#------------------------------------------------------------------------------ #$Date: 2021-04-16 11:46:56 +0300 (Fri, 16 Apr 2021) $ #$Revision: 264242 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/34/31/4343173.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4343173 loop_ _publ_author_name 'Sietzen, Malte' 'Wadepohl, Hubert' 'Ballmann, Joachim' _publ_section_title ; Synthesis and reactivity of cyclometalated triamidophosphine complexes of niobium and tantalum. ; _journal_issue 8 _journal_name_full 'Inorganic chemistry' _journal_page_first 4094 _journal_page_last 4103 _journal_paper_doi 10.1021/acs.inorgchem.5b00333 _journal_volume 54 _journal_year 2015 _chemical_formula_moiety 'C45 H44 N3 P Ta, 1.5(C6 H6)' _chemical_formula_sum 'C54 H54 N3 P Ta' _chemical_formula_weight 956.92 _chemical_properties_physical 'air-sensitive, moisture-sensitive' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_block_code ba_ms7 _audit_creation_date ; 'Wed Dec 04 12:29:14 2013' ; _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998) ; _audit_update_record '10.02.2015 17:26:42 CET UTC+01:00 encif 1.29' _cell_angle_alpha 77.885(5) _cell_angle_beta 68.693(5) _cell_angle_gamma 70.190(5) _cell_formula_units_Z 2 _cell_length_a 12.0019(6) _cell_length_b 13.7239(7) _cell_length_c 15.1796(9) _cell_measurement_reflns_used 5944 _cell_measurement_temperature 110(1) _cell_measurement_theta_max 65.7680 _cell_measurement_theta_min 4.1220 _cell_volume 2180.8(2) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'SUPERFLIP (Palatinus, 2007-2009)' _diffrn_ambient_temperature 110(1) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 7.9621 _diffrn_detector_type 'Agilent EOS' 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35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 77.0000 30.0000 27 106 omega 79.00 177.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 77.0000 -60.0000 98 107 omega 85.00 174.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 64.0000 -90.0000 89 108 omega 125.00 171.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 77.0000 0.0000 46 109 omega 78.00 105.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 77.0000 0.0000 27 110 omega 90.00 117.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 64.0000 -120.0000 27 111 omega 147.00 177.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 77.0000 60.0000 30 112 omega 84.00 109.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -80.0000 -29.0823 25 113 omega 78.00 104.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 77.0000 60.0000 26 114 omega 49.00 75.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -80.0000 -29.0823 26 115 omega 79.00 163.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 77.0000 -180.0000 84 116 omega 85.00 173.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 64.0000 90.0000 88 117 omega 37.00 130.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -79.0000 -105.9044 93 118 omega 82.00 177.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 38.0000 60.0000 95 119 omega 78.00 172.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 77.0000 150.0000 94 120 omega 86.00 134.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 64.0000 -30.0000 48 121 omega 41.00 138.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -80.0000 88.5149 97 122 omega 117.00 175.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 64.0000 -150.0000 58 123 omega 86.00 111.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 64.0000 -150.0000 25 124 omega 86.00 133.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 64.0000 120.0000 47 ; _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Agilent SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'polyimid foil' _diffrn_orient_matrix_UB_11 -0.0214934000 _diffrn_orient_matrix_UB_12 0.0384684000 _diffrn_orient_matrix_UB_13 -0.0970589000 _diffrn_orient_matrix_UB_21 -0.0334217000 _diffrn_orient_matrix_UB_22 -0.0998390000 _diffrn_orient_matrix_UB_23 0.0030096000 _diffrn_orient_matrix_UB_31 -0.1382927000 _diffrn_orient_matrix_UB_32 0.0541212000 _diffrn_orient_matrix_UB_33 0.0505430000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents 0.1702 _diffrn_reflns_av_unetI/netI 0.1426 _diffrn_reflns_laue_measured_fraction_full 0.974 _diffrn_reflns_laue_measured_fraction_max 0.974 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 48943 _diffrn_reflns_point_group_measured_fraction_full 0.974 _diffrn_reflns_point_group_measured_fraction_max 0.974 _diffrn_reflns_theta_full 67.564 _diffrn_reflns_theta_max 67.564 _diffrn_reflns_theta_min 4.129 _diffrn_source 'microfocus X-Ray tube' _diffrn_source_type 'Agilent SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 5.300 _exptl_absorpt_correction_T_max 0.811 _exptl_absorpt_correction_T_min 0.623 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.457 _exptl_crystal_description irregular _exptl_crystal_F_000 974 _exptl_crystal_size_max 0.127 _exptl_crystal_size_mid 0.094 _exptl_crystal_size_min 0.045 _refine_diff_density_max 1.868 _refine_diff_density_min -3.895 _refine_diff_density_rms 0.228 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 