957 no Ta101 . C124 . C123 . 74.4(3) yes Ta101 . C124 . C125 . 72.6(3) yes C123 . C124 . C125 . 109.8(5) yes Ta101 . C124 . H1241 . 119.595 no C123 . C124 . H1241 . 125.089 no C125 . C124 . H1241 . 125.089 no Ta101 . C125 . C121 . 72.0(3) yes Ta101 . C125 . C124 . 74.7(3) yes C121 . C125 . C124 . 106.5(5) yes Ta101 . C125 . H1251 . 118.530 no C121 . C125 . H1251 . 126.770 no C124 . C125 . H1251 . 126.770 no data_CRYSTALS_cif _database_code_CSD 190866 _audit_creation_method CRYSTALS_ver_12-03-99 #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Enraf-Nonius DIP2000 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; DIP software 'Xpress' (MAC Science, 1989) ; _computing_data_reduction ; DIP software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #============================================================= _cell_length_a 7.876(1) _cell_angle_alpha 90 _cell_length_b 26.392(1) _cell_angle_beta 97.01(1) _cell_length_c 12.650(1) _cell_angle_gamma 90 _cell_volume 2609.8 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 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' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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' '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' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C28.50 H25 Cl3 Nb1 O1 P1 ' _chemical_formula_moiety ' C28.50 H25 Cl3 Nb1 O1 P1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 613.75 _cell_measurement_reflns_used 17664 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1237.170 _exptl_absorpt_coefficient_mu 0.851 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.84 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 17664 _reflns_number_total 5001 _diffrn_reflns_av_R_equivalents 0.106 _diffrn_measured_fraction_theta_max 0.934 _reflns_number_gt 4100 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.40 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -9 _reflns_limit_h_max 9 _reflns_limit_k_min -32 _reflns_limit_k_max 32 _reflns_limit_l_min -15 _reflns_limit_l_max 15 _refine_diff_density_min -0.44 _refine_diff_density_max 1.30 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 4100 _refine_ls_number_parameters 308 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.0543 _refine_ls_goodness_of_fit_ref 0.8072 _refine_ls_shift/su_max 0.020591 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 1.87 1.24 1.23 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_adp_type