#------------------------------------------------------------------------------ #$Date: 2015-06-04 14:02:18 +0300 (Thu, 04 Jun 2015) $ #$Revision: 137925 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/34/31/4343170.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_4343170 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 'C46 H44 F3 N3 Nb O3 P S' _chemical_formula_sum 'C49.5 H48 F3 N3 Nb O3 P S' _chemical_formula_weight 945.85 _chemical_properties_physical air-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_ms16 _audit_creation_date ; 'Thu Jul 03 11:50:11 2014' ; _audit_update_record 'Thu Jul 3 12:16:37 CEST 2014' _cell_angle_alpha 106.3805(17) _cell_angle_beta 107.6771(15) _cell_angle_gamma 105.6233(15) _cell_formula_units_Z 2 _cell_length_a 12.93050(18) _cell_length_b 13.1452(3) _cell_length_c 15.4214(3) _cell_measurement_reflns_used 23309 _cell_measurement_temperature 120(1) _cell_measurement_theta_max 28.3770 _cell_measurement_theta_min 3.8930 _cell_volume 2208.09(9) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'encif (Wadepohl, 2009-14); encifer 1.4 (CCDC, 2011)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'SUPERFLIP (Palatinus, 2007-2009)' _diffrn_ambient_environment 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 0.934 _diffrn_measurement_details ; 1 omega -8.00 89.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 77.0000 -30.0000 194 2 omega -47.00 -17.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -77.0000 -60.0000 60 3 omega 13.00 49.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -77.0000 -60.0000 72 4 omega -2.00 83.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 57.0000 90.0000 170 5 omega -11.00 89.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 77.0000 -180.0000 200 6 omega 17.00 77.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 57.0000 -90.0000 120 7 omega -32.00 49.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -77.0000 30.0000 162 8 omega -44.00 49.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -77.0000 -150.0000 186 9 omega 17.00 49.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -77.0000 -120.0000 64 10 omega 22.00 49.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -77.0000 150.0000 54 11 omega 22.00 49.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -77.0000 60.0000 54 12 omega 2.00 31.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 38.0000 -90.0000 58 13 omega -48.00 8.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -77.0000 -30.0000 112 14 omega 18.00 49.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -77.0000 -30.0000 62 15 omega -47.00 50.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -79.0000 117.1702 194 16 omega -3.00 87.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 57.0000 150.0000 180 17 omega -51.00 48.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -75.0000 -145.0000 198 18 omega -54.00 44.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -38.0000 -30.0000 196 19 omega -3.00 87.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 57.0000 -90.0000 180 20 omega -3.00 87.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 57.0000 60.0000 180 21 omega -47.00 50.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -79.0000 117.1702 194 22 omega -50.00 40.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -57.0000 -90.0000 180 23 omega -50.00 40.