544 _refine_ls_number_reflns 7677 _refine_ls_number_restraints 30 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0672 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+8.4041P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1472 _refine_ls_wR_factor_ref 0.1948 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5378 _reflns_number_total 7677 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; ba_ms7.res created by SHELXL-2014/7 TITL ba_ms7 - #1917 - in P-1 - superflip - nova CELL 1.54184 12.001889 13.723927 15.179621 77.8853 68.6933 70.1898 ZERR 1 0.000639 0.000719 0.000856 0.0047 0.0051 0.0048 LATT 1 SFAC C H N P Ta UNIT 108 108 6 2 2 EQIV $1 1-X,1-Y,1-Z SADI 0.01 C81 C82 C82 C83 C81 C83_$1 SADI C83_$1 C82 C81 C83 C82 C81_$1 RIGU N1 C2 C7 RIGU N2 C22 RIGU N3 C38 RIGU C81 C82 C83 L.S. 10 PLAN 40 SIZE 0.1 0.1 0.1 TEMP -163.14 BOND $H CONF MORE -1 fmap 2 acta REM REM REM WGHT 0.063700 8.404099 FVAR 1.64048 TA 5 0.931196 0.004062 0.114197 11.00000 0.02726 0.01910 = 0.03393 -0.00487 -0.01308 -0.00461 P 4 0.715221 0.090944 0.224863 11.00000 0.02598 0.01825 = 0.03708 -0.00606 -0.01133 -0.00484 N1 3 1.037319 -0.060188 0.194498 11.00000 0.01308 0.03525 = 0.02100 -0.00225 -0.00042 -0.00758 N2 3 0.920344 0.159428 0.104905 11.00000 0.02149 0.01554 = 0.03443 0.01476 -0.02060 -0.00657 N3 3 0.837640 -0.095128 0.108593 11.00000 0.01787 0.02298 = 0.01883 0.00294 -0.01015 0.00024 C1 1 0.751106 0.107854 0.326546 11.00000 0.03109 0.02671 = 0.02686 -0.00349 -0.00462 -0.01970 C2 1 0.865698 0.038758 0.332513 11.00000 0.03790 0.03281 = 0.02602 -0.00570 -0.00819 -0.01153 C3 1 0.916064 0.052713 0.395349 11.00000 0.04607 0.03872 = 0.02903 -0.00417 -0.01553 -0.01137 AFIX 43 H3 2 0.993594 0.006281 0.399839 11.00000 -1.20000 AFIX 0 C4 1 0.854738 0.133825 0.452079 11.00000 0.05056 0.02952 = 0.04911 -0.00083 -0.02728 -0.01886 AFIX 43 H4 2 0.891750 0.145306 0.493220 11.00000 -1.20000 AFIX 0 C5 1 0.738864 0.198313 0.448547 11.00000 0.02985 0.02069 = 0.04630 -0.01380 -0.00683 -0.00231 AFIX 43 H5 2 0.695350 0.251587 0.490210 11.00000 -1.20000 AFIX 0 C6 1 0.685572 0.187683 0.387313 11.00000 0.03353 0.02685 = 0.05256 -0.01133 -0.01725 -0.00991 AFIX 43 H6 2 0.606278 0.232871 0.385552 11.00000 -1.20000 AFIX 0 C7 1 0.915854 -0.045367 0.267483 11.00000 0.02953 0.03208 = 0.03337 -0.00130 -0.01377 -0.01227 AFIX 13 H7 2 0.888983 -0.109764 0.295027 11.00000 -1.20000 AFIX 0 C8 1 1.144799 -0.138322 0.207293 11.00000 0.01963 0.01915 = 0.03488 -0.00959 -0.00879 -0.00491 C9 1 1.255926 -0.155231 0.131220 11.00000 0.03414 0.02060 = 0.04269 -0.00286 -0.02280 -0.00633 AFIX 43 H9 2 1.260194 -0.111943 0.073064 11.00000 -1.20000 AFIX 0 C10 1 1.359431 -0.234813 0.140610 11.00000 0.03136 0.02941 = 0.04827 -0.00966 -0.02159 -0.00430 C11 1 1.353919 -0.298844 0.224582 11.00000 0.03600 0.02010 = 0.05637 -0.01206 -0.02602 0.00406 AFIX 43 H11 2 1.425859 -0.353881 0.229472 11.00000 -1.20000 AFIX 0 C12 1 1.245956 -0.284418 0.301496 11.00000 0.03558 0.01744 = 0.05074 -0.00897 -0.02018 -0.00709 C13 1 1.138749 -0.201037 0.293144 11.00000 0.03298 0.01551 = 0.03495 -0.00433 -0.01329 -0.00044 AFIX 43 H13 2 1.063975 -0.188392 0.345589 11.00000 -1.20000 AFIX 0 C14 1 1.478407 -0.253435 0.054137 11.00000 0.03089 0.05430 = 0.06169 -0.02092 -0.02101 -0.00754 AFIX 137 H14A 2 1.466641 -0.285117 0.007239 11.00000 -1.50000 H14B 2 1.548934 -0.300175 0.074365 11.00000 -1.50000 H14C 2 1.495567 -0.186896 0.025630 11.00000 -1.50000 AFIX 0 C15 1 1.236129 -0.358492 0.390541 11.00000 0.04121 0.04102 = 0.04229 0.00148 -0.01642 -0.00866 AFIX 137 H15A 2 1.231695 -0.424184 0.378282 11.00000 -1.50000 H15B 2 1.160620 -0.327854 0.441199 11.00000 -1.50000 H15C 2 1.309671 -0.371693 0.410151 11.00000 -1.50000 AFIX 0 C16 1 0.627721 0.221784 0.190296 11.00000 0.02991 0.02828 = 0.03190 -0.00486 -0.01085 -0.01307 C17 1 0.696544 0.280659 0.119428 11.00000 0.03239 0.02954 = 0.03859 -0.01349 -0.02477 -0.00489 C18 1 0.633017 0.382894 0.091724 11.00000 0.02092 0.02289 = 0.04383 -0.01129 -0.00976 0.00539 AFIX 43 H18 2 0.678430 0.423960 0.042963 11.00000 -1.20000 AFIX 0 C19 1 0.507410 0.424369 0.133454 11.00000 0.05150 0.02486 = 0.04898 -0.00277 -0.03204 -0.00727 AFIX 43 H19 2 0.466268 0.493562 0.114085 11.00000 -1.20000 AFIX 0 C20 1 0.440036 0.363653 0.205126 11.00000 0.02299 0.04253 = 0.05367 -0.02323 -0.01082 -0.00227 AFIX 43 H20 2 0.352773 0.391346 0.234587 11.00000 -1.20000 AFIX 0 C21 1 0.501811 0.262880 0.232641 11.00000 0.03310 0.01694 = 0.03697 0.00141 -0.01259 -0.00662 AFIX 43 H21 2 0.456397 0.221810 0.281397 11.00000 -1.20000 AFIX 0 C22 1 0.834440 0.243335 0.061013 11.00000 0.02509 0.01879 = 0.03368 -0.00635 -0.00727 -0.00510 AFIX 23 H22A 2 0.838987 0.219325 0.002352 11.00000 -1.20000 H22B 2 0.867260 0.304406 0.041401 11.00000 -1.20000 AFIX 0 C23 1 0.983127 0.196204 0.149956 11.00000 0.04397 0.03118 = 0.05386 0.00152 -0.02603 -0.02400 C24 1 1.109177 0.146822 0.137498 11.00000 0.03201 0.03886 = 0.04490 -0.01897 -0.01527 -0.00551 AFIX 43 H24 2 1.152334 0.090553 0.099116 11.00000 -1.20000 AFIX 0 C25 1 1.171848 0.179587 0.180983 11.00000 0.02116 0.04329 = 0.03089 -0.00278 -0.01292 -0.01029 C26 1 1.105151 0.262146 0.238684 11.00000 