#------------------------------------------------------------------------------ #$Date: 2015-06-04 14:02:18 +0300 (Thu, 04 Jun 2015) $ #$Revision: 137925 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/34/31/4343172.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_4343172 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 'C48 H52 N3 P2 Ta' _chemical_formula_sum 'C62 H68 N3 P2 Ta' _chemical_formula_weight 1098.08 _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 geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_block_code ba_ms23 _audit_creation_date ; 'Wed Nov 26 11:01:35 2014' ; _audit_creation_method ; Olex2 1.2 (compiled 2014.11.25 svn.r3098 for OlexSys, GUI svn.r4951) ; _audit_update_record '26.11.2014 11:18:46 CET UTC+01:00 encif 1.29' _cell_angle_alpha 72.9853(17) _cell_angle_beta 88.354(2) _cell_angle_gamma 69.0792(18) _cell_formula_units_Z 2 _cell_length_a 11.5569(3) _cell_length_b 14.4348(2) _cell_length_c 17.0151(4) _cell_measurement_reflns_used 51957 _cell_measurement_temperature 120(1) _cell_measurement_theta_max 30.8150 _cell_measurement_theta_min 3.7370 _cell_volume 2526.17(10) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _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_environment 'perfluoro polyether oil / N~2~' _diffrn_ambient_temperature 120(1) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 7.9621 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.930 _diffrn_measurement_details ; 1 omega -30.00 15.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 -38.0000 30.0000 90 2 omega 38.00 65.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 57.0000 120.0000 54 3 omega -44.00 59.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 -80.0000 -115.2592 206 4 omega 8.00 74.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 77.0000 150.0000 132 5 omega -4.00 22.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 80.0000 -7.3301 52 6 omega -24.00 59.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 -80.0000 55.0587 166 7 omega -6.00 61.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 19.0000 -90.0000 134 8 omega 67.00 96.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 77.0000 60.0000 58 9 omega 18.00 45.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 57.0000 -30.0000 54 10 omega 1.00 70.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 38.0000 30.0000 138 11 omega -42.00 57.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 -77.0000 -30.0000 198 12 omega -2.00 96.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 77.0000 -120.0000 196 13 omega 6.00 64.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 57.0000 60.0000 116 14 omega -2.00 53.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 77.0000 90.0000 110 15 omega 62.00 88.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 57.0000 -60.0000 52 16 omega -42.00 -14.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 28.0000 -78.0000 -51.4972 56 17 omega -35.00 59.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 28.0000 -78.0000 119.4231 188 18 omega 33.00 59.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 28.0000 -78.0000 -51.4972 52 19 omega -40.00 60.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 28.0000 -80.0000 -168.7403 200 20 omega 6.00 96.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 57.0000 -90.0000 180 21 omega -3.00 74.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 77.0000 -180.0000 154 22 omega 6.00 96.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 57.0000 60.0000 180 23 omega -42.00 48.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 -57.0000 120.0000 180 24 omega -44.00 59.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 -80.0000 55.0587 206 25 omega -42.00 48.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 -57.0000 -60.0000 180 26 omega -3.00 97.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 77.0000 -60.0000 200 27 omega 6.00 96.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 57.0000 90.0000 180 28 omega 1.00 99.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 38.0000 -90.0000 196 29 omega -3.00 97.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 77.0000 150.0000 200 30 omega -3.00 97.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 77.0000 30.0000 200 31 omega -43.00 57.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 26.8662 -77.0000 -30.0000 200 32 omega -43.00 60.