Nb1 0.70068(4) 0.109332(12) 0.43990(2) 0.0485 1.0000 Uani Cl2 0.76313(12) 0.13091(4) 0.26395(7) 0.0595 1.0000 Uani Cl1 0.85354(12) 0.18445(3) 0.50695(7) 0.0569 1.0000 Uani Cl3 0.44582(12) 0.06583(3) 0.35456(8) 0.0593 1.0000 Uani P1 0.47624(12) 0.18412(3) 0.39352(7) 0.0493 1.0000 Uani O1 0.5681(3) 0.11433(9) 0.5625(2) 0.0531 1.0000 Uani C1 0.3709(5) 0.17883(15) 0.5097(3) 0.0551 1.0000 Uani C2 0.4304(5) 0.14223(13) 0.5784(3) 0.0508 1.0000 Uani C11 0.3503(5) 0.12708(14) 0.6731(3) 0.0518 1.0000 Uani C12 0.3820(5) 0.07888(15) 0.7171(3) 0.0570 1.0000 Uani C13 0.2985(6) 0.06301(17) 0.8013(3) 0.0676 1.0000 Uani C14 0.1820(6) 0.09503(19) 0.8415(3) 0.0689 1.0000 Uani C15 0.1543(6) 0.14286(18) 0.8020(3) 0.0654 1.0000 Uani C16 0.2370(5) 0.15933(15) 0.7171(3) 0.0565 1.0000 Uani C21 0.3113(5) 0.18413(14) 0.2800(3) 0.0542 1.0000 Uani C22 0.1599(5) 0.21110(16) 0.2862(3) 0.0606 1.0000 Uani C23 0.0413(5) 0.21661(17) 0.1957(4) 0.0673 1.0000 Uani C24 0.0709(6) 0.19591(18) 0.1009(3) 0.0689 1.0000 Uani C25 0.2178(6) 0.16846(19) 0.0948(3) 0.0733 1.0000 Uani C26 0.3369(6) 0.16204(17) 0.1835(3) 0.0635 1.0000 Uani C31 0.5567(5) 0.24832(13) 0.3866(3) 0.0522 1.0000 Uani C32 0.6245(5) 0.26337(14) 0.2944(3) 0.0547 1.0000 Uani C33 0.6952(5) 0.31101(15) 0.2886(3) 0.0579 1.0000 Uani C34 0.6981(5) 0.34423(15) 0.3734(4) 0.0634 1.0000 Uani C35 0.6302(6) 0.32978(16) 0.4640(3) 0.0651 1.0000 Uani C36 0.5621(5) 0.28155(15) 0.4715(3) 0.0593 1.0000 Uani C41 0.7648(6) 0.01964(16) 0.4715(4) 0.0716 1.0000 Uani C42 0.8686(7) 0.03636(18) 0.3991(4) 0.0773 1.0000 Uani C43 0.9821(6) 0.07235(19) 0.4503(5) 0.0835 1.0000 Uani C44 0.9436(6) 0.07596(17) 0.5565(4) 0.0736 1.0000 Uani C45 0.8127(6) 0.04282(18) 0.5651(4) 0.0704 1.0000 Uani C91 -0.096(1) 0.4998(4) 0.4707(8) 0.089(3) 0.5000 Uiso C92 0.0350(14) 0.5281(6) 0.4475(11) 0.097(5) 0.5000 Uiso C93 0.1876(13) 0.5243(5) 0.5091(9) 0.103(3) 0.5000 Uiso C94 0.2070(15) 0.4929(6) 0.5918(12) 0.117(5) 0.5000 Uiso C95 0.0786(12) 0.4637(4) 0.6109(8) 0.089(3) 0.5000 Uiso C96 -0.0752(12) 0.4668(4) 0.5515(8) 0.069(3) 0.5000 Uiso C97 -0.2698(16) 0.5035(7) 0.4056(12) 0.116(5) 0.5000 Uiso H11 0.2741 0.2015 0.5231 0.0668 1.0000 Uiso H121 0.4653 0.0558 0.6876 0.0685 1.0000 Uiso H131 0.3220 0.0286 0.8331 0.0814 1.0000 Uiso H141 0.1176 0.0829 0.9000 0.0836 1.0000 Uiso H151 0.0745 0.1661 0.8342 0.0789 1.0000 Uiso H161 0.2153 0.1942 0.6876 0.0678 1.0000 Uiso H221 0.1369 0.2264 0.3554 0.0728 1.0000 Uiso H231 -0.0667 0.2360 0.2004 0.0802 