0.03807 0.03862 = 0.05372 -0.00670 -0.01799 -0.02122 AFIX 43 H26 2 1.147358 0.284478 0.269295 11.00000 -1.20000 AFIX 0 C27 1 0.980676 0.311093 0.251743 11.00000 0.05937 0.02024 = 0.05053 -0.00986 -0.02718 -0.00787 C28 1 0.917743 0.278917 0.205885 11.00000 0.04866 0.00733 = 0.03994 0.00022 -0.02281 -0.00992 AFIX 43 H28 2 0.832075 0.313098 0.213002 11.00000 -1.20000 AFIX 0 C29 1 1.307666 0.127213 0.168685 11.00000 0.03755 0.05832 = 0.06116 -0.01413 -0.01407 -0.02238 AFIX 137 H29A 2 1.317495 0.092654 0.229951 11.00000 -1.50000 H29B 2 1.353662 0.179303 0.145141 11.00000 -1.50000 H29C 2 1.340584 0.075461 0.122929 11.00000 -1.50000 AFIX 0 C30 1 0.907852 0.395568 0.316452 11.00000 0.06635 0.03514 = 0.04507 -0.01048 -0.01573 -0.02102 AFIX 137 H30A 2 0.869118 0.365142 0.380130 11.00000 -1.50000 H30B 2 0.842728 0.445374 0.291853 11.00000 -1.50000 H30C 2 0.964027 0.431500 0.319743 11.00000 -1.50000 AFIX 0 C31 1 0.603973 0.015885 0.264749 11.00000 0.03066 0.02614 = 0.05482 -0.01107 -0.02496 -0.00156 C32 1 0.613035 -0.046494 0.198278 11.00000 0.02239 0.02221 = 0.03272 -0.00570 -0.01005 0.00021 C33 1 0.530651 -0.107243 0.226240 11.00000 0.03331 0.02527 = 0.04544 -0.01311 -0.01858 -0.00521 AFIX 43 H33 2 0.534355 -0.149806 0.182726 11.00000 -1.20000 AFIX 0 C34 1 0.443561 -0.106354 0.316543 11.00000 0.03521 0.04525 = 0.04156 -0.02254 0.00581 -0.01954 AFIX 43 H34 2 0.387587 -0.147351 0.333953 11.00000 -1.20000 AFIX 0 C35 1 0.438183 -0.046766 0.380305 11.00000 0.03124 0.04255 = 0.04354 -0.00318 0.00114 -0.02455 AFIX 43 H35 2 0.379300 -0.047684 0.442279 11.00000 -1.20000 AFIX 0 C36 1 0.517097 0.014877 0.356074 11.00000 0.03608 0.02385 = 0.03778 -0.01331 -0.00640 0.00110 AFIX 43 H36 2 0.512477 0.056215 0.400954 11.00000 -1.20000 AFIX 0 C37 1 0.710015 -0.047240 0.100484 11.00000 0.01302 0.02213 = 0.03089 -0.01111 0.00101 -0.00551 H37A 2 0.677841 -0.080928 0.060648 11.00000 -1.20000 H37B 2 0.699857 0.028891 0.065546 11.00000 -1.20000 C38 1 0.875887 -0.204196 0.116308 11.00000 0.02252 0.01543 = 0.02463 0.00476 -0.00528 -0.00846 C39 1 0.818147 -0.265508 0.093863 11.00000 0.02841 0.03031 = 0.03914 -0.00783 -0.00939 -0.00651 AFIX 43 H39 2 0.745985 -0.232113 0.074722 11.00000 -1.20000 AFIX 0 C40 1 0.863848 -0.373191 0.098974 11.00000 0.04122 0.02493 = 0.05447 -0.00813 -0.01798 -0.01550 C41 1 0.969410 -0.424515 0.127623 11.00000 0.02867 0.01989 = 0.04147 -0.00625 -0.01266 -0.00738 AFIX 43 H41 2 1.001925 -0.498128 0.129508 11.00000 -1.20000 AFIX 0 C42 1 1.026077 -0.367182 0.153191 11.00000 0.01724 0.02814 = 0.04003 -0.00940 -0.00807 -0.00289 C43 1 0.976500 -0.259015 0.149133 11.00000 0.01805 0.02546 = 0.04664 -0.01494 -0.00682 -0.01260 AFIX 43 H43 2 1.013517 -0.220751 0.169933 11.00000 -1.20000 AFIX 0 C44 1 0.795938 -0.434705 0.073408 11.00000 0.05222 0.03877 = 0.09513 -0.02264 -0.04136 -0.01532 AFIX 137 H44A 2 0.716542 -0.433462 0.123973 11.00000 -1.50000 H44B 2 0.848189 -0.506891 0.066504 11.00000 -1.50000 H44C 2 0.779775 -0.402993 0.013444 11.00000 -1.50000 AFIX 0 C45 1 1.137217 -0.421017 0.186403 11.00000 0.04122 0.02797 = 0.06023 -0.00210 -0.01900 -0.01445 AFIX 137 H45A 2 1.113314 -0.416335 0.254695 11.00000 -1.50000 H45B 2 1.203480 -0.387592 0.152029 11.00000 -1.50000 H45C 2 1.167570 -0.494347 0.174214 11.00000 -1.50000 AFIX 0 C51 1 0.868989 0.611369 0.461263 11.00000 0.06487 0.04304 = 0.04821 -0.00693 -0.02640 0.00845 AFIX 43 H51 2 0.915104 0.539824 0.460160 11.00000 -1.20000 AFIX 0 C52 1 0.817278 0.661128 0.391486 11.00000 0.03282 0.04715 = 0.03838 -0.02277 0.00283 -0.01670 AFIX 43 H52 2 0.829314 0.624491 0.340621 11.00000 -1.20000 AFIX 0 C53 1 0.747423 0.764590 0.394299 11.00000 0.05721 0.03888 = 0.05756 -0.01043 -0.02176 -0.01363 AFIX 43 H53 2 0.709295 0.798606 0.346733 11.00000 -1.20000 AFIX 0 C54 1 0.733715 0.818006 0.467259 11.00000 0.05493 0.02376 = 0.04393 -0.00775 -0.00463 -0.00089 AFIX 43 H54 2 0.686208 0.889166 0.469581 11.00000 -1.20000 AFIX 0 C55 1 0.788122 0.768987 0.535986 11.00000 0.06673 0.04016 = 0.04715 -0.01334 -0.02330 -0.00009 AFIX 43 H55 2 0.780385 0.806281 0.585038 11.00000 -1.20000 AFIX 0 C56 1 0.853565 0.666158 0.533555 11.00000 0.09864 0.06977 = 0.06809 -0.01946 -0.05898 0.01742 AFIX 43 H56 2 0.889156 0.631609 0.582406 11.00000 -1.20000 AFIX 0 C81 1 0.570211 0.549182 0.420333 11.00000 0.02694 0.02792 = 0.20311 -0.00138 -0.03496 0.00226 AFIX 43 H81 2 0.618557 0.582630 0.365934 11.00000 -1.20000 AFIX 0 C82 1 0.539489 0.579941 0.509624 11.00000 0.04484 0.04441 = 0.20677 -0.01023 -0.03160 -0.00877 AFIX 43 H82 2 0.566201 0.634972 0.516233 11.00000 -1.20000 AFIX 0 C83 1 0.469827 0.530606 0.589414 11.00000 0.03741 0.04477 = 0.20329 -0.01382 -0.03131 -0.00090 AFIX 43 H83 2 0.449592 0.551402 0.650566 11.00000 -1.20000 AFIX 0 HKLF 4 REM ba_ms7 - #1917 - in P-1 - superflip - nova REM R1 = 0.0672 for 5378 Fo > 4sig(Fo) and 0.1089 for all 7677 data REM 544 parameters refined using 30 restraints END WGHT 0.0639 8.3263 REM Highest difference peak 1.868, deepest hole -3.895, 1-sigma level 0.228 Q1 1 0.8964 0.0562 0.0190 11.00000 0.05 1.87 Q2 1 1.0578 -0.0209 0.0396 11.00000 0.05 1.84 Q3 1 0.8054 0.0261 0.1877 11.00000 0.05 1.84 Q4 1 0.9890 -0.0966 0.1475 