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 28.0000 -80.0000 -168.7403 206 33 omega -42.00 59.00 0.5000 5.0000 omega____ theta____ kappa____ phi______ frames - 28.0000 -78.0000 119.4231 202 ; _diffrn_measurement_device 'four-circle 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 -0.0035751000 _diffrn_orient_matrix_UB_12 -0.0172081000 _diffrn_orient_matrix_UB_13 0.0432297000 _diffrn_orient_matrix_UB_21 0.0282637000 _diffrn_orient_matrix_UB_22 -0.0524164000 _diffrn_orient_matrix_UB_23 -0.0000607000 _diffrn_orient_matrix_UB_31 0.0594723000 _diffrn_orient_matrix_UB_32 0.0015525000 _diffrn_orient_matrix_UB_33 0.0067430000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_unetI/netI 0.0371 _diffrn_reflns_laue_measured_fraction_full 0.998 _diffrn_reflns_laue_measured_fraction_max 0.930 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 156680 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.930 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.861 _diffrn_reflns_theta_min 3.273 _diffrn_source 'microfocus X-Ray tube' _exptl_absorpt_coefficient_mu 2.283 _exptl_absorpt_correction_T_max 0.812 _exptl_absorpt_correction_T_min 0.626 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.444 _exptl_crystal_description block _exptl_crystal_F_000 1128 _exptl_crystal_size_max 0.287 _exptl_crystal_size_mid 0.237 _exptl_crystal_size_min 0.117 _refine_diff_density_max 1.299 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.115 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 496 _refine_ls_number_reflns 17503 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.075 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0331 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+1.4338P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.0846 _reflns_Friedel_coverage 0.000 _reflns_number_gt 15315 _reflns_number_total 17503 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL ba_ms23 - #2274 - in P-1 - superflip - nova CELL 0.71073 11.556949 14.434769 17.015072 72.9853 88.3544 69.0792 ZERR 2 0.000288 0.000214 0.000393 0.0017 0.002 0.0018 LATT 1 SFAC C H N P Ta UNIT 124 136 6 4 2 L.S. 10 0 81 PLAN 25 SIZE 0.1 0.1 0.1 TEMP -153.14 BOND $H CONF HTAB MORE -1 ABIN fmap 2 acta REM REM REM WGHT 0.041600 1.433800 FVAR 3.58002 TA 5 0.799812 0.964507 0.320551 11.00000 0.02060 0.02049 = 0.02583 -0.00786 -0.00085 -0.00733 P1 4 0.860891 1.078171 0.199695 11.00000 0.02394 0.02637 = 0.02548 -0.00655 -0.00215 -0.00873 P2 4 0.800325 0.874974 0.483086 11.00000 0.02622 0.02315 = 0.02951 -0.00538 0.00111 -0.00665 N1 3 0.685183 0.907675 0.278186 11.00000 0.02573 0.03150 = 0.03627 -0.01347 0.00087 -0.01290 N2 3 0.668560 1.097437 0.319275 11.00000 0.02339 0.02353 = 0.02814 -0.00833 0.00304 -0.00759 N3 3 0.991845 0.884145 0.340326 11.00000 0.02187 0.02141 = 0.03137 -0.00715 -0.00190 -0.00804 C1 1 0.743299 1.106922 0.118615 11.00000 0.02586 0.03804 = 0.02462 -0.01135 -0.00206 -0.00640 C2 1 0.689566 1.030433 0.136159 11.00000 0.02449 0.04238 = 0.02729 -0.01751 -0.00014 -0.00843 C3 1 0.585436 1.047152 0.086633 11.00000 0.02977 0.06023 = 0.03478 -0.02281 -0.00002 -0.01575 AFIX 43 H3 2 0.547953 0.996376 0.097094 11.00000 -1.20000 AFIX 0 C4 1 0.536925 1.139240 0.021571 11.00000 0.03270 0.06633 = 0.03907 -0.02168 -0.00604 -0.00958 AFIX 43 H4 2 0.464793 1.151544 -0.011316 11.00000 -1.20000 AFIX 0 C5 1 0.591821 1.212458 0.004286 11.00000 0.04528 0.05154 = 0.03291 -0.00692 -0.01144 -0.00149 AFIX 43 H5 2 0.558635 1.273690 -0.041233 11.00000 -1.20000 AFIX 0 C6 1 0.695218 1.197674 0.052736 11.00000 0.04024 0.04470 = 0.03151 -0.00699 -0.00383 -0.01080 AFIX 43 H6 2 0.732566 1.248603 0.041158 11.00000 -1.20000 AFIX 0 C7 1 0.750767 0.933922 0.208168 11.00000 0.02370 0.03165 = 0.03293 -0.01569 -0.00106 -0.00910 AFIX 13 H7 2 0.813995 0.873880 0.194193 11.00000 -1.20000 AFIX 0 C8 1 0.621152 0.839944 0.296468 11.00000 0.02297 0.02740 = 0.04187 -0.01000 -0.00729 -0.00853 C9 1 0.560735 0.830170 0.369986 11.00000 0.02364 0.03787 = 0.04794 -0.01382 -0.00067 -0.01380 AFIX 43 H9 2 0.560578 0.873157 0.402953 11.00000 -1.20000 AFIX 0 C10 1 0.501229 0.758966 0.395472 11.00000 0.02709 0.04261 = 0.04738 -0.00734 -0.00506 -0.01524 C11 1 0.501353 0.698110 0.345891 11.00000 0.03527 0.03412 = 0.05220 -0.00168 -0.01550 -0.01403 AFIX 43 H11 2 0.461055 0.649355 0.362651 11.00000 -1.20000 AFIX 0 C12 1 0.557924 0.705772 0.273014 11.00000 0.03966 0.03392 = 0.04948 -0.00829 -0.02081 -0.01186 C13 1 0.617741 0.778530 0.247704 11.00000 0.03571 0.03384 = 0.03908 -0.01138 -0.00960 -0.01108 AFIX 43 H13 2 0.655753 0.785442 0.197140 11.00000 -1.20000 AFIX 0 C14 1 0.441570 0.749742 0.475655 11.00000 0.04710 0.07055 = 0.05901 -0.01595 0.01094 -0.03751 AFIX 137 H14A 2 0.490299 0.761646 0.515298 11.00000 -1.50000 H14B 2 0.438638 0.679897 0.497598 11.00000 -1.50000 H14C 2 0.356880 0.801671 0.466343 11.00000 -1.50000 AFIX 0 C15 1 