1.0000 Uiso H241 -0.0138 0.2007 0.0361 0.0811 1.0000 Uiso H251 0.2387 0.1530 0.0254 0.0874 1.0000 Uiso H261 0.4421 0.1414 0.1782 0.0758 1.0000 Uiso H321 0.6218 0.2396 0.2327 0.0658 1.0000 Uiso H331 0.7446 0.3215 0.2228 0.0695 1.0000 Uiso H341 0.7494 0.3787 0.3689 0.0756 1.0000 Uiso H351 0.6299 0.3541 0.5246 0.0780 1.0000 Uiso H361 0.5168 0.2708 0.5386 0.0713 1.0000 Uiso H411 0.6698 -0.0055 0.4571 0.0852 1.0000 Uiso H421 0.8643 0.0250 0.3234 0.0919 1.0000 Uiso H431 1.0722 0.0916 0.4180 0.1019 1.0000 Uiso H441 1.0009 0.0983 0.6139 0.0859 1.0000 Uiso H451 0.7596 0.0367 0.6318 0.0848 1.0000 Uiso H921 0.0206 0.5518 0.3853 0.1167 0.5000 Uiso H931 0.2865 0.5454 0.4923 0.1234 0.5000 Uiso H941 0.3183 0.4914 0.6392 0.1406 0.5000 Uiso H951 0.0955 0.4387 0.6707 0.1064 0.5000 Uiso H961 -0.1721 0.4448 0.5676 0.0826 0.5000 Uiso H971 -0.3507 0.4796 0.4349 0.1390 0.5000 Uiso H972 -0.3139 0.5389 0.4089 0.1390 0.5000 Uiso H973 -0.2596 0.4944 0.3299 0.1390 0.5000 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 0.0466(2) 0.04966(18) 0.04949(18) -0.00029(12) 0.00661(13) 0.00212(12) Cl2 0.0589(5) 0.0677(5) 0.0536(5) 0.0012(4) 0.0139(4) 0.0037(4) Cl1 0.0540(5) 0.0546(5) 0.0610(5) -0.0028(4) 0.0022(4) -0.0007(3) Cl3 0.0548(5) 0.0572(5) 0.0649(5) -0.0014(4) 0.0030(4) -0.0042(4) P1 0.0494(5) 0.0528(5) 0.0464(4) 0.0026(3) 0.0084(4) 0.0028(3) O1 0.0525(14) 0.0577(14) 0.0499(13) 0.004(1) 0.0096(11) 0.005(1) C1 0.056(2) 0.061(2) 0.0499(18) 0.0015(15) 0.0134(16) 0.0042(15) C2 0.0489(19) 0.0516(18) 0.0523(18) -0.0018(14) 0.0076(15) 0.0006(14) C11 0.0472(19) 0.0601(19) 0.0473(17) 0.0007(14) 0.0029(15) -0.0046(14) C12 0.058(2) 0.060(2) 0.0533(19) 0.0001(16) 0.0072(17) -0.0046(16) C13 0.079(3) 0.068(2) 0.056(2) 0.0046(18) 0.011(2) -0.011(2) C14 0.073(3) 0.085(3) 0.051(2) 0.0006(19) 0.0159(19) -0.014(2) C15 0.062(2) 0.082(3) 0.053(2) -0.0049(19) 0.0116(18) -0.0049(19) C16 0.055(2) 0.064(2) 0.0509(18) -0.0037(16) 0.0060(16) -0.0018(16) C21 0.052(2) 0.058(2) 0.0527(19) 0.0070(15) 0.0072(16) -0.0013(15) C22 0.056(2) 0.065(2) 0.061(2) 0.0065(17) 0.0075(17) 0.0036(17) C23 0.054(2) 0.069(2) 0.077(3) 0.015(2) 0.0025(19) 0.0034(17) C24 0.061(3) 0.075(3) 0.067(2) 0.015(2) -0.0079(19) -0.0068(19) C25 0.076(3) 0.087(3) 0.055(2) -0.002(2) 0.002(2) -0.001(2) C26 0.061(2) 0.075(3) 0.054(2) -0.0012(17) 0.0025(18) 0.0069(18) C31 0.053(2) 0.0519(18) 0.0508(18) 0.0014(14) 0.0038(15) 0.0059(14) C32 0.058(2) 0.0564(19) 0.0506(18) 0.0013(15) 0.0087(16) 0.0022(15) C33 0.054(2) 