11.00000 0.05 1.80 Q5 1 1.0204 0.0172 0.0036 11.00000 0.05 1.77 Q6 1 0.8695 0.1100 0.0849 11.00000 0.05 1.74 Q7 1 0.8038 0.0083 0.3420 11.00000 0.05 1.65 Q8 1 1.0341 -0.0004 0.0187 11.00000 0.05 1.64 Q9 1 0.8377 0.0012 0.0844 11.00000 0.05 1.51 Q10 1 0.8759 0.0200 0.2321 11.00000 0.05 1.41 Q11 1 1.0474 -0.0745 0.0462 11.00000 0.05 1.38 Q12 1 0.9619 -0.0422 0.2122 11.00000 0.05 1.36 Q13 1 0.9583 0.0417 0.0922 11.00000 0.05 1.32 Q14 1 0.8237 0.1549 0.0383 11.00000 0.05 1.28 Q15 1 1.0322 -0.1419 0.1883 11.00000 0.05 1.20 Q16 1 0.9736 -0.0223 0.1076 11.00000 0.05 1.14 Q17 1 0.9143 0.1394 -0.0073 11.00000 0.05 1.11 Q18 1 0.9151 -0.1378 0.0585 11.00000 0.05 1.09 Q19 1 0.7593 0.1452 0.1191 11.00000 0.05 1.04 Q20 1 0.9645 -0.0812 0.0778 11.00000 0.05 1.04 Q21 1 0.7784 -0.0067 0.2664 11.00000 0.05 1.03 Q22 1 0.9140 -0.0384 0.0250 11.00000 0.05 1.01 Q23 1 0.9222 0.1067 0.1371 11.00000 0.05 1.01 Q24 1 0.9423 0.0742 0.2046 11.00000 0.05 1.00 Q25 1 1.0893 -0.1127 0.0995 11.00000 0.05 1.00 Q26 1 0.8954 0.0166 0.1046 11.00000 0.05 0.95 Q27 1 0.9496 -0.1187 0.2381 11.00000 0.05 0.93 Q28 1 0.9031 -0.1032 0.1796 11.00000 0.05 0.92 Q29 1 0.8455 0.0994 0.1819 11.00000 0.05 0.86 Q30 1 0.8989 0.2003 0.0563 11.00000 0.05 0.85 Q31 1 1.1485 0.0230 0.0432 11.00000 0.05 0.85 Q32 1 0.8573 -0.0365 0.2184 11.00000 0.05 0.83 Q33 1 0.6648 0.1386 0.1395 11.00000 0.05 0.82 Q34 1 1.1599 -0.0037 0.0574 11.00000 0.05 0.81 Q35 1 1.0173 0.0183 0.1441 11.00000 0.05 0.80 Q36 1 0.7578 -0.0589 0.3354 11.00000 0.05 0.80 Q37 1 1.1668 -0.0321 0.0620 11.00000 0.05 0.80 Q38 1 1.0391 0.0851 0.1017 11.00000 0.05 0.79 Q39 1 0.9603 0.1246 0.0516 11.00000 0.05 0.78 Q40 1 0.7643 0.8870 0.2913 11.00000 0.05 0.78 ; _cod_data_source_file ic5b00333_si_001.cif _cod_data_source_block ba_ms7 _cod_depositor_comments ; 2021-04-15 Z value and formula fixed to values more according to usual chemical conventions. miguel ; _cod_original_formula_sum 'C108 H108 N6 P2 Ta2' _cod_original_formula_weight 1913.84 _cod_original_formula_moiety 'C90 H88 N6 P2 Ta2, 3(C6 H6)' _cod_original_formula_units_Z 1 _cod_database_code 4343173 _audit_block_refno 1917 _audit_block_usercomment 'MS281, irregular, orange' _chemical_oxdiff_formula 'C108 H106 N6 P2 Ta2 ' _chemical_oxdiff_usercomment 'MS281, irregular, orange' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.619 _shelx_estimated_absorpt_t_min 0.619 _reflns_odcompleteness_completeness 98.36 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _shelxl_version_number 2014/7 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C81-C82 \\sim C82-C83 \\sim C81-C83_$1 with sigma of 0.01 C83_$1-C82 \\sim C81-C83 \\sim C82-C81_$1 with sigma of 0.02 3. Rigid body (RIGU) restrains N1, C2, C7 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 N2, C22 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 N3, C38 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C81, C82, C83 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4.a Ternary CH refined with riding coordinates: C7(H7) 4.b Secondary CH2 refined with riding coordinates: C22(H22A,H22B) 4.c Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C13(H13), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C26(H26), C28(H28), C33(H33), C34(H34), C35(H35), C36(H36), C39(H39), C41(H41), C43(H43), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C81(H81), C82(H82), C83(H83) 4.d Idealised Me refined as rotating group: C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C30(H30A,H30B, H30C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C) ; _shelx_res_checksum 11035 _olex2_submission_special_instructions 'No special instructions were received' _cell_oxdiff_length_a 12.0019(6) _cell_oxdiff_length_b 13.7239(7) _cell_oxdiff_length_c 15.1796(9) _cell_oxdiff_angle_alpha 77.885(5) _cell_oxdiff_angle_beta 68.693(5) _cell_oxdiff_angle_gamma 70.190(5) _cell_oxdiff_volume 2180.8(2) _cell_oxdiff_measurement_reflns_used 5944 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Ta Ta 0.93120(4) 0.00406(3) 0.11420(3) 0.02598(18) Uani 1 1 d . . P P 0.7152(2) 0.09094(18) 0.22486(19) 0.0266(6) Uani 1 1 d . . N1 N 1.0373(7) -0.0602(6) 0.1945(5) 0.0245(17) Uani 1 1 d . U N2 N 0.9203(7) 0.1594(5) 0.1049(6) 0.0228(18) Uani 1 1 d . U N3 N 0.8376(7) -0.0951(6) 0.1086(5) 0.0211(17) Uani 1 1 d . U C1 C 0.7511(10) 0.1079(7) 0.3265(7) 0.026(2) Uani 1 1 d . . C2 C 0.8657(10) 0.0388(8) 0.3325(7) 0.032(2) Uani 1 1 d . U C3 C 0.9161(11) 0.0527(8) 0.3953(7) 0.037(3) Uani 1 1 d . . H3 H 0.9936 0.0063 0.3998 0.044 Uiso 1 1 calc R . C4 C 0.8547(11) 0.1338(8) 0.4521(8) 0.038(3) Uani 1 1 d . . H4 H 0.8918 0.1453 0.4932 0.046 Uiso 1 1 calc R . C5 C 0.7389(10) 0.1983(7) 0.4485(8) 0.033(3) Uani 1 1 d . . H5 H 0.6953 0.2516 0.4902 0.040 Uiso 1 1 calc R . C6 C 0.6856(10) 0.1877(8) 0.3873(8) 0.035(3) Uani 1 1 d . . H6 H 0.6063 0.2329 0.3856 0.042 Uiso 1 1 calc R . C7 C 0.9159(10) -0.0454(8) 0.2675(7) 0.030(2) Uani 1 1 d . U H7 H 0.8890 -0.1098 0.2950 0.036 Uiso 1 1 calc R . C8 C 1.1448(9) -0.1383(7) 0.2073(7) 0.024(2) Uani 1 1 d . . C9 C 1.2559(10) -0.1552(7) 0.1312(8) 0.030(2) Uani 1 1 d . . H9 H 1.2602 -0.1119 0.0731 0.036 Uiso 1 1 calc R . C10 C 