0.559434 0.637055 0.220807 11.00000 0.08145 0.04631 = 0.05990 -0.01624 -0.01622 -0.03232 AFIX 137 H15A 2 0.585024 0.564630 0.255843 11.00000 -1.50000 H15B 2 0.618227 0.642930 0.178674 11.00000 -1.50000 H15C 2 0.476033 0.658966 0.193987 11.00000 -1.50000 AFIX 0 C16 1 0.852477 1.194564 0.223015 11.00000 0.02472 0.02212 = 0.03514 -0.00472 -0.00578 -0.00680 C17 1 0.812328 1.196224 0.301912 11.00000 0.02779 0.01955 = 0.03484 -0.00562 -0.00844 -0.00494 C18 1 0.815503 1.278343 0.329730 11.00000 0.03838 0.02633 = 0.04494 -0.01406 -0.00953 -0.00782 AFIX 43 H18 2 0.789157 1.282046 0.382499 11.00000 -1.20000 AFIX 0 C19 1 0.856847 1.353844 0.280581 11.00000 0.04220 0.02614 = 0.07518 -0.01396 -0.01629 -0.01311 AFIX 43 H19 2 0.858793 1.408300 0.300513 11.00000 -1.20000 AFIX 0 C20 1 0.895503 1.351307 0.202670 11.00000 0.03878 0.02931 = 0.07265 -0.00279 -0.00229 -0.01742 AFIX 43 H20 2 0.923029 1.403697 0.169575 11.00000 -1.20000 AFIX 0 C21 1 0.893268 1.271816 0.174283 11.00000 0.03195 0.02921 = 0.04696 -0.00032 -0.00151 -0.01140 AFIX 43 H21 2 0.919567 1.269319 0.121279 11.00000 -1.20000 AFIX 0 C22 1 0.771187 1.112179 0.354628 11.00000 0.03264 0.02311 = 0.02577 -0.00859 -0.00197 -0.00820 AFIX 13 H22 2 0.771508 1.104898 0.414911 11.00000 -1.20000 AFIX 0 C23 1 0.547400 1.170789 0.296679 11.00000 0.02410 0.02666 = 0.02834 -0.00559 0.00409 -0.00497 C24 1 0.509692 1.265661 0.313412 11.00000 0.03208 0.03177 = 0.04879 -0.01605 0.00544 -0.00668 AFIX 43 H24 2 0.568054 1.283116 0.338558 11.00000 -1.20000 AFIX 0 C25 1 0.386211 1.335670 0.293433 11.00000 0.03596 0.03354 = 0.06621 -0.01916 0.01068 -0.00037 C26 1 0.302138 1.309434 0.256685 11.00000 0.02553 0.03948 = 0.06178 -0.00885 0.00511 -0.00046 AFIX 43 H26 2 0.218295 1.356329 0.243573 11.00000 -1.20000 AFIX 0 C27 1 0.337944 1.216179 0.238697 11.00000 0.02480 0.04030 = 0.04561 -0.00570 0.00264 -0.00644 C28 1 0.460167 1.146613 0.259092 11.00000 0.02674 0.03157 = 0.03392 -0.00799 0.00292 -0.00851 AFIX 43 H28 2 0.484763 1.082120 0.247443 11.00000 -1.20000 AFIX 0 C29 1 0.349666 1.438865 0.311165 11.00000 0.05134 0.05184 = 0.13782 -0.05158 0.00294 0.00331 AFIX 137 H29A 2 0.373939 1.426548 0.369121 11.00000 -1.50000 H29B 2 0.259481 1.475439 0.300201 11.00000 -1.50000 H29C 2 0.391935 1.481369 0.275646 11.00000 -1.50000 AFIX 0 C30 1 0.244572 1.189803 0.198236 11.00000 0.02826 0.06772 = 0.08077 -0.02031 -0.00442 -0.01062 AFIX 137 H30A 2 0.189367 1.169723 0.238963 11.00000 -1.50000 H30B 2 0.288310 1.131892 0.176456 11.00000 -1.50000 H30C 2 0.195342 1.250647 0.152987 11.00000 -1.50000 AFIX 0 C31 1 1.017488 1.023311 0.170227 11.00000 0.02579 0.03208 = 0.03211 -0.01128 0.00437 -0.01327 C32 1 1.111410 0.961367 0.235165 11.00000 0.02629 0.02804 = 0.03634 -0.01119 0.00228 -0.01290 C33 1 1.233341 0.921511 0.215281 11.00000 0.02669 0.04034 = 0.05052 -0.01834 0.00210 -0.01211 AFIX 43 H33 2 1.297817 0.880656 0.258240 11.00000 -1.20000 AFIX 0 C34 1 1.262373 0.940462 0.133665 11.00000 0.03039 0.05897 = 0.05276 -0.02653 0.01224 -0.01530 AFIX 43 H34 2 1.346220 0.913289 0.121275 11.00000 -1.20000 AFIX 0 C35 1 1.170128 0.998300 0.071101 11.00000 0.04230 0.06719 = 0.04377 -0.02563 0.01766 -0.02564 AFIX 43 H35 2 1.189961 1.009938 0.015345 11.00000 -1.20000 AFIX 0 C36 1 1.046498 1.040411 0.089039 11.00000 0.03753 0.05105 = 0.03118 -0.01416 0.00348 -0.01708 AFIX 43 H36 2 0.982765 1.080619 0.045504 11.00000 -1.20000 AFIX 0 C37 1 1.081361 0.937786 0.324767 11.00000 0.02585 0.02646 = 0.03092 -0.00628 -0.00289 -0.01206 AFIX 23 H37A 2 1.158925 0.893547 0.360752 11.00000 -1.20000 H37B 2 1.046226 1.003645 0.338965 11.00000 -1.20000 AFIX 0 C38 1 1.039214 0.774296 0.368874 11.00000 0.01997 0.02233 = 0.03584 -0.00919 0.00226 -0.00672 C39 1 0.975338 0.721049 0.342516 11.00000 0.02631 0.02489 = 0.04558 -0.01406 -0.00074 -0.00822 AFIX 43 H39 2 0.906736 0.759488 0.302137 11.00000 -1.20000 AFIX 0 C40 1 1.009291 0.613483 0.373677 11.00000 0.03104 0.02637 = 0.06168 -0.01881 -0.00076 -0.00996 C41 1 1.110625 0.557410 0.432203 11.00000 0.03008 0.02147 = 0.06689 -0.01099 -0.00095 -0.00698 AFIX 43 H41 2 1.133243 0.484264 0.454955 11.00000 -1.20000 AFIX 0 C42 1 1.179053 0.606528 0.457825 11.00000 0.02392 0.02387 = 0.05323 -0.00697 -0.00193 -0.00505 C43 1 1.142766 0.714576 0.426283 11.00000 0.02324 0.02484 = 0.04470 -0.00907 -0.00182 -0.00877 AFIX 43 H43 2 1.189297 0.748357 0.444131 11.00000 -1.20000 AFIX 0 C44 1 0.939447 0.559143 0.341914 11.00000 0.05169 0.03404 = 0.09223 -0.02385 -0.01418 -0.01768 AFIX 137 H44A 2 0.852592 0.605765 0.325982 11.00000 -1.50000 H44B 2 0.942774 0.495995 0.385318 11.00000 -1.50000 H44C 2 0.977686 0.540434 0.293848 11.00000 -1.50000 AFIX 0 C45 1 