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -57.0000 0.0000 180 24 omega -51.00 -26.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -77.0000 -90.0000 50 25 omega -54.00 44.00 0.5000 20.0000 omega____ theta____ kappa____ phi______ frames - 18.6942 -38.0000 60.0000 196 ; _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 0.0503517000 _diffrn_orient_matrix_UB_12 -0.0062047000 _diffrn_orient_matrix_UB_13 -0.0063680000 _diffrn_orient_matrix_UB_21 0.0368670000 _diffrn_orient_matrix_UB_22 0.0512386000 _diffrn_orient_matrix_UB_23 0.0429314000 _diffrn_orient_matrix_UB_31 0.0029495000 _diffrn_orient_matrix_UB_32 -0.0325702000 _diffrn_orient_matrix_UB_33 0.0296873000 _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 0.0541 _diffrn_reflns_av_unetI/netI 0.0383 _diffrn_reflns_laue_measured_fraction_full 0.998 _diffrn_reflns_laue_measured_fraction_max 0.934 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 76928 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.934 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.993 _diffrn_reflns_theta_min 3.307 _diffrn_source 'microfocus X-Ray tube' _exptl_absorpt_coefficient_mu 0.415 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_correction_T_min 0.928 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) 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 orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.423 _exptl_crystal_description plate _exptl_crystal_F_000 978 _exptl_crystal_size_max 0.2511 _exptl_crystal_size_mid 0.2047 _exptl_crystal_size_min 0.0651 _refine_diff_density_max 0.822 _refine_diff_density_min -1.035 _refine_diff_density_rms 0.097 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.278 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 529 _refine_ls_number_reflns 10965 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.278 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0596 _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^)+(0.0357P)^2^+4.4885P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1226 _refine_ls_wR_factor_ref 0.1244 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10404 _reflns_number_total 10965 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL ba_ms16 - #2089 - in P-1 - superflip - nova CELL 0.71073 12.930504 13.145229 15.421371 106.3805 107.6771 105.6233 ZERR 2 0.00018 0.000255 0.000297 0.0017 0.0015 0.0015 LATT 1 SFAC C H F N Nb O P S UNIT 99 96 6 6 2 6 2 2 L.S. 5 0 16 PLAN 25 SIZE 0.1 0.1 0.1 TEMP -153.14 BOND $H CONF MORE -1 ABIN fmap 2 acta REM /struk/ba/ba_ms16/squeeze/ba_ms16_sq.hkl WGHT 0.035700 4.488500 FVAR 2.53189 NB 5 0.621475 0.711979 0.374926 11.00000 0.00960 0.01205 = 0.01285 0.00562 0.00576 0.00528 S 8 0.381356 0.539599 0.266571 11.00000 0.01257 0.01684 = 0.01645 0.00789 0.00587 0.00611 P 7 0.719202 0.888246 0.534856 11.00000 0.01089 0.01479 = 0.01509 0.00614 0.00600 0.00583 F1 3 0.184014 0.560169 0.189691 11.00000 0.02574 0.06428 = 0.04803 0.02963 0.01687 0.02907 F2 3 0.319976 0.653533 0.157542 11.00000 0.03005 0.04911 = 0.05699 0.04211 -0.00132 0.00471 F3 3 0.235052 0.469109 0.083699 11.00000 0.05188 0.05146 = 0.02112 0.00395 -0.00059 0.02923 O1 6 0.418810 0.642183 0.355897 11.00000 0.01621 0.02154 = 0.01798 0.00838 0.00891 0.00997 O2 6 0.483908 0.545796 0.240959 11.00000 0.01471 0.01824 = 0.01899 0.00731 0.00899 