1.3594(10) -0.2348(8) 0.1406(8) 0.034(3) Uani 1 1 d . . C11 C 1.3539(11) -0.2988(8) 0.2246(8) 0.036(3) Uani 1 1 d . . H11 H 1.4259 -0.3539 0.2295 0.043 Uiso 1 1 calc R . C12 C 1.2460(10) -0.2844(7) 0.3015(8) 0.032(3) Uani 1 1 d . . C13 C 1.1387(10) -0.2010(7) 0.2931(7) 0.029(2) Uani 1 1 d . . H13 H 1.0640 -0.1884 0.3456 0.034 Uiso 1 1 calc R . C14 C 1.4784(11) -0.2534(10) 0.0541(9) 0.046(3) Uani 1 1 d . . H14A H 1.4666 -0.2851 0.0072 0.069 Uiso 1 1 calc GR . H14B H 1.5489 -0.3002 0.0744 0.069 Uiso 1 1 calc GR . H14C H 1.4956 -0.1869 0.0256 0.069 Uiso 1 1 calc GR . C15 C 1.2361(11) -0.3585(9) 0.3905(8) 0.042(3) Uani 1 1 d . . H15A H 1.2317 -0.4242 0.3783 0.064 Uiso 1 1 calc GR . H15B H 1.1606 -0.3279 0.4412 0.064 Uiso 1 1 calc GR . H15C H 1.3097 -0.3717 0.4102 0.064 Uiso 1 1 calc GR . C16 C 0.6277(10) 0.2218(8) 0.1903(7) 0.028(2) Uani 1 1 d . . C17 C 0.6965(10) 0.2807(7) 0.1194(7) 0.029(2) Uani 1 1 d . . C18 C 0.6330(10) 0.3829(7) 0.0917(8) 0.031(2) Uani 1 1 d . . H18 H 0.6784 0.4240 0.0430 0.037 Uiso 1 1 calc R . C19 C 0.5074(11) 0.4244(8) 0.1335(8) 0.038(3) Uani 1 1 d . . H19 H 0.4663 0.4936 0.1141 0.046 Uiso 1 1 calc R . C20 C 0.4400(11) 0.3637(9) 0.2051(9) 0.039(3) Uani 1 1 d . . H20 H 0.3528 0.3913 0.2346 0.047 Uiso 1 1 calc R . C21 C 0.5018(10) 0.2629(7) 0.2326(8) 0.029(2) Uani 1 1 d . . H21 H 0.4564 0.2218 0.2814 0.035 Uiso 1 1 calc R . C22 C 0.8344(9) 0.2433(7) 0.0610(7) 0.026(2) Uani 1 1 d . U H22A H 0.8390 0.2193 0.0024 0.031 Uiso 1 1 calc R . H22B H 0.8673 0.3044 0.0414 0.031 Uiso 1 1 calc R . C23 C 0.9831(11) 0.1962(8) 0.1500(8) 0.037(3) Uani 1 1 d . . C24 C 1.1092(10) 0.1468(8) 0.1375(8) 0.037(3) Uani 1 1 d . . H24 H 1.1523 0.0906 0.0991 0.044 Uiso 1 1 calc R . C25 C 1.1718(9) 0.1796(8) 0.1810(7) 0.030(2) Uani 1 1 d . . C26 C 1.1052(11) 0.2621(8) 0.2387(8) 0.039(3) Uani 1 1 d . . H26 H 1.1474 0.2845 0.2693 0.047 Uiso 1 1 calc R . C27 C 0.9807(12) 0.3111(8) 0.2517(9) 0.040(3) Uani 1 1 d . . C28 C 0.9177(11) 0.2789(6) 0.2059(7) 0.029(2) Uani 1 1 d . . H28 H 0.8321 0.3131 0.2130 0.035 Uiso 1 1 calc R . C29 C 1.3077(11) 0.1272(10) 0.1687(9) 0.049(3) Uani 1 1 d . . H29A H 1.3175 0.0927 0.2300 0.074 Uiso 1 1 calc GR . H29B H 1.3537 0.1793 0.1451 0.074 Uiso 1 1 calc GR . H29C H 1.3406 0.0755 0.1229 0.074 Uiso 1 1 calc GR . C30 C 0.9079(12) 0.3956(9) 0.3165(9) 0.047(3) Uani 1 1 d . . H30A H 0.8691 0.3651 0.3801 0.070 Uiso 1 1 calc GR . H30B H 0.8427 0.4454 0.2919 0.070 Uiso 1 1 calc GR . H30C H 0.9640 0.4315 0.3197 0.070 Uiso 1 1 calc GR . C31 C 0.6040(10) 0.0159(8) 0.2647(8) 0.035(3) Uani 1 1 d . . C32 C 0.6130(9) -0.0465(7) 0.1983(7) 0.027(2) Uani 1 1 d . . C33 C 0.5307(10) -0.1072(7) 0.2262(8) 0.032(2) Uani 1 1 d . . H33 H 0.5344 -0.1498 0.1827 0.039 Uiso 1 1 calc R . C34 C 0.4436(11) -0.1064(9) 0.3165(8) 0.041(3) Uani 1 1 d . . H34 H 0.3876 -0.1474 0.3340 0.049 Uiso 1 1 calc R . C35 C 0.4382(10) -0.0468(9) 0.3803(8) 0.039(3) Uani 1 1 d . . H35 H 0.3793 -0.0477 0.4423 0.047 Uiso 1 1 calc R . C36 C 0.5171(10) 0.0149(8) 0.3561(8) 0.035(3) Uani 1 1 d . . H36 H 0.5125 0.0562 0.4010 0.042 Uiso 1 1 calc R . C37 C 0.7100(9) -0.0472(7) 0.1005(7) 0.023(2) Uani 1 1 d . . H37A H 0.678(9) -0.081(7) 0.061(7) 0.027 Uiso 1 1 d R . H37B H 0.700(9) 0.029(8) 0.066(7) 0.027 Uiso 1 1 d R . C38 C 0.8759(9) -0.2042(7) 0.1163(7) 0.022(2) Uani 1 1 d . U C39 C 0.8181(10) -0.2655(8) 0.0939(8) 0.033(2) Uani 1 1 d . . H39 H 0.7460 -0.2321 0.0747 0.039 Uiso 1 1 calc R . C40 C 0.8638(11) -0.3732(8) 0.0990(8) 0.037(3) Uani 1 1 d . . C41 C 0.9694(10) -0.4245(7) 0.1276(7) 0.029(2) Uani 1 1 d . . H41 H 1.0019 -0.4981 0.1295 0.035 Uiso 1 1 calc R . C42 C 1.0261(9) -0.3672(8) 0.1532(8) 0.029(2) Uani 1 1 d . . C43 C 0.9765(9) -0.2590(7) 0.1491(7) 0.028(2) Uani 1 1 d . . H43 H 1.0135 -0.2208 0.1699 0.033 Uiso 1 1 calc R . C44 C 0.7959(12) -0.4347(9) 0.0734(10) 0.054(4) Uani 1 1 d . . H44A H 0.7165 -0.4335 0.1240 0.080 Uiso 1 1 calc GR . H44B H 0.8482 -0.5069 0.0665 0.080 Uiso 1 1 calc GR . H44C H 0.7798 -0.4030 0.0134 0.080 Uiso 1 1 calc GR . C45 C 1.1372(11) -0.4210(8) 0.1864(9) 0.041(3) Uani 1 1 d . . H45A H 1.1133 -0.4163 0.2547 0.062 Uiso 1 1 calc GR . H45B H 1.2035 -0.3876 0.1520 0.062 Uiso 1 1 calc GR . H45C H 1.1676 -0.4943 0.1742 0.062 Uiso 1 1 calc GR . C51 C 0.8690(13) 0.6114(10) 0.4613(9) 0.056(4) Uani 1 1 d . . H51 H 0.9151 0.5398 0.4602 0.067 Uiso 1 1 calc R . C52 C 0.8173(10) 0.6611(9) 0.3915(8) 0.039(3) Uani 1 1 d . . H52 H 0.8293 0.6245 0.3406 0.047 Uiso 1 1 calc R . C53 C 0.7474(12) 0.7646(9) 0.3943(9) 0.049(3) Uani 1 1 d . . H53 H 0.7093 0.7986 0.3467 0.059 Uiso 1 1 calc R . C54 C 0.7337(12) 0.8180(8) 0.4673(8) 0.046(3) Uani 1 1 d . . H54 H 0.6862 0.8892 0.4696 0.055 Uiso 1 1 calc R . C55 C 0.7881(13) 0.7690(9) 0.5360(9) 0.053(3) Uani 1 1 d . . H55 H 0.7804 0.8063 0.5850 0.063 Uiso 1 1 calc R . C56 C 0.8536(16) 0.6662(12) 0.5336(11) 0.079(5) Uani 1 1 d . . H56 H 0.8892 0.6316 0.5824 0.094 Uiso 1 1 calc R . C81 C 0.5702(12) 0.5492(9) 0.4203(10) 0.091(5) Uani 1 1 d D U H81 H 0.6186 0.5826 0.3659 0.109 Uiso 1 1 calc R . C82 C 0.5395(15) 0.5799(11) 0.5096(10) 0.103(6) Uani 1 1 d D U H82 H 0.5662 0.6350 0.5162 0.123 Uiso 1 1 calc R . C83 C 0.4698(13) 0.5306(10) 