0.063(2) 0.057(2) 0.0077(16) 0.0072(17) 0.0013(16) C34 0.058(2) 0.058(2) 0.073(3) 0.0060(18) 0.0026(19) -0.0012(16) C35 0.075(3) 0.062(2) 0.058(2) -0.0075(17) 0.0071(19) 0.0028(18) C36 0.065(2) 0.062(2) 0.0509(18) 0.0016(16) 0.0086(17) 0.0028(17) C41 0.061(3) 0.058(2) 0.094(3) 0.009(2) 0.002(2) 0.0036(18) C42 0.097(4) 0.067(3) 0.066(2) -0.008(2) 0.002(2) 0.032(2) C43 0.052(2) 0.075(3) 0.128(4) 0.036(3) 0.028(3) 0.018(2) C44 0.068(3) 0.061(2) 0.086(3) -0.007(2) -0.016(2) 0.0144(19) C45 0.068(3) 0.070(3) 0.074(3) 0.018(2) 0.012(2) 0.019(2) _refine_ls_extinction_method '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 . Cl2 . 2.4057(9) yes Nb1 . Cl1 . 2.4186(9) yes Nb1 . Cl3 . 2.446(1) yes Nb1 . P1 . 2.667(1) yes Nb1 . O1 . 1.977(2) yes Nb1 . C41 . 2.443(4) yes Nb1 . C42 . 2.427(4) yes Nb1 . C43 . 2.411(4) yes Nb1 . C44 . 2.433(4) yes Nb1 . C45 . 2.455(4) yes P1 . C1 . 1.779(4) yes P1 . C21 . 1.815(4) yes P1 . C31 . 1.815(4) yes O1 . C2 . 1.346(4) yes C1 . C2 . 1.345(5) yes C1 . H11 . 1.000 no C2 . C11 . 1.476(5) yes C11 . C12 . 1.399(5) yes C11 . C16 . 1.397(5) yes C12 . C13 . 1.383(5) yes C12 . H121 . 1.000 no C13 . C14 . 1.389(7) yes C13 . H131 . 1.000 no C14 . C15 . 1.365(7) yes C14 . H141 . 1.000 no C15 . C16 . 1.392(6) yes C15 . H151 . 1.000 no C16 . H161 . 1.000 no C21 . C22 . 1.399(5) yes C21 . C26 . 1.389(5) yes C22 . C23 . 1.394(6) yes C22 . H221 . 1.000 no C23 . C24 . 1.364(7) yes C23 . H231 . 1.000 no C24 . C25 . 1.375(7) yes C24 . H241 . 1.000 no C25 . C26 . 1.382(6) yes C25 . H251 . 1.000 no C26 . H261 . 1.000 no C31 . C32 . 1.398(5) yes C31 . C36 . 1.383(5) yes C32 . C33 . 1.381(6) yes C32 . H321 . 1.000 no C33 . C34 . 1.384(6) yes C33 . H331 . 1.000 no C34 . C35 . 1.376(6) yes C34 . H341 . 1.000 no C35 . C36 . 1.389(6) yes C35 . H351 . 1.000 no C36 . H361 . 1.000 no C41 . C42 . 1.373(7) yes C41 . C45 . 1.345(7) yes C41 . H411 . 1.000 no C42 . C43 . 1.407(8) yes C42 . H421 . 1.000 no C43 . C44 . 1.416(8) yes C43 . H431 . 1.000 no C44 . C45 . 1.367(7) yes C44 . H441 . 1.000 no C45 . H451 . 1.000 no C91 . C92 . 1.334(8) yes C91 . C96 . 1.339(8) yes C91 . C97 . 1.511(9) yes C92 . C93 . 1.354(9) yes C92 . H921 . 1.000 no C93 . C94 . 1.330(9) yes C93 . H931 . 1.000 no C94 . C95 . 1.316(9) yes C94 . H941 . 1.00 no C95 . C96 . 1.348(8) yes C95 . H951 . 1.000 no C96 . H961 . 1.000 no C97 . H971 . 1.000 no C97 . H972 . 1.000 no C97 . H973 . 1.000 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 Cl2 . Nb1 . Cl1 . 