1.292333 0.542638 0.518963 11.00000 0.03413 0.02641 = 0.07379 -0.00073 -0.01474 -0.00572 AFIX 137 H45A 2 1.289537 0.473684 0.546494 11.00000 -1.50000 H45B 2 1.292783 0.577826 0.560179 11.00000 -1.50000 H45C 2 1.367861 0.535129 0.489714 11.00000 -1.50000 AFIX 0 C46 1 0.665319 0.937005 0.532426 11.00000 0.03680 0.03879 = 0.04289 -0.01322 0.00909 -0.00489 AFIX 137 H46A 2 0.646173 1.012250 0.515227 11.00000 -1.50000 H46B 2 0.683092 0.909049 0.592471 11.00000 -1.50000 H46C 2 0.593947 0.923137 0.516167 11.00000 -1.50000 AFIX 0 C47 1 0.824481 0.737098 0.524560 11.00000 0.03995 0.02236 = 0.04885 -0.00127 0.00636 -0.00797 AFIX 137 H47A 2 0.762155 0.722289 0.497648 11.00000 -1.50000 H47B 2 0.816414 0.719627 0.584098 11.00000 -1.50000 H47C 2 0.907849 0.695327 0.514208 11.00000 -1.50000 AFIX 0 C48 1 0.925279 0.886248 0.537540 11.00000 0.04024 0.04486 = 0.02973 -0.00890 -0.00575 -0.01432 AFIX 137 H48A 2 1.005146 0.849996 0.518991 11.00000 -1.50000 H48B 2 0.925027 0.854946 0.596980 11.00000 -1.50000 H48C 2 0.913039 0.959881 0.526010 11.00000 -1.50000 AFIX 0 HKLF 4 REM ba_ms23 - #2274 - in P-1 - superflip - nova REM R1 = 0.0331 for 15315 Fo > 4sig(Fo) and 0.0413 for all 17503 data REM 496 parameters refined using 0 restraints END WGHT 0.0416 1.4337 REM Instructions for potential hydrogen bonds HTAB C28 N1 HTAB C39 N1 REM Highest difference peak 1.299, deepest hole -0.862, 1-sigma level 0.115 Q1 1 0.7877 0.9679 0.2823 11.00000 0.05 1.30 Q2 1 0.7848 1.0290 0.3062 11.00000 0.05 1.01 Q3 1 0.8179 0.9066 0.3321 11.00000 0.05 1.00 Q4 1 0.8435 1.0383 0.2386 11.00000 0.05 0.87 Q5 1 0.7668 0.8675 0.4538 11.00000 0.05 0.87 Q6 1 0.6027 1.0975 0.0373 11.00000 0.05 0.77 Q7 1 0.8985 0.9090 0.2572 11.00000 0.05 0.74 Q8 1 0.7564 0.8988 0.3986 11.00000 0.05 0.74 Q9 1 0.8696 0.9793 0.2494 11.00000 0.05 0.73 Q10 1 0.6414 0.8240 0.2565 11.00000 0.05 0.73 Q11 1 0.7026 1.0229 0.3773 11.00000 0.05 0.71 Q12 1 0.8477 0.8536 0.3429 11.00000 0.05 0.70 Q13 1 0.7397 0.9627 0.3823 11.00000 0.05 0.69 Q14 1 0.6168 0.6899 0.2305 11.00000 0.05 0.64 Q15 1 0.8577 0.9615 0.3133 11.00000 0.05 0.64 Q16 1 0.7790 0.8619 0.4002 11.00000 0.05 0.60 Q17 1 0.6873 1.0890 0.3628 11.00000 0.05 0.58 Q18 1 0.5224 0.7363 0.3582 11.00000 0.05 0.58 Q19 1 0.7476 1.0907 0.3019 11.00000 0.05 0.57 Q20 1 0.9184 0.8628 0.2628 11.00000 0.05 0.57 Q21 1 0.5758 0.8121 0.3289 11.00000 0.05 0.55 Q22 1 0.9397 1.0417 0.1705 11.00000 0.05 0.53 Q23 1 0.6625 0.6287 0.1611 11.00000 0.05 0.53 Q24 1 0.8129 0.7969 0.4932 11.00000 0.05 0.52 Q25 1 0.8627 0.8741 0.5266 11.00000 0.05 0.51 ; _cod_data_source_file ic5b00333_si_001.cif _cod_data_source_block ba_ms23_sq _cod_database_code 4343172 _audit_block_refno 2274 _audit_block_usercomment 'MS374B, block, yellow' _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 0.804 _shelx_estimated_absorpt_t_min 0.804 _shelxl_version_number 2014/6 _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.a Ternary CH refined with riding coordinates: C7(H7), C22(H22) 2.b Secondary CH2 refined with riding coordinates: C37(H37A,H37B) 2.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) 2.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), C46(H46A,H46B,H46C), C47(H47A, H47B,H47C), C48(H48A,H48B,H48C) ; _shelx_res_checksum 96618 _olex2_submission_special_instructions 'No special instructions were received' _cell_oxdiff_length_a 11.5569(3) _cell_oxdiff_length_b 14.4348(2) _cell_oxdiff_length_c 17.0151(4) _cell_oxdiff_angle_alpha 72.9853(17) _cell_oxdiff_angle_beta 88.354(2) _cell_oxdiff_angle_gamma 69.0792(18) _cell_oxdiff_volume 2526.17(9) _cell_oxdiff_measurement_reflns_used 51957 _reflns_odcompleteness_completeness 99.81 _reflns_odcompleteness_theta 26.32 _reflns_odcompleteness_iscentric 1 _platon_squeeze_void_probe_radius 1.20 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 Ta Ta 0.79981(2) 0.96451(2) 0.32055(2) 0.02210(3) Uani 1 1 d . P1 P 0.86089(6) 1.07817(5) 0.19970(4) 0.02559(12) Uani 1 1 d . P2 P 0.80033(6) 0.87497(5) 0.48309(4) 0.02754(13) Uani 1 1 d . N1 N 0.6852(2) 0.90767(17) 0.27819(14) 0.0297(4) Uani 1 1 d . N2 N 0.66856(19) 1.09744(16) 0.31927(13) 0.0252(4) Uani 1 1 d . N3 N 0.99185(18) 0.88414(15) 0.34033(13) 0.0249(4) Uani 1 1 d . C1 C 0.7433(2) 1.1069(2) 0.11861(16) 0.0305(5) Uani 1 1 d . C2 C 0.6896(2) 1.0304(2) 0.13616(16) 0.0308(5) Uani 1 1 d . C3 C 0.5854(3) 1.0472(3) 0.08663(18) 0.0398(7) Uani 1 1 d . H3 H 0.5480 0.9964 0.0971 0.048 Uiso 1 1 calc R C4 C 0.5369(3) 1.1392(3) 0.0216(2) 0.0470(8) Uani 1 1 d . H4 H 0.4648 1.1515 -0.0113 0.056 Uiso 1 1 calc R C5 C 0.5918(3) 1.2125(3) 0.0043(2) 0.0489(8) Uani 1 1 d . H5 H 0.5586 1.2737 -0.0412 0.059 Uiso 1 1 calc R C6 C 0.6952(3) 