0.5894(10) 0.100(6) Uani 1 1 d D U H83 H 0.4496 0.5514 0.6506 0.120 Uiso 1 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta 0.0273(3) 0.0191(3) 0.0339(3) -0.00487(19) -0.0131(2) -0.0046(2) P 0.0260(15) 0.0182(12) 0.0371(15) -0.0061(11) -0.0113(12) -0.0048(11) N1 0.013(4) 0.035(4) 0.021(4) -0.002(3) 0.000(3) -0.008(3) N2 0.021(4) 0.016(4) 0.034(5) 0.015(3) -0.021(4) -0.007(3) N3 0.018(4) 0.023(4) 0.019(4) 0.003(3) -0.010(3) 0.000(3) C1 0.031(6) 0.027(5) 0.027(5) -0.003(4) -0.005(5) -0.020(5) C2 0.038(6) 0.033(5) 0.026(5) -0.006(4) -0.008(4) -0.012(4) C3 0.046(8) 0.039(6) 0.029(6) -0.004(5) -0.016(5) -0.011(5) C4 0.051(8) 0.030(6) 0.049(7) -0.001(5) -0.027(6) -0.019(5) C5 0.030(7) 0.021(5) 0.046(7) -0.014(5) -0.007(5) -0.002(5) C6 0.034(7) 0.027(5) 0.053(7) -0.011(5) -0.017(6) -0.010(5) C7 0.030(5) 0.032(5) 0.033(5) -0.001(4) -0.014(4) -0.012(4) C8 0.020(6) 0.019(5) 0.035(6) -0.010(4) -0.009(5) -0.005(4) C9 0.034(7) 0.021(5) 0.043(6) -0.003(4) -0.023(5) -0.006(4) C10 0.031(7) 0.029(5) 0.048(7) -0.010(5) -0.022(6) -0.004(5) C11 0.036(7) 0.020(5) 0.056(8) -0.012(5) -0.026(6) 0.004(5) C12 0.036(7) 0.017(5) 0.051(7) -0.009(5) -0.020(6) -0.007(5) C13 0.033(6) 0.016(5) 0.035(6) -0.004(4) -0.013(5) 0.000(4) C14 0.031(7) 0.054(7) 0.062(8) -0.021(6) -0.021(6) -0.008(6) C15 0.041(8) 0.041(6) 0.042(7) 0.001(5) -0.016(6) -0.009(6) C16 0.030(7) 0.028(5) 0.032(6) -0.005(4) -0.011(5) -0.013(5) C17 0.032(6) 0.030(5) 0.039(6) -0.013(5) -0.025(5) -0.005(5) C18 0.021(6) 0.023(5) 0.044(6) -0.011(5) -0.010(5) 0.005(4) C19 0.051(8) 0.025(5) 0.049(7) -0.003(5) -0.032(6) -0.007(5) C20 0.023(7) 0.043(6) 0.054(8) -0.023(6) -0.011(6) -0.002(5) C21 0.033(7) 0.017(5) 0.037(6) 0.001(4) -0.013(5) -0.007(4) C22 0.025(5) 0.019(4) 0.034(5) -0.006(4) -0.007(4) -0.005(4) C23 0.044(8) 0.031(6) 0.054(7) 0.002(5) -0.026(6) -0.024(5) C24 0.032(7) 0.039(6) 0.045(7) -0.019(5) -0.015(6) -0.006(5) C25 0.021(6) 0.043(6) 0.031(6) -0.003(5) -0.013(5) -0.010(5) C26 0.038(7) 0.039(6) 0.054(8) -0.007(5) -0.018(6) -0.021(6) C27 0.059(9) 0.020(5) 0.051(7) -0.010(5) -0.027(7) -0.008(5) C28 0.049(7) 0.007(4) 0.040(6) 0.000(4) -0.023(5) -0.010(4) C29 0.038(8) 0.058(8) 0.061(9) -0.014(7) -0.014(6) -0.022(6) C30 0.066(9) 0.035(6) 0.045(7) -0.010(5) -0.016(7) -0.021(6) C31 0.031(7) 0.026(5) 0.055(7) -0.011(5) -0.025(6) -0.002(5) C32 0.022(6) 0.022(5) 0.033(6) -0.006(4) -0.010(5) 0.000(4) C33 0.033(7) 0.025(5) 0.045(7) -0.013(5) -0.019(5) -0.005(5) C34 0.035(7) 0.045(7) 0.042(7) -0.023(6) 0.006(5) -0.020(6) C35 0.031(7) 0.043(6) 0.044(7) -0.003(5) 0.001(5) -0.025(5) C36 0.036(7) 0.024(5) 0.038(6) -0.013(5) -0.006(5) 0.001(5) C37 0.013(5) 0.022(5) 0.031(5) -0.011(4) 0.001(4) -0.006(4) C38 0.023(5) 0.015(4) 0.025(5) 0.005(3) -0.005(4) -0.008(3) C39 0.028(6) 0.030(5) 0.039(6) -0.008(5) -0.009(5) -0.007(5) C40 0.041(7) 0.025(5) 0.054(7) -0.008(5) -0.018(6) -0.016(5) C41 0.029(6) 0.020(5) 0.041(6) -0.006(4) -0.013(5) -0.007(4) C42 0.017(6) 0.028(5) 0.040(6) -0.009(5) -0.008(5) -0.003(4) C43 0.018(6) 0.025(5) 0.047(6) -0.015(5) -0.007(5) -0.013(4) C44 0.052(9) 0.039(7) 0.095(11) -0.023(7) -0.041(8) -0.015(6) C45 0.041(8) 0.028(6) 0.060(8) -0.002(5) -0.019(6) -0.014(5) C51 0.065(10) 0.043(7) 0.048(8) -0.007(6) -0.026(7) 0.008(7) C52 0.033(7) 0.047(7) 0.038(7) -0.023(6) 0.003(5) -0.017(6) C53 0.057(9) 0.039(7) 0.058(8) -0.010(6) -0.022(7) -0.014(6) C54 0.055(9) 0.024(6) 0.044(7) -0.008(5) -0.005(6) -0.001(5) C55 0.067(10) 0.040(7) 0.047(8) -0.013(6) -0.023(7) 0.000(6) C56 0.099(13) 0.070(10) 0.068(10) -0.019(8) -0.059(10) 0.017(9) C81 0.027(8) 0.028(7) 0.203(16) -0.001(8) -0.035(9) 0.002(6) C82 0.045(10) 0.044(9) 0.207(16) -0.010(8) -0.032(9) -0.009(7) C83 0.037(9) 0.045(8) 0.203(16) -0.014(8) -0.031(9) -0.001(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -5.7959 5.2718 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -7 -6 0 0.0437 -7.0040 -5.9961 -0.0019 -0.0799 0.8327 0.6440 -2 3 -9 0.0223 -1.9859 3.0041 -9.0012 1.0319 -0.2606 -0.0177 2 5 9 0.0447 1.9912 4.9891 9.0017 -0.7246 -0.5376 0.4496 -4 0 6 0.0451 -4.0081 -0.0054 5.9997 -0.4964 0.1525 0.8572 6 -3 2 0.0367 5.9954 -2.9979 2.0014 -0.4384 0.1050 -0.8902 -5 4 2 0.0468 -5.0001 3.9941 1.9993 0.0671 -0.2256 1.0087 5 -4 -2 0.0468 5.0001 -3.9941 -1.9993 -0.0671 0.2256 -1.0087 7 6 0 0.0437 7.0040 5.9961 0.0019 0.0799 -0.8327 -0.6440 2 -3 9 0.0223 1.9859 -3.0041 9.0012 -1.0319 0.2606 0.0177 -3 -9 -4 0.0625 -3.0008 -8.9943 -4.0030 0.1070 0.9862 -0.2741 2 9 1 0.0596 2.0034 8.9936 1.0010 0.2057 -0.9619 0.2603 7 2 6 0.0302 6.9933 1.9949 6.0024 -0.6562 -0.4148 -0.5558 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 P Ta Ta 137.04(6) . 2_755 N1 Ta Ta 116.4(2) . 2_755 N1 Ta P 106.2(2) . . N1 Ta N2 101.6(3) . . N1 Ta N3 111.2(3) . . N1 Ta C7 39.9(3) . . N2 Ta Ta 92.0(2) . 2_755 N2 Ta P 73.7(2) . . N2 Ta C7 101.1(3) . . N3 Ta Ta 88.1(2) . 2_755 N3 Ta P 81.5(2) . . N3 Ta N2 143.3(3) . . N3 Ta C7 94.0(3) . . C7 Ta Ta 154.6(3) . 