0.00799 O3 6 0.316619 0.431413 0.263539 11.00000 0.02000 0.02161 = 0.02856 0.01305 0.01010 0.00568 N1 4 0.749648 0.692859 0.335809 11.00000 0.01377 0.01623 = 0.01932 0.00698 0.00942 0.00805 N2 4 0.636201 0.645612 0.481832 11.00000 0.01371 0.01573 = 0.01733 0.00907 0.00779 0.00738 N3 4 0.562333 0.817341 0.314553 11.00000 0.01297 0.01499 = 0.01697 0.00673 0.00695 0.00675 C1 1 0.803225 0.809595 0.399055 11.00000 0.01503 0.01723 = 0.02247 0.01018 0.01154 0.00948 AFIX 13 H1 2 0.810351 0.863966 0.365032 11.00000 -1.20000 AFIX 0 C2 1 0.898362 0.853030 0.500837 11.00000 0.01248 0.01368 = 0.02269 0.00792 0.00666 0.00428 C3 1 0.873118 0.906814 0.579536 11.00000 0.01231 0.01556 = 0.02274 0.00943 0.00656 0.00573 C4 1 0.956256 0.956583 0.677338 11.00000 0.01851 0.01940 = 0.02486 0.00729 0.00794 0.00831 AFIX 43 H4 2 0.937697 0.992478 0.729979 11.00000 -1.20000 AFIX 0 C5 1 1.067942 0.952613 0.696507 11.00000 0.01688 0.02427 = 0.02580 0.00890 0.00001 0.00748 AFIX 43 H5 2 1.126856 0.988151 0.762445 11.00000 -1.20000 AFIX 0 C6 1 1.092278 0.896694 0.619010 11.00000 0.01253 0.02777 = 0.03759 0.01376 0.00807 0.00878 AFIX 43 H6 2 1.167487 0.892657 0.632724 11.00000 -1.20000 AFIX 0 C7 1 1.009023 0.846812 0.522286 11.00000 0.01556 0.02235 = 0.03144 0.01132 0.01168 0.00804 AFIX 43 H7 2 1.026971 0.808208 0.470237 11.00000 -1.20000 AFIX 0 C8 1 0.779783 0.634834 0.262107 11.00000 0.01742 0.01991 = 0.01629 0.00766 0.00798 0.01165 C9 1 0.719375 0.516371 0.207318 11.00000 0.01997 0.01739 = 0.02135 0.00860 0.01117 0.00923 AFIX 43 H9 2 0.654170 0.475676 0.217268 11.00000 -1.20000 AFIX 0 C10 1 0.753589 0.457296 0.138353 11.00000 0.02160 0.02078 = 0.02005 0.00880 0.00703 0.01257 C11 1 0.846851 0.518999 0.122124 11.00000 0.02342 0.03034 = 0.01593 0.00935 0.00996 0.01803 AFIX 43 H11 2 0.871422 0.478925 0.075899 11.00000 -1.20000 AFIX 0 C12 1 0.904642 0.637668 0.171967 11.00000 0.01653 0.02917 = 0.01882 0.01200 0.00876 0.01296 C13 1 0.871947 0.695701 0.243493 11.00000 0.01366 0.01877 = 0.01976 0.00698 0.00648 0.00594 AFIX 43 H13 2 0.912307 0.776542 0.279522 11.00000 -1.20000 AFIX 0 C14 1 0.690990 0.328767 0.081372 11.00000 0.03513 0.02366 = 0.02717 0.00907 0.01557 0.01447 AFIX 137 H14A 2 0.634956 0.298161 0.107478 11.00000 -1.50000 H14B 2 0.748790 0.292992 0.088503 11.00000 -1.50000 H14C 2 0.648559 0.311655 0.011121 11.00000 -1.50000 AFIX 0 C15 1 1.000435 0.703656 0.148389 11.00000 0.02184 0.03664 = 0.02469 0.01061 0.01449 0.01065 AFIX 137 H15A 2 1.077289 0.712269 0.193583 11.00000 -1.50000 H15B 2 0.999018 0.779868 0.156466 11.00000 -1.50000 H15C 2 0.987011 0.661549 0.079855 11.00000 -1.50000 AFIX 0 C16 1 0.576553 0.657098 0.549820 11.00000 0.01508 0.01975 = 0.01930 0.01024 0.00857 0.00799 AFIX 23 H16A 2 0.581023 0.599236 0.578739 11.00000 -1.20000 H16B 2 0.492234 0.635675 0.509303 11.00000 -1.20000 AFIX 0 C17 1 0.619476 0.772674 0.635139 11.00000 0.01352 0.02370 = 0.01734 0.01002 0.00670 0.01154 C18 1 0.678532 0.880125 0.636938 11.00000 0.01193 0.02241 = 0.01611 0.00915 0.00570 0.00954 C19 1 0.708256 0.980859 0.718621 11.00000 0.01949 0.02413 = 0.02145 0.00899 0.00806 0.00992 AFIX 43 H19 2 0.749666 1.053582 0.720353 11.00000 -1.20000 AFIX 0 C20 1 0.678037 0.975642 0.796665 11.00000 0.03493 0.03165 = 0.01832 0.00846 0.01175 0.01846 AFIX 43 H20 2 0.698652 1.044278 0.851442 11.00000 -1.20000 AFIX 0 C21 1 0.617411 0.869344 0.794173 11.00000 