1.1977(3) 0.05274(18) 0.0411(7) Uani 1 1 d . H6 H 0.7326 1.2486 0.0412 0.049 Uiso 1 1 calc R C7 C 0.7508(2) 0.9339(2) 0.20817(16) 0.0283(5) Uani 1 1 d . H7 H 0.8140 0.8739 0.1942 0.034 Uiso 1 1 calc R C8 C 0.6212(2) 0.8399(2) 0.29647(18) 0.0308(5) Uani 1 1 d . C9 C 0.5607(2) 0.8302(2) 0.36999(19) 0.0355(6) Uani 1 1 d . H9 H 0.5606 0.8732 0.4030 0.043 Uiso 1 1 calc R C10 C 0.5012(3) 0.7590(2) 0.3955(2) 0.0396(6) Uani 1 1 d . C11 C 0.5014(3) 0.6981(2) 0.3459(2) 0.0423(7) Uani 1 1 d . H11 H 0.4611 0.6494 0.3627 0.051 Uiso 1 1 calc R C12 C 0.5579(3) 0.7058(2) 0.2730(2) 0.0419(7) Uani 1 1 d . C13 C 0.6177(3) 0.7785(2) 0.24770(19) 0.0363(6) Uani 1 1 d . H13 H 0.6558 0.7854 0.1971 0.044 Uiso 1 1 calc R C14 C 0.4416(3) 0.7497(3) 0.4757(2) 0.0553(9) Uani 1 1 d . H14A H 0.4903 0.7616 0.5153 0.083 Uiso 1 1 calc GR H14B H 0.4386 0.6799 0.4976 0.083 Uiso 1 1 calc GR H14C H 0.3569 0.8017 0.4663 0.083 Uiso 1 1 calc GR C15 C 0.5594(4) 0.6371(3) 0.2208(2) 0.0594(10) Uani 1 1 d . H15A H 0.5850 0.5646 0.2558 0.089 Uiso 1 1 calc GR H15B H 0.6182 0.6429 0.1787 0.089 Uiso 1 1 calc GR H15C H 0.4760 0.6590 0.1940 0.089 Uiso 1 1 calc GR C16 C 0.8525(2) 1.19456(19) 0.22302(16) 0.0286(5) Uani 1 1 d . C17 C 0.8123(2) 1.19622(18) 0.30191(16) 0.0288(5) Uani 1 1 d . C18 C 0.8155(3) 1.2783(2) 0.32973(19) 0.0367(6) Uani 1 1 d . H18 H 0.7892 1.2820 0.3825 0.044 Uiso 1 1 calc R C19 C 0.8568(3) 1.3538(2) 0.2806(2) 0.0475(8) Uani 1 1 d . H19 H 0.8588 1.4083 0.3005 0.057 Uiso 1 1 calc R C20 C 0.8955(3) 1.3513(2) 0.2027(2) 0.0482(8) Uani 1 1 d . H20 H 0.9230 1.4037 0.1696 0.058 Uiso 1 1 calc R C21 C 0.8933(3) 1.2718(2) 0.1743(2) 0.0384(6) Uani 1 1 d . H21 H 0.9196 1.2693 0.1213 0.046 Uiso 1 1 calc R C22 C 0.7712(2) 1.11218(19) 0.35463(15) 0.0274(5) Uani 1 1 d . H22 H 0.7715 1.1049 0.4149 0.033 Uiso 1 1 calc R C23 C 0.5474(2) 1.1708(2) 0.29668(16) 0.0283(5) Uani 1 1 d . C24 C 0.5097(3) 1.2657(2) 0.3134(2) 0.0381(6) Uani 1 1 d . H24 H 0.5681 1.2831 0.3386 0.046 Uiso 1 1 calc R C25 C 0.3862(3) 1.3357(2) 0.2934(2) 0.0480(8) Uani 1 1 d . C26 C 0.3021(3) 1.3094(3) 0.2567(2) 0.0471(8) Uani 1 1 d . H26 H 0.2183 1.3563 0.2436 0.056 Uiso 1 1 calc R C27 C 0.3379(3) 1.2162(2) 0.2387(2) 0.0401(6) Uani 1 1 d . C28 C 0.4602(2) 1.1466(2) 0.25909(17) 0.0318(5) Uani 1 1 d . H28 H 0.4848 1.0821 0.2474 0.038 Uiso 1 1 calc R C29 C 0.3497(4) 1.4389(3) 0.3112(4) 0.0813(15) Uani 1 1 d . H29A H 0.3739 1.4265 0.3691 0.122 Uiso 1 1 calc GR H29B H 0.2595 1.4754 0.3002 0.122 Uiso 1 1 calc GR H29C H 0.3919 1.4814 0.2756 0.122 Uiso 1 1 calc GR C30 C 0.2446(3) 1.1898(3) 0.1982(3) 0.0612(10) Uani 1 1 d . H30A H 0.1894 1.1697 0.2390 0.092 Uiso 1 1 calc GR H30B H 0.2883 1.1319 0.1765 0.092 Uiso 1 1 calc GR H30C H 0.1953 1.2506 0.1530 0.092 Uiso 1 1 calc GR C31 C 1.0175(2) 1.0233(2) 0.17023(16) 0.0289(5) Uani 1 1 d . C32 C 1.1114(2) 0.9614(2) 0.23517(17) 0.0290(5) Uani 1 1 d . C33 C 1.2333(3) 0.9215(2) 0.2153(2) 0.0381(6) Uani 1 1 d . H33 H 1.2978 0.8807 0.2582 0.046 Uiso 1 1 calc R C34 C 1.2624(3) 0.9405(3) 0.1337(2) 0.0456(7) Uani 1 1 d . H34 H 1.3462 0.9133 0.1213 0.055 Uiso 1 1 calc R C35 C 1.1701(3) 0.9983(3) 0.0711(2) 0.0477(8) Uani 1 1 d . H35 H 1.1900 1.0099 0.0153 0.057 Uiso 1 1 calc R C36 C 1.0465(3) 1.0404(3) 0.08904(18) 0.0393(6) Uani 1 1 d . H36 H 0.9828 1.0806 0.0455 0.047 Uiso 1 1 calc R C37 C 1.0814(2) 0.93779(19) 0.32477(16) 0.0275(5) Uani 1 1 d . H37A H 1.1589 0.8935 0.3608 0.033 Uiso 1 1 calc R H37B H 1.0462 1.0036 0.3390 0.033 Uiso 1 1 calc R C38 C 1.0392(2) 0.77430(18) 0.36887(16) 0.0262(5) Uani 1 1 d . C39 C 0.9753(2) 0.7210(2) 0.34252(18) 0.0317(5) Uani 1 1 d . H39 H 0.9067 0.7595 0.3021 0.038 Uiso 1 1 calc R C40 C 1.0093(3) 0.6135(2) 0.3737(2) 0.0385(6) Uani 1 1 d . C41 C 1.1106(3) 0.5574(2) 0.4322(2) 0.0406(7) Uani 1 1 d . H41 H 1.1332 0.4843 0.4550 0.049 Uiso 1 1 calc R C42 C 1.1791(2) 0.6065(2) 0.4578(2) 0.0357(6) Uani 1 1 d . C43 C 1.1428(2) 0.7146(2) 0.42628(18) 0.0312(5) Uani 1 1 d . H43 H 1.1893 0.7484 0.4441 0.037 Uiso 1 1 calc R C44 C 0.9394(3) 0.5591(3) 0.3419(3) 0.0572(10) Uani 1 1 d . H44A H 0.8526 0.6058 0.3260 0.086 Uiso 1 1 calc GR H44B H 0.9428 0.4960 0.3853 0.086 Uiso 1 1 calc GR H44C H 0.9777 0.5404 0.2938 0.086 Uiso 1 1 calc GR C45 C 1.2923(3) 0.5426(2) 0.5190(2) 0.0492(8) Uani 1 1 d . H45A H 1.2895 0.4737 0.5465 0.074 Uiso 1 1 calc GR H45B H 1.2928 0.5778 0.5602 0.074 Uiso 1 1 calc GR H45C H 1.3679 0.5351 0.4897 0.074 Uiso 1 1 calc GR C46 C 0.6653(3) 0.9370(2) 0.5324(2) 0.0420(7) Uani 1 1 d . H46A H 0.6462 1.0123 0.5152 0.063 Uiso 1 1 calc GR H46B H 0.6831 0.9090 0.5925 0.063 Uiso 1 1 calc GR H46C H 0.5939 0.9231 0.5162 0.063 Uiso 1 1 calc GR C47 C 0.8245(3) 0.7371(2) 0.5246(2) 