2_755 C7 Ta P 68.1(3) . . C1 P Ta 102.4(3) . . C1 P C16 103.6(4) . . C16 P Ta 120.0(4) . . C31 P Ta 115.8(4) . . C31 P C1 109.3(5) . . C31 P C16 104.8(5) . . C7 N1 Ta 80.9(5) . . C8 N1 Ta 147.4(7) . . C8 N1 C7 121.9(8) . . C22 N2 Ta 122.3(6) . . C23 N2 Ta 123.1(6) . . C23 N2 C22 114.3(7) . . C37 N3 Ta 117.3(5) . . C38 N3 Ta 128.4(6) . . C38 N3 C37 114.1(7) . . C2 C1 P 112.2(7) . . C2 C1 C6 120.4(9) . . C6 C1 P 126.9(8) . . C1 C2 C7 112.4(9) . . C3 C2 C1 119.2(10) . . C3 C2 C7 128.3(10) . . C2 C3 H3 119.8 . . C2 C3 C4 120.4(11) . . C4 C3 H3 119.8 . . C3 C4 H4 120.2 . . C3 C4 C5 119.5(10) . . C5 C4 H4 120.2 . . C4 C5 H5 119.0 . . C6 C5 C4 122.0(10) . . C6 C5 H5 119.0 . . C1 C6 H6 120.9 . . C5 C6 C1 118.2(10) . . C5 C6 H6 120.9 . . Ta C7 H7 115.6 . . N1 C7 Ta 59.2(5) . . N1 C7 C2 121.5(9) . . N1 C7 H7 115.6 . . C2 C7 Ta 117.3(7) . . C2 C7 H7 115.6 . . C9 C8 N1 119.1(9) . . C13 C8 N1 120.7(9) . . C13 C8 C9 120.1(9) . . C8 C9 H9 120.0 . . C10 C9 C8 119.9(10) . . C10 C9 H9 120.0 . . C9 C10 C11 120.5(11) . . C9 C10 C14 118.3(10) . . C11 C10 C14 121.1(10) . . C10 C11 H11 119.3 . . C12 C11 C10 121.3(10) . . C12 C11 H11 119.3 . . C11 C12 C13 118.7(10) . . C11 C12 C15 121.6(9) . . C13 C12 C15 119.6(10) . . C8 C13 C12 119.4(10) . . C8 C13 H13 120.3 . . C12 C13 H13 120.3 . . C10 C14 H14A 109.5 . . C10 C14 H14B 109.5 . . C10 C14 H14C 109.5 . . H14A C14 H14B 109.5 . . H14A C14 H14C 109.5 . . H14B C14 H14C 109.5 . . C12 C15 H15A 109.5 . . C12 C15 H15B 109.5 . . C12 C15 H15C 109.5 . . H15A C15 H15B 109.5 . . H15A C15 H15C 109.5 . . H15B C15 H15C 109.5 . . C17 C16 P 116.2(8) . . C21 C16 P 123.0(8) . . C21 C16 C17 120.7(9) . . C16 C17 C18 118.1(10) . . C16 C17 C22 126.6(9) . . C18 C17 C22 115.0(9) . . C17 C18 H18 119.2 . . C19 C18 C17 121.5(11) . . C19 C18 H18 119.2 . . C18 C19 H19 120.3 . . C18 C19 C20 119.3(10) . . C20 C19 H19 120.3 . . C19 C20 H20 120.2 . . C21 C20 C19 119.5(11) . . C21 C20 H20 120.2 . . C16 C21 C20 120.8(10) . . C16 C21 H21 119.6 . . C20 C21 H21 119.6 . . N2 C22 C17 118.7(8) . . N2 C22 H22A 107.6 . . N2 C22 H22B 107.6 . . C17 C22 H22A 107.6 . . C17 C22 H22B 107.6 . . H22A C22 H22B 107.1 . . C24 C23 N2 118.7(10) . . C24 C23 C28 121.1(9) . . C28 C23 N2 120.2(10) . . C23 C24 H24 120.0 . . C25 C24 C23 120.1(10) . . C25 C24 H24 120.0 . . C24 C25 C26 118.8(10) . . C24 C25 C29 120.9(10) . . C26 C25 C29 120.3(9) . . C25 C26 H26 119.2 . . C27 C26 C25 121.6(10) . . C27 C26 H26 119.2 . . C26 C27 C28 119.5(10) . . C26 C27 C30 121.9(10) . . C28 C27 C30 118.6(11) . . C23 C28 C27 119.0(10) . . C23 C28 H28 120.5 . . C27 C28 H28 120.5 . . C25 C29 H29A 109.5 . . C25 C29 H29B 109.5 . . C25 C29 H29C 109.5 . . H29A C29 H29B 109.5 . . H29A C29 H29C 109.5 . . H29B C29 H29C 109.5 . . C27 C30 H30A 109.5 . . C27 C30 H30B 109.5 . . C27 C30 H30C 109.5 . . H30A C30 H30B 109.5 . . H30A C30 H30C 109.5 . . H30B C30 H30C 109.5 . . C32 C31 P 115.4(9) . . C36 C31 P 123.8(8) . . C36 C31 C32 120.7(10) . . C31 C32 C37 120.3(9) . . C33 C32 C31 117.6(10) . . C33 C32 C37 122.0(9) . . C32 C33 H33 119.4 . . C34 C33 C32 121.1(9) . . C34 C33 H33 119.4 . . C33 C34 H34 119.9 . . C35 C34 C33 120.2(10) . . C35 C34 H34 119.9 . . C34 C35 H35 119.5 . . C34 C35 C36 121.0(11) . . C36 C35 H35 119.5 . . C31 C36 H36 120.3 . . C35 C36 C31 119.4(10) . . C35 C36 H36 120.3 . . N3 C37 C32 110.0(8) . . N3 C37 H37A 120(5) . . N3 C37 H37B 111(5) . . C32 C37 H37A 103(5) . . C32 C37 H37B 111(5) . . H37A C37 H37B 101(7) . . N3 C38 C39 124.6(8) . . C43 C38 N3 119.8(8) . . C43 C38 C39 115.7(8) . . C38 C39 H39 119.1 . . C40 C39 C38 121.8(10) . . C40 C39 H39 119.1 . . C39 C40 C41 120.3(9) . . C39 C40 C44 118.8(10) . . C41 C40 C44 120.8(9) . . C40 C41 H41 120.3 . . C42 C41 C40 119.5(9) . . C42 C41 H41 120.3 . . C41 C42 C43 118.9(9) . . C41 C42 C45 120.2(9) . . C43 C42 C45 120.9(9) . . C38 C43 C42 123.6(8) . . C38 C43 H43 118.2 . . C42 C43 H43 118.2 . . C40 C44 H44A 109.5 . . C40 C44 H44B 109.5 . . C40 C44 H44C 109.5 . . H44A C44 H44B 109.5 . . H44A C44 H44C 109.5 . . H44B C44 H44C 109.5 . . C42 C45 H45A 109.5 . . C42 C45 H45B 109.5 . . C42 C45 H45C 109.5 . . H45A C45 H45B 109.5 . . H45A C45 H45C 109.5 . . H45B C45 H45C 109.5 . . C52 C51 H51 120.4 . . C52 C51 C56 119.3(12) . . C56 C51 H51 120.4 . . C51 C52 H52 119.8 . . C51 C52 C53 120.4(11) . . C53 C52 H52 119.8 . . C52 C53 H53 120.4 . . C52 C53 C54 119.2(12) . . C54 C53 H53 120.4 . . C53 C54 H54 119.8 . . C55 C54 C53 120.4(11) . . C55 C54 H54 119.8 . . C54 C55 H55 120.3 . . C56 C55 C54 119.5(12) . . C56 C55 H55 120.3 . . C51 C56 H56 119.4 . . C55 C56 C51 121.1(12) . . C55 C56 H56 119.4 . . C82 C81 H81 120.1 . . C82 C81 C83 119.9(9) . 