88.92(3) yes Cl2 . Nb1 . Cl3 . 87.26(3) yes Cl1 . Nb1 . Cl3 . 152.37(3) yes Cl2 . Nb1 . P1 . 79.99(3) yes Cl1 . Nb1 . P1 . 76.03(3) yes Cl3 . Nb1 . P1 . 76.36(3) yes Cl2 . Nb1 . O1 . 153.80(8) yes Cl1 . Nb1 . O1 . 87.60(8) yes Cl3 . Nb1 . O1 . 83.92(8) yes P1 . Nb1 . O1 . 73.97(7) yes Cl2 . Nb1 . C41 . 108.61(13) yes Cl1 . Nb1 . C41 . 130.74(12) yes Cl3 . Nb1 . C41 . 76.09(12) yes P1 . Nb1 . C41 . 150.62(12) yes O1 . Nb1 . C41 . 93.14(14) yes Cl2 . Nb1 . C42 . 79.21(12) yes Cl1 . Nb1 . C42 . 117.65(14) yes Cl3 . Nb1 . C42 . 88.44(14) yes P1 . Nb1 . C42 . 154.72(11) yes O1 . Nb1 . C42 . 124.99(14) yes Cl2 . Nb1 . C43 . 81.71(14) yes Cl1 . Nb1 . C43 . 84.14(14) yes Cl3 . Nb1 . C43 . 122.24(15) yes P1 . Nb1 . C43 . 153.13(11) yes O1 . Nb1 . C43 . 123.67(16) yes Cl2 . Nb1 . C44 . 114.33(14) yes Cl1 . Nb1 . C44 . 76.31(11) yes Cl3 . Nb1 . C44 . 129.76(12) yes P1 . Nb1 . C44 . 148.45(11) yes O1 . Nb1 . C44 . 90.01(15) yes Cl2 . Nb1 . C45 . 131.9(1) yes Cl1 . Nb1 . C45 . 103.63(13) yes Cl3 . Nb1 . C45 . 99.20(13) yes P1 . Nb1 . C45 . 147.9(1) yes O1 . Nb1 . C45 . 73.99(12) yes C41 . Nb1 . C42 . 32.74(17) yes C41 . Nb1 . C43 . 55.14(16) yes C42 . Nb1 . C43 . 33.80(19) yes C41 . Nb1 . C44 . 54.45(16) yes C42 . Nb1 . C44 . 55.47(16) yes C43 . Nb1 . C44 . 33.99(18) yes C41 . Nb1 . C45 . 31.87(17) yes C42 . Nb1 . C45 . 53.67(15) yes C43 . Nb1 . C45 . 54.54(15) yes C44 . Nb1 . C45 . 32.46(16) yes Nb1 . P1 . C1 . 97.09(13) yes Nb1 . P1 . C21 . 124.43(13) yes C1 . P1 . C21 . 107.02(18) yes Nb1 . P1 . C31 . 118.40(12) yes C1 . P1 . C31 . 108.27(17) yes C21 . P1 . C31 . 100.50(17) yes Nb1 . O1 . C2 . 131.8(2) yes P1 . C1 . C2 . 115.4(3) yes P1 . C1 . H11 . 122.3 no C2 . C1 . H11 . 122.3 no O1 . C2 . C1 . 121.3(3) yes O1 . C2 . C11 . 113.9(3) yes C1 . C2 . C11 . 124.7(3) yes C2 . C11 . C12 . 119.7(3) yes C2 . C11 . C16 . 121.0(3) yes C12 . C11 . C16 . 119.1(3) yes C11 . C12 . C13 . 120.2(4) yes C11 . C12 . H121 . 119.9 no C13 . C12 . H121 . 119.9 no C12 . C13 . C14 . 119.7(4) yes C12 . C13 . H131 . 120.2 no C14 . C13 . H131 . 120.2 no C13 . C14 . C15 . 120.8(4) yes C13 . C14 . H141 . 119.6 no C15 . C14 . H141 . 119.6 no C14 . C15 . C16 . 120.1(4) yes C14 . C15 . H151 . 119.9 no C16 . C15 . H151 . 119.9 no C11 . C16 . C15 . 119.9(4) yes C11 . C16 . H161 . 120.0 no C15 . C16 . H161 . 120.0 no P1 . C21 . C22 . 119.2(3) yes P1 . C21 . C26 . 121.9(3) yes C22 . C21 . C26 . 118.6(4) yes C21 . C22 . C23 . 119.8(4) yes C21 . C22 . H221 . 120.1 no C23 . C22 . H221 . 