0.0403(7) Uani 1 1 d . H47A H 0.7622 0.7223 0.4976 0.060 Uiso 1 1 calc GR H47B H 0.8164 0.7196 0.5841 0.060 Uiso 1 1 calc GR H47C H 0.9078 0.6953 0.5142 0.060 Uiso 1 1 calc GR C48 C 0.9253(3) 0.8862(3) 0.53754(18) 0.0390(6) Uani 1 1 d . H48A H 1.0051 0.8500 0.5190 0.058 Uiso 1 1 calc GR H48B H 0.9250 0.8549 0.5970 0.058 Uiso 1 1 calc GR H48C H 0.9130 0.9599 0.5260 0.058 Uiso 1 1 calc GR 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 0.02060(5) 0.02049(5) 0.02583(5) -0.00786(3) -0.00085(3) -0.00733(3) P1 0.0239(3) 0.0264(3) 0.0255(3) -0.0065(2) -0.0022(2) -0.0087(2) P2 0.0262(3) 0.0231(3) 0.0295(3) -0.0054(2) 0.0011(2) -0.0066(2) N1 0.0257(10) 0.0315(11) 0.0363(11) -0.0135(9) 0.0009(8) -0.0129(9) N2 0.0234(9) 0.0235(9) 0.0281(10) -0.0083(8) 0.0030(8) -0.0076(8) N3 0.0219(9) 0.0214(9) 0.0314(10) -0.0071(8) -0.0019(8) -0.0080(7) C1 0.0259(11) 0.0380(13) 0.0246(11) -0.0113(10) -0.0021(9) -0.0064(10) C2 0.0245(11) 0.0424(14) 0.0273(12) -0.0175(11) -0.0001(9) -0.0084(10) C3 0.0298(13) 0.0602(19) 0.0348(14) -0.0228(14) 0.0000(11) -0.0158(13) C4 0.0327(15) 0.066(2) 0.0391(16) -0.0217(15) -0.0060(12) -0.0096(15) C5 0.0453(17) 0.0515(19) 0.0329(15) -0.0069(13) -0.0114(13) -0.0015(15) C6 0.0402(15) 0.0447(16) 0.0315(14) -0.0070(12) -0.0038(12) -0.0108(13) C7 0.0237(11) 0.0316(12) 0.0329(12) -0.0157(10) -0.0011(9) -0.0091(9) C8 0.0230(11) 0.0274(12) 0.0419(14) -0.0100(10) -0.0073(10) -0.0085(9) C9 0.0236(12) 0.0379(14) 0.0479(16) -0.0138(12) -0.0007(11) -0.0138(11) C10 0.0271(13) 0.0426(16) 0.0474(16) -0.0073(13) -0.0051(11) -0.0152(12) C11 0.0353(14) 0.0341(14) 0.0522(18) -0.0017(13) -0.0155(13) -0.0140(12) C12 0.0397(15) 0.0339(14) 0.0495(17) -0.0083(12) -0.0208(13) -0.0119(12) C13 0.0357(14) 0.0338(13) 0.0391(14) -0.0114(11) -0.0096(11) -0.0111(11) C14 0.0471(19) 0.071(2) 0.059(2) -0.0159(18) 0.0109(16) -0.0375(19) C15 0.081(3) 0.0463(19) 0.060(2) -0.0162(17) -0.016(2) -0.0323(19) C16 0.0247(11) 0.0221(11) 0.0351(13) -0.0047(9) -0.0058(9) -0.0068(9) C17 0.0278(11) 0.0196(10) 0.0348(13) -0.0056(9) -0.0084(10) -0.0049(9) C18 0.0384(14) 0.0263(12) 0.0449(16) -0.0141(11) -0.0095(12) -0.0078(11) C19 0.0422(16) 0.0261(13) 0.075(2) -0.0140(14) -0.0163(16) -0.0131(12) C20 0.0388(16) 0.0293(14) 0.073(2) -0.0028(14) -0.0023(15) -0.0174(12) C21 0.0320(13) 0.0292(13) 0.0470(16) -0.0003(11) -0.0015(12) -0.0114(11) C22 0.0326(12) 0.0231(11) 0.0258(11) -0.0086(9) -0.0020(9) -0.0082(9) C23 0.0241(11) 0.0267(11) 0.0283(12) -0.0056(9) 0.0041(9) -0.0050(9) C24 0.0321(13) 0.0318(13) 0.0488(17) -0.0161(12) 0.0054(12) -0.0067(11) C25 0.0360(15) 0.0335(15) 0.066(2) -0.0192(15) 0.0107(15) -0.0004(12) C26 0.0255(13) 0.0395(16) 0.062(2) -0.0088(14) 0.0051(13) -0.0005(12) C27 0.0248(12) 0.0403(15) 0.0456(16) -0.0057(13) 0.0026(11) -0.0064(11) C28 0.0267(12) 0.0316(13) 0.0339(13) -0.0080(10) 0.0029(10) -0.0085(10) C29 0.051(2) 0.052(2) 0.138(5) -0.052(3) 0.003(3) 0.0033(19) C30 0.0283(15) 0.068(2) 0.081(3) -0.020(2) -0.0044(16) -0.0106(16) C31 0.0258(11) 0.0321(12) 0.0321(12) -0.0113(10) 0.0044(9) -0.0133(10) C32 0.0263(11) 0.0280(12) 0.0363(13) -0.0112(10) 0.0023(10) -0.0129(10) C33 0.0267(12) 0.0403(15) 0.0505(17) -0.0183(13) 0.0021(12) -0.0121(11) C34 0.0304(14) 0.059(2) 0.0528(19) -0.0265(16) 0.0122(13) -0.0153(14) C35 0.0423(17) 0.067(2) 0.0438(17) -0.0256(16) 0.0177(14) -0.0256(16) C36 0.0375(15) 0.0510(17) 0.0312(13) -0.0142(12) 0.0035(11) -0.0171(13) C37 0.0259(11) 0.0265(11) 0.0309(12) -0.0063(9) -0.0029(9) -0.0121(9) C38 0.0200(10) 0.0223(10) 0.0358(13) -0.0092(9) 0.0023(9) -0.0067(8) C39 0.0263(12) 0.0249(11) 0.0456(15) -0.0141(11) -0.0007(10) -0.0082(9) C40 0.0310(13) 0.0264(12) 0.0617(19) -0.0188(12) -0.0008(12) -0.0100(10) C41 0.0301(13) 0.0215(12) 0.067(2) -0.0110(12) -0.0009(13) -0.0070(10) C42 0.0239(12) 0.0239(12) 0.0532(17) -0.0070(11) -0.0019(11) -0.0050(9) C43 0.0232(11) 0.0248(11) 0.0447(15) -0.0091(10) -0.0018(10) -0.0088(9) C44 0.052(2) 0.0340(16) 0.092(3) -0.0238(17) -0.0142(19) -0.0177(15) C45 0.0341(15) 0.0264(13) 0.074(2) -0.0007(14) -0.0147(15) -0.0057(11) C46 0.0368(15) 0.0388(15) 0.0429(16) -0.0132(13) 0.0091(12) -0.0049(12) C47 0.0399(15) 0.0224(12) 0.0488(17) -0.0013(11) 0.0064(13) -0.0080(11) C48 0.0402(15) 0.0449(16) 0.0297(13) -0.0089(12) -0.0057(11) -0.0143(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 '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 15 8 8 0.1296 15.0002 8.0058 8.0425 0.1563 0.0038 0.9588 -3 -5 20 0.0489 -3.0337 -5.0068 20.0231 0.9626 0.1755 -0.0532 3 12 -14 0.0870 3.0292 12.0103 -14.0241 -0.8238 -0.5431 0.1042 -12 -12 11 0.1039 -12.0290 -12.0110 10.9949 0.7250 0.2889 -0.6599 16 7 5 0.1293 16.0044 7.0057 