2_666 C83 C81 H81 120.1 2_666 . C81 C82 H82 119.9 . . C81 C82 C83 120.2(9) . . C83 C82 H82 119.9 . . C81 C83 C82 119.9(9) 2_666 . C81 C83 H83 120.1 2_666 . C82 C83 H83 120.1 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ta Ta 3.2613(10) 2_755 Ta P 2.558(3) . Ta N1 1.950(8) . Ta N2 2.069(7) . Ta N3 2.068(8) . Ta C7 2.240(10) . P C1 1.823(10) . P C16 1.825(10) . P C31 1.815(11) . N1 C7 1.454(13) . N1 C8 1.417(12) . N2 C22 1.485(11) . N2 C23 1.438(12) . N3 C37 1.488(12) . N3 C38 1.402(11) . C1 C2 1.403(15) . C1 C6 1.408(14) . C2 C3 1.373(14) . C2 C7 1.498(14) . C3 H3 0.9500 . C3 C4 1.382(15) . C4 H4 0.9500 . C4 C5 1.386(15) . C5 H5 0.9500 . C5 C6 1.359(14) . C6 H6 0.9500 . C7 H7 1.0000 . C8 C9 1.396(14) . C8 C13 1.395(13) . C9 H9 0.9500 . C9 C10 1.378(14) . C10 C11 1.382(15) . C10 C14 1.536(16) . C11 H11 0.9500 . C11 C12 1.380(16) . C12 C13 1.429(14) . C12 C15 1.504(15) . C13 H13 0.9500 . C14 H14A 0.9800 . C14 H14B 0.9800 . C14 H14C 0.9800 . C15 H15A 0.9800 . C15 H15B 0.9800 . C15 H15C 0.9800 . C16 C17 1.391(15) . C16 C21 1.372(14) . C17 C18 1.410(13) . C17 C22 1.529(14) . C18 H18 0.9500 . C18 C19 1.369(15) . C19 H19 0.9500 . C19 C20 1.403(16) . C20 H20 0.9500 . C20 C21 1.387(14) . C21 H21 0.9500 . C22 H22A 0.9900 . C22 H22B 0.9900 . C23 C24 1.391(15) . C23 C28 1.393(15) . C24 H24 0.9500 . C24 C25 1.385(13) . C25 C26 1.409(15) . C25 C29 1.500(15) . C26 H26 0.9500 . C26 C27 1.372(16) . C27 C28 1.410(14) . C27 C30 1.497(15) . C28 H28 0.9500 . C29 H29A 0.9800 . C29 H29B 0.9800 . C29 H29C 0.9800 . C30 H30A 0.9800 . C30 H30B 0.9800 . C30 H30C 0.9800 . C31 C32 1.408(14) . C31 C36 1.400(15) . C32 C33 1.399(14) . C32 C37 1.517(14) . C33 H33 0.9500 . C33 C34 1.389(15) . C34 H34 0.9500 . C34 C35 1.364(15) . C35 H35 0.9500 . C35 C36 1.381(14) . C36 H36 0.9500 . C37 H37A 1.07(10) . C37 H37B 1.06(10) . C38 C39 1.411(13) . C38 C43 1.392(13) . C39 H39 0.9500 . C39 C40 1.387(14) . C40 C41 1.399(14) . C40 C44 1.537(13) . C41 H41 0.9500 . C41 C42 1.384(13) . C42 C43 1.397(13) . C42 C45 1.498(14) . C43 H43 0.9500 . C44 H44A 0.9800 . C44 H44B 0.9800 . C44 H44C 0.9800 . C45 H45A 0.9800 . C45 H45B 0.9800 . C45 H45C 0.9800 . C51 H51 0.9500 . C51 C52 1.364(16) . C51 C56 1.381(18) . C52 H52 0.9500 . C52 C53 1.383(16) . C53 H53 0.9500 . C53 C54 1.385(16) . C54 H54 0.9500 . C54 C55 1.368(16) . C55 H55 0.9500 . C55 C56 1.364(17) . C56 H56 0.9500 . C81 H81 0.9500 . C81 C82 1.387(11) . C81 C83 1.389(11) 2_666 C82 H82 0.9500 . C82 C83 1.389(11) . C83 C81 1.389(11) 2_666 C83 H83 0.9500 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 Ta P C1 C2 -22.4(8) . . Ta P C1 C6 149.3(9) . . Ta P C16 C17 -18.9(8) . . Ta P C16 C21 163.0(7) . . Ta P C31 C32 -34.6(9) . . Ta P C31 C36 143.0(8) . . Ta N1 C7 C2 -105.1(9) . . Ta N1 C8 C9 44.9(16) . . Ta N1 C8 C13 -132.1(11) . . Ta N2 C22 C17 79.6(10) . . Ta N2 C23 C24 49.3(13) . . Ta N2 C23 C28 -129.9(9) . . Ta N3 C37 C32 -94.7(8) . . Ta N3 C38 C39 -167.3(8) . . Ta N3 C38 C43 13.5(13) . . P C1 C2 C3 169.3(8) . . P C1 C2 C7 -12.2(11) . . P C1 C6 C5 -168.3(8) . . P C16 C17 C18 -178.9(7) . . P C16 C17 C22 6.7(12) . . P C16 C21 C20 178.6(8) . . P C31 C32 C33 178.9(7) . . P C31 C32 C37 -0.6(12) . . P C31 C36 C35 -178.5(8) . . N1 C8 C9 C10 -176.3(8) . . N1 C8 C13 C12 175.1(8) . . N2 C23 C24 C25 -179.2(10) . . N2 C23 C28 C27 177.9(9) . . N3 C38 C39 C40 177.1(10) . . N3 C38 C43 C42 -175.6(9) . . C1 P C16 C17 94.3(8) . . C1 P C16 C21 -83.7(9) . . C1 P C31 C32 -149.5(7) . . C1 P C31 C36 28.0(10) . . C1 C2 C3 C4 0.0(17) . . C1 C2 C7 Ta 52.4(11) . . C1 C2 C7 N1 121.4(10) . . C2 C1 C6 C5 2.7(16) . . C2 C3 C4 C5 3.1(17) . . C3 C2 C7 Ta -129.3(10) . . C3 C2 C7 N1 -60.3(15) . . C3 C4 C5 C6 -3.3(17) . . C4 C5 C6 C1 0.4(17) . . C6 C1 C2 C3 -2.9(16) . . C6 C1 C2 C7 175.6(9) . . C7 N1 C8 C9 173.8(8) . . C7 N1 C8 C13 -3.2(13) . . C7 C2 C3 C4 -178.2(11) . . C8 N1 C7 Ta -154.9(9) . . C8 N1 C7 C2 100.0(11) . . C8 C9 C10 C11 0.6(14) . . C8 C9 C10 C14 177.8(8) . . C9 C8 C13 C12 -1.8(13) . . C9 C10 C11 C12 -0.8(15) . . C10 C11 C12 C13 -0.3(14) . . C10 C11 C12 C15 175.3(10) . . C11 C12 C13 C8 1.6(14) . . C13 C8 C9 C10 0.8(13) . . C14 C10 C11 C12 -177.9(9) . . C15 C12 C13 C8 -174.1(9) . . C16 P C1 C2 -147.8(7) . . C16 P C1 C6 23.8(10) . . C16 P C31 C32 100.0(8) . . C16 P C31 C36 -82.4(10) . . C16 C17 C18 C19 0.6(14) . . C16 C17 C22 N2 -30.0(13) . . C17 C16 C21 C20 0.7(15) . . C17 C18 C19 C20 -0.3(15) . . C18 C17 C22 N2 155.4(8) . . C18 C19 C20 C21 0.2(15) . . C19 C20 C21 C16 -0.3(15) . . C21 C16 C17 C18 -0.8(14) . . C21 C16 C17 C22 -175.2(9) . . C22 N2 C23 C24 -137.9(10) . . C22 N2 C23 C28 42.9(13) . . C22 C17 C18 C19 175.7(9) . . C23 N2 C22 C17 -93.3(10) . . C23 C24 C25 C26 1.0(17) . . C23 C24 C25 C29 179.8(11) . . C24 C23 C28 C27 -1.2(16) . . C24 C25 C26 C27 -0.7(17) . . C25 C26 C27 C28 -0.5(17) . . C25 C26 C27 C30 177.1(11) . . C26 C27 C28 C23 1.5(16) . . C28 C23 C24 C25 0.0(17) . . C29 C25 C26 C27 -179.6(11) . . C30 C27 C28 C23 -176.3(10) . . C31 P C1 C2 100.9(8) . . C31 P C1 C6 -87.5(10) . . C31 P C16 C17 -151.1(7) . . C31 P C16 C21 30.8(10) . . C31 C32 C33 C34 -0.3(15) . . C31 C32 C37 N3 66.9(11) . . C32 C31 C36 C35 -1.1(16) . . C32 C33 C34 C35 -0.9(17) . . C33 C32 C37 N3 -112.6(10) . . C33 C34 C35 C36 1.2(18) . . C34 C35 C36 C31 -0.1(17) . . C36 C31 C32 C33 1.3(14) . . C36 C31 C32 C37 -178.2(9) . . C37 N3 C38 C39 16.2(13) . . C37 N3 C38 C43 -163.0(9) . . C37 C32 C33 C34 179.2(10) . . C38 N3 C37 C32 82.2(9) . . C38 C39 C40 C41 0.5(18) . . C38 C39 C40 C44 -180.0(10) . . C39 C38 C43 C42 5.1(15) . . C39 C40 C41 C42 1.6(17) . . C40 C41 C42 C43 -0.4(16) . . C40 C41 C42 C45 178.4(11) . . C41 C42 C43 C38 -3.2(17) . . C43 C38 C39 C40 -3.7(16) . . C44 C40 C41 C42 -177.9(11) . . C45 C42 C43 C38 178.0(10) . . C51 C52 C53 C54 2(2) . . C52 C51 C56 C55 0(3) . . C52 C53 C54 C55 0(2) . . C53 C54 C55 C56 -2(2) . . C54 C55 C56 C51 2(3) . . C56 C51 C52 C53 -2(2) . . C81 C82 C83 C81 -1(3) . 2_666 C83 C81 C82 C83 1(3) 2_666 .