120.1 no C22 . C23 . C24 . 120.7(4) yes C22 . C23 . H231 . 119.6 no C24 . C23 . H231 . 119.6 no C23 . C24 . C25 . 119.7(4) yes C23 . C24 . H241 . 120.1 no C25 . C24 . H241 . 120.1 no C24 . C25 . C26 . 120.7(4) yes C24 . C25 . H251 . 119.6 no C26 . C25 . H251 . 119.6 no C21 . C26 . C25 . 120.3(4) yes C21 . C26 . H261 . 119.8 no C25 . C26 . H261 . 119.8 no P1 . C31 . C32 . 118.4(3) yes P1 . C31 . C36 . 122.2(3) yes C32 . C31 . C36 . 119.3(3) yes C31 . C32 . C33 . 120.1(3) yes C31 . C32 . H321 . 120.0 no C33 . C32 . H321 . 120.0 no C32 . C33 . C34 . 120.2(3) yes C32 . C33 . H331 . 119.9 no C34 . C33 . H331 . 119.9 no C33 . C34 . C35 . 119.9(4) yes C33 . C34 . H341 . 120.0 no C35 . C34 . H341 . 120.0 no C34 . C35 . C36 . 120.2(4) yes C34 . C35 . H351 . 119.9 no C36 . C35 . H351 . 119.9 no C31 . C36 . C35 . 120.2(4) yes C31 . C36 . H361 . 119.9 no C35 . C36 . H361 . 119.9 no Nb1 . C41 . C42 . 73.0(2) yes Nb1 . C41 . C45 . 74.5(3) yes C42 . C41 . C45 . 108.4(4) yes Nb1 . C41 . H411 . 118.5 no C42 . C41 . H411 . 125.8 no C45 . C41 . H411 . 125.8 no Nb1 . C42 . C41 . 74.3(3) yes Nb1 . C42 . C43 . 72.4(2) yes C41 . C42 . C43 . 107.9(4) yes Nb1 . C42 . H421 . 119.1 no C41 . C42 . H421 . 126.1 no C43 . C42 . H421 . 126.1 no Nb1 . C43 . C42 . 73.7(3) yes Nb1 . C43 . C44 . 73.9(2) yes C42 . C43 . C44 . 106.5(4) yes Nb1 . C43 . H431 . 117.8 no C42 . C43 . H431 . 126.7 no C44 . C43 . H431 . 126.7 no Nb1 . C44 . C43 . 72.1(2) yes Nb1 . C44 . C45 . 74.6(3) yes C43 . C44 . C45 . 106.5(4) yes Nb1 . C44 . H441 . 118.6 no C43 . C44 . H441 . 126.8 no C45 . C44 . H441 . 126.8 no Nb1 . C45 . C41 . 73.6(3) yes Nb1 . C45 . C44 . 72.9(3) yes C41 . C45 . C44 . 110.7(4) yes Nb1 . C45 . H451 . 120.5 no C41 . C45 . H451 . 124.6 no C44 . C45 . H451 . 124.6 no C92 . C91 . C96 . 120.4(6) yes C92 . C91 . C97 . 121.2(6) yes C96 . C91 . C97 . 118.5(6) yes C91 . C92 . C93 . 119.3(6) yes C91 . C92 . H921 . 120.4 no C93 . C92 . H921 . 120.4 no C92 . C93 . C94 . 120.5(7) yes C92 . C93 . H931 . 119.8 no C94 . C93 . H931 . 119.8 no C93 . C94 . C95 . 119.5(7) yes C93 . C94 . H941 . 120.3 no C95 . C94 . H941 . 120.3 no C94 . C95 . C96 . 121.4(6) yes C94 . C95 . H951 . 119.3 no C96 . C95 . H951 . 119.3 no C91 . C96 . C95 . 118.9(6) yes C91 . C96 . H961 . 120.5 no C95 . C96 . H961 . 120.5 no C91 . C97 . H971 . 109.5 no C91 . C97 . H972 . 109.5 no H971 . C97 . H972 . 109.5 no C91 . C97 . H973 . 109.5 no H971 . C97 . H973 . 109.5 no H972 . C97 . H973 . 109.5 no