5.0427 0.0402 0.0848 0.9967 0 19 2 0.0977 0.0087 19.0119 1.9792 -0.2416 -0.9964 0.0434 -15 -13 -5 0.1240 -15.0076 -13.0094 -5.0326 0.0600 0.2580 -0.9467 -1 -18 3 0.0800 -1.0159 -18.0121 3.0231 0.4443 0.9152 -0.0680 13 -4 6 0.1206 12.9948 -4.0019 6.0491 0.2839 0.5767 0.8074 9 9 21 0.1028 8.9790 9.0036 21.0409 0.7226 -0.2194 0.6899 3 1 -22 0.0522 3.0341 1.0045 -22.0207 -0.9801 0.0344 0.0335 11 5 -17 0.0877 11.0330 5.0073 -16.9968 -0.8604 0.0504 0.5493 -7 -3 20 0.0692 -7.0343 -3.0060 20.0094 0.9419 -0.0425 -0.2881 4 -16 2 0.0937 3.9891 -16.0101 2.0334 0.3491 0.9518 0.2261 -2 0 23 0.0689 -2.0345 -0.0039 23.0236 1.0026 -0.0587 0.0342 14 -4 -4 0.1076 14.0099 -4.0001 -3.9608 -0.1525 0.6059 0.8003 -5 16 12 0.1149 -5.0100 16.0077 11.9816 0.2604 -0.9814 -0.1923 0 6 -20 0.0868 0.0329 6.0070 -20.0327 -0.9695 -0.3127 -0.1238 1 20 7 0.1092 1.0025 20.0118 6.9872 -0.0459 -1.0210 0.1378 -14 3 -2 0.1591 -14.0017 3.0005 -2.0456 -0.0900 -0.5529 -0.8418 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle P1 Ta P2 153.15(2) N1 Ta P1 108.11(7) N1 Ta P2 98.73(7) N1 Ta N3 121.68(8) N1 Ta C7 38.87(9) N1 Ta C22 134.47(9) N2 Ta P1 82.48(6) N2 Ta P2 94.38(6) N2 Ta N1 95.44(9) N2 Ta N3 142.65(8) N2 Ta C7 104.36(9) N2 Ta C22 39.12(9) N3 Ta P1 82.09(6) N3 Ta P2 84.62(6) N3 Ta C7 102.81(9) N3 Ta C22 103.84(8) C7 Ta P1 71.96(7) C7 Ta P2 134.06(7) C7 Ta C22 133.87(9) C22 Ta P1 75.27(7) C22 Ta P2 85.47(6) C1 P1 Ta 102.89(9) C1 P1 C31 112.01(12) C16 P1 Ta 108.59(9) C16 P1 C1 111.28(12) C16 P1 C31 106.05(12) C31 P1 Ta 116.06(9) C46 P2 Ta 116.23(11) C46 P2 C47 103.17(15) C47 P2 Ta 121.16(11) C48 P2 Ta 109.01(10) C48 P2 C46 101.92(16) C48 P2 C47 103.00(15) C7 N1 Ta 77.58(13) C8 N1 Ta 147.33(19) C8 N1 C7 129.6(2) C22 N2 Ta 82.03(13) C23 N2 Ta 151.49(18) C23 N2 C22 126.1(2) C37 N3 Ta 122.45(15) C38 N3 Ta 119.44(15) C38 N3 C37 118.10(19) C2 C1 P1 110.94(19) C6 C1 P1 127.2(2) C6 C1 C2 121.2(3) C1 C2 C7 116.8(2) C3 C2 C1 118.9(3) C3 C2 C7 124.3(3) C2 C3 H3 120.3 C2 C3 C4 119.3(3) C4 C3 H3 120.3 C3 C4 H4 119.4 C5 C4 C3 121.1(3) C5 C4 H4 119.4 C4 C5 H5 119.7 C4 C5 C6 120.6(3) C6 C5 H5 119.7 C1 C6 H6 120.6 C5 C6 C1 118.9(3) C5 C6 H6 120.6 Ta C7 H7 115.8 N1 C7 Ta 63.55(13) N1 C7 C2 121.0(2) N1 C7 H7 115.8 C2 C7 Ta 114.61(17) C2 C7 H7 115.8 N1 C8 C9 118.1(2) N1 C8 C13 123.3(3) C13 C8 C9 118.6(3) C8 C9 H9 119.2 C10 C9 C8 121.6(3) C10 C9 H9 119.2 C9 C10 C14 119.3(3) C11 C10 C9 118.1(3) C11 C10 C14 122.6(3) C10 C11 H11 118.8 C12 C11 C10 122.3(3) C12 C11 H11 118.8 C11 C12 C13 119.0(3) C11 C12 C15 121.5(3) C13 C12 C15 119.5(3) C8 C13 C12 120.3(3) C8 C13 H13 119.8 C12 C13 H13 119.8 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 P1 112.91(18) C21 C16 P1 125.6(2) C21 C16 C17 121.2(3) C16 C17 C22 121.0(2) C18 C17 C16 117.3(2) C18 C17 C22 121.6(3) C17 C18 H18 119.7 C19 C18 C17 120.5(3) C19 C18 H18 119.7 C18 C19 H19 119.3 C18 C19 C20 121.3(3) C20 C19 H19 119.3 C19 C20 H20 120.5 C21 C20 C19 119.1(3) C21 C20 H20 120.5 C16 C21 H21 119.8 C20 C21 C16 120.5(3) C20 C21 H21 119.8 Ta C22 H22 115.9 N2 C22 Ta 58.85(11) N2 C22 C17 116.4(2) N2 C22 H22 115.9 C17 C22 Ta 121.54(17) C17 C22 H22 115.9 N2 C23 C28 119.2(2) C24 C23 N2 121.8(3) C24 C23 C28 118.9(2) C23 C24 H24 119.7 C23 C24 C25 120.6(3) C25 C24 H24 119.7 C24 C25 C29 118.9(3) C26 C25 C24 119.2(3) C26 C25 C29 121.9(3) C25 C26 H26 119.4 C27 C26 C25 121.2(3) C27 C26 H26 119.4 C26 C27 C28 119.5(3) C26 C27 C30 120.1(3) C28 C27 C30 120.4(3) C23 C28 H28 119.7 C27 C28 C23 120.6(3) C27 C28 H28 119.7 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 P1 116.59(19) C36 C31 P1 123.1(2) C36 C31 C32 120.3(2) C31 C32 C37 121.4(2) C33 C32 C31 118.3(3) C33 C32 C37 120.3(2) C32 C33 H33 119.4 C34 C33 C32 121.2(3) C34 C33 H33 119.4 C33 C34 H34 120.0 C35 C34 C33 120.0(3) C35 C34 H34 120.0 C34 C35 H35 119.9 C34 C35 C36 120.3(3) C36 C35 H35 119.9 C31 C36 C35 119.9(3) C31 C36 H36 120.0 C35 C36 H36 120.0 N3 C37 C32 111.7(2) N3 C37 H37A 109.3 N3 C37 H37B 109.3 C32 C37 H37A 109.3 C32 C37 H37B 109.3 H37A C37 H37B 107.9 C39 C38 N3 118.6(2) C39 C38 C43 117.4(2) C43 C38 N3 124.0(2) C38 C39 H39 119.0 C40 C39 C38 122.0(3) C40 C39 H39 119.0 C39 C40 C44 120.2(3) C41 C40 C39 118.8(3) C41 C40 C44 121.1(3) C40 C41 H41 119.5 C42 C41 C40 121.1(3) C42 C41 H41 119.5 C41 C42 C43 119.2(3) C41 C42 C45 119.8(2) C43 C42 C45 121.0(3) C38 C43 H43 119.2 C42 C43 C38 121.5(2) C42 C43 H43 119.2 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 P2 C46 H46A 109.5 P2 C46 H46B 109.5 P2 C46 H46C 109.5 H46A C46 H46B 109.5 H46A C46 H46C 109.5 H46B C46 H46C 109.5 P2 C47 H47A 109.5 P2 C47 H47B 109.5 P2 C47 H47C 109.5 H47A C47 H47B 109.5 H47A C47 H47C 109.5 H47B C47 H47C 109.5 P2 C48 H48A 109.5 P2 C48 H48B 109.5 P2 C48 H48C 109.5 H48A C48 H48B 109.5 H48A C48 H48C 109.5 H48B C48 H48C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ta P1 2.4876(7) Ta P2 2.6874(7) Ta N1 2.031(2) Ta N2 1.970(2) Ta N3 2.088(2) Ta C7 2.215(2) Ta C22 2.280(2) P1 C1 1.814(3) P1 C16 1.806(3) P1 C31 1.820(3) P2 C46 1.819(3) P2 C47 1.825(3) P2 C48 1.817(3) N1 C7 1.424(3) N1 C8 1.388(3) N2 C22 1.453(3) N2 C23 1.401(3) N3 C37 1.475(3) N3 C38 1.412(3) C1 C2 1.407(4) C1 C6 1.392(4) C2 C3 1.396(4) C2 C7 1.513(4) C3 H3 0.9500 C3 C4 1.396(5) C4 H4 0.9500 C4 C5 1.376(5) C5 H5 0.9500 C5 C6 1.387(4) C6 H6 0.9500 C7 H7 1.0000 C8 C9 1.410(4) C8 C13 1.390(4) C9 H9 0.9500 C9 C10 1.394(4) C10 C11 1.384(5) C10 C14 1.503(5) C11 H11 0.9500 C11 C12 1.379(5) C12 C13 1.415(4) C12 C15 1.509(5) 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 1.412(4) C16 C21 1.402(4) C17 C18 1.411(4) C17 C22 1.501(4) C18 H18 0.9500 C18 C19 1.390(5) C19 H19 0.9500 C19 C20 1.393(5) C20 H20 0.9500 C20 C21 1.377(5) C21 H21 0.9500 C22 H22 1.0000 C23 C24 1.393(4) C23 C28 1.402(4) C24 H24 0.9500 C24 C25 1.404(4) C25 C26 1.384(5) C25 C29 1.515(5) C26 H26 0.9500 C26 C27 1.383(5) C27 C28 1.391(4) C27 C30 1.508(5) 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 1.413(4) C31 C36 1.384(4) C32 C33 1.392(4) C32 C37 1.520(4) C33 H33 0.9500 C33 C34 1.390(5) C34 H34 0.9500 C34 C35 1.370(5) C35 H35 0.9500 C35 C36 1.403(4) C36 H36 0.9500 C37 H37A 0.9900 C37 H37B 0.9900 C38 C39 1.401(3) C38 C43 1.403(4) C39 H39 0.9500 C39 C40 1.393(4) C40 C41 1.392(4) C40 C44 1.511(4) C41 H41 0.9500 C41 C42 1.385(4) C42 C43 1.397(4) C42 C45 1.517(4) 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 C46 H46A 0.9800 C46 H46B 0.9800 C46 H46C 0.9800 C47 H47A 0.9800 C47 H47B 0.9800 C47 H47C 0.9800 C48 H48A 0.9800 C48 H48B 0.9800 C48 H48C 0.9800 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 Ta P1 C1 C2 -22.9(2) Ta P1 C1 C6 148.1(2) Ta P1 C16 C17 -0.9(2) Ta P1 C16 C21 172.3(2) Ta P1 C31 C32 -37.9(2) Ta P1 C31 C36 142.5(2) Ta N1 C7 C2 -104.1(2) Ta N1 C8 C9 41.1(4) Ta N1 C8 C13 -136.3(3) Ta N2 C22 C17 112.5(2) Ta N2 C23 C24 -175.5(3) Ta N2 C23 C28 7.0(5) Ta N3 C37 C32 -85.8(2) Ta N3 C38 C39 34.3(3) Ta N3 C38 C43 -141.7(2) P1 C1 C2 C3 171.1(2) P1 C1 C2 C7 -9.5(3) P1 C1 C6 C5 -169.8(2) P1 C16 C17 C18 173.28(19) P1 C16 C17 C22 -5.2(3) P1 C16 C21 C20 -172.5(2) P1 C31 C32 C33 -177.4(2) P1 C31 C32 C37 2.9(3) P1 C31 C36 C35 177.9(2) N1 C8 C9 C10 -175.8(2) N1 C8 C13 C12 175.5(2) N2 C23 C24 C25 -177.1(3) N2 C23 C28 C27 177.6(2) N3 C38 C39 C40 -174.0(3) N3 C38 C43 C42 174.3(3) C1 P1 C16 C17 111.63(19) C1 P1 C16 C21 -75.1(3) C1 P1 C31 C32 -155.7(2) C1 P1 C31 C36 24.8(3) C1 C2 C3 C4 -0.4(4) C1 C2 C7 Ta 45.1(3) C1 C2 C7 N1 117.9(3) C2 C1 C6 C5 0.5(4) C2 C3 C4 C5 1.6(5) C3 C2 C7 Ta -135.5(2) C3 C2 C7 N1 -62.7(4) C3 C4 C5 C6 -1.8(5) C4 C5 C6 C1 0.7(5) C6 C1 C2 C3 -0.6(4) C6 C1 C2 C7 178.8(3) C7 N1 C8 C9 -178.3(2) C7 N1 C8 C13 4.3(4) C7 C2 C3 C4 -179.8(3) C8 N1 C7 Ta -159.5(3) C8 N1 C7 C2 96.4(3) C8 C9 C10 C11 -0.8(4) C8 C9 C10 C14 178.2(3) C9 C8 C13 C12 -1.9(4) C9 C10 C11 C12 0.0(4) C10 C11 C12 C13 -0.2(4) C10 C11 C12 C15 178.6(3) C11 C12 C13 C8 1.1(4) C13 C8 C9 C10 1.7(4) C14 C10 C11 C12 -179.0(3) C15 C12 C13 C8 -177.7(3) C16 P1 C1 C2 -139.05(19) C16 P1 C1 C6 32.0(3) C16 P1 C31 C32 82.7(2) C16 P1 C31 C36 -96.8(3) C16 C17 C18 C19 0.0(4) C16 C17 C22 Ta 10.0(3) C16 C17 C22 N2 -58.1(3) C17 C16 C21 C20 0.2(4) C17 C18 C19 C20 0.4(5) C18 C17 C22 Ta -168.42(19) C18 C17 C22 N2 123.5(3) C18 C19 C20 C21 -0.4(5) C19 C20 C21 C16 0.1(5) C21 C16 C17 C18 -0.3(4) C21 C16 C17 C22 -178.7(2) C22 N2 C23 C24 -5.9(4) C22 N2 C23 C28 176.6(2) C22 C17 C18 C19 178.4(3) C23 N2 C22 Ta -175.0(3) C23 N2 C22 C17 -62.5(3) C23 C24 C25 C26 -0.1(5) C23 C24 C25 C29 -178.8(4) C24 C23 C28 C27 0.1(4) C24 C25 C26 C27 -0.6(5) C25 C26 C27 C28 1.1(5) C25 C26 C27 C30 -179.7(3) C26 C27 C28 C23 -0.8(4) C28 C23 C24 C25 0.4(4) C29 C25 C26 C27 178.1(4) C30 C27 C28 C23 180.0(3) C31 P1 C1 C2 102.4(2) C31 P1 C1 C6 -86.5(3) C31 P1 C16 C17 -126.32(19) C31 P1 C16 C21 46.9(3) C31 C32 C33 C34 -1.0(4) C31 C32 C37 N3 58.9(3) C32 C31 C36 C35 -1.6(4) C32 C33 C34 C35 -0.7(5) C33 C32 C37 N3 -120.8(3) C33 C34 C35 C36 1.3(5) C34 C35 C36 C31 -0.1(5) C36 C31 C32 C33 2.2(4) C36 C31 C32 C37 -177.6(3) C37 N3 C38 C39 -145.1(2) C37 N3 C38 C43 39.0(4) C37 C32 C33 C34 178.7(3) C38 N3 C37 C32 93.6(3) C38 C39 C40 C41 -0.6(5) C38 C39 C40 C44 -178.6(3) C39 C38 C43 C42 -1.7(4) C39 C40 C41 C42 -1.7(5) C40 C41 C42 C43 2.2(5) C40 C41 C42 C45 -177.4(3) C41 C42 C43 C38 -0.5(5) C43 C38 C39 C40 2.3(4) C44 C40 C41 C42 176.2(3) C45 C42 C43 C38 179.1(3) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.121 0.500 1.000 553 145 toluene