0.03577 0.03491 = 0.02094 0.01540 0.01781 0.01795 AFIX 43 H21 2 0.595256 0.865127 0.846824 11.00000 -1.20000 AFIX 0 C22 1 0.589292 0.769477 0.714806 11.00000 0.02563 0.02713 = 0.02191 0.01403 0.01274 0.01348 AFIX 43 H22 2 0.548678 0.697189 0.714233 11.00000 -1.20000 AFIX 0 C23 1 0.722475 0.597051 0.506611 11.00000 0.01478 0.01660 = 0.02204 0.01165 0.01000 0.00740 C24 1 0.719170 0.504336 0.432382 11.00000 0.01823 0.01682 = 0.02151 0.01163 0.01006 0.00741 AFIX 43 H24 2 0.659987 0.474890 0.367064 11.00000 -1.20000 AFIX 0 C25 1 0.801124 0.454268 0.452425 11.00000 0.02136 0.02095 = 0.03297 0.01582 0.01826 0.01085 C26 1 0.886210 0.497719 0.549207 11.00000 0.01909 0.02772 = 0.04048 0.02200 0.01764 0.01519 AFIX 43 H26 2 0.943178 0.464975 0.563592 11.00000 -1.20000 AFIX 0 C27 1 0.889554 0.587859 0.625108 11.00000 0.01804 0.02804 = 0.02975 0.01889 0.01160 0.01138 C28 1 0.807565 0.638066 0.602820 11.00000 0.01853 0.02076 = 0.02284 0.01016 0.01131 0.00902 AFIX 43 H28 2 0.809999 0.700685 0.653791 11.00000 -1.20000 AFIX 0 C29 1 0.794213 0.353511 0.370455 11.00000 0.03497 0.02933 = 0.03721 0.01493 0.02267 0.01808 AFIX 137 H29A 2 0.718805 0.289102 0.345718 11.00000 -1.50000 H29B 2 0.858941 0.330007 0.396218 11.00000 -1.50000 H29C 2 0.800412 0.376082 0.316270 11.00000 -1.50000 AFIX 0 C30 1 0.979840 0.632354 0.729997 11.00000 0.02328 0.04784 = 0.02819 0.01912 0.00781 0.01988 AFIX 137 H30A 2 1.022316 0.581268 0.734894 11.00000 -1.50000 H30B 2 0.940221 0.634719 0.775116 11.00000 -1.50000 H30C 2 1.035669 0.709997 0.748159 11.00000 -1.50000 AFIX 0 C31 1 0.517998 0.896028 0.366709 11.00000 0.01280 0.01678 = 0.01767 0.00659 0.00748 0.00786 AFIX 23 H31A 2 0.474593 0.857169 0.398896 11.00000 -1.20000 H31B 2 0.461238 0.910715 0.317087 11.00000 -1.20000 AFIX 0 C32 1 0.612975 1.011611 0.445309 11.00000 0.01441 0.01695 = 0.01729 0.00671 0.01122 0.00696 C33 1 0.709885 1.019618 0.523818 11.00000 0.01443 0.01590 = 0.01795 0.00765 0.01056 0.00771 C34 1 0.796252 1.127638 0.591683 11.00000 0.01597 0.01886 = 0.01826 0.00567 0.00816 0.00697 AFIX 43 H34 2 0.863306 1.132336 0.642602 11.00000 -1.20000 AFIX 0 C35 1 0.785608 1.228417 0.585873 11.00000 0.02186 0.01559 = 0.02113 0.00531 0.01305 0.00461 AFIX 43 H35 2 0.844327 1.301353 0.632832 11.00000 -1.20000 AFIX 0 C36 1 0.688358 1.220951 0.510783 11.00000 0.02569 0.01892 = 0.02906 0.01272 0.02075 0.01361 AFIX 43 H36 2 0.679172 1.289081 0.506958 11.00000 -1.20000 AFIX 0 C37 1 0.604157 1.113969 0.440998 11.00000 0.01683 0.02200 = 0.02132 0.01144 0.01267 0.01099 AFIX 43 H37 2 0.538890 1.110262 0.388996 11.00000 -1.20000 AFIX 0 C38 1 0.582927 0.834734 0.234281 11.00000 0.01022 0.01860 = 0.01593 0.00747 0.00388 0.00533 C39 1 0.597552 0.937828 0.220009 11.00000 0.01413 0.01893 = 0.01700 0.00658 0.00570 0.00602 AFIX 43 H39 2 0.590813 0.999302 0.265138 11.00000 -1.20000 AFIX 0 C40 1 0.621774 0.951660 0.140858 11.00000 0.01706 0.02003 = 0.02114 0.00992 0.00637 0.00571 C41 1 0.631626 0.861648 0.074420 11.00000 0.02110 0.02735 = 0.01706 0.01036 0.01027 0.00883 AFIX 43 H41 2 0.650099 0.871683 0.021504 11.00000 -1.20000 AFIX 0 C42 1 0.614695 0.756980 0.084652 11.00000 0.01967 0.02446 = 0.01758 0.00784 0.00858 0.01049 C43 1 0.589595 0.744315 0.163375 11.00000 0.02145 0.01860 = 0.01962 0.01002 0.01000 0.01012 AFIX 43 H43 2 0.576512 0.672614 0.169701 11.00000 -1.20000 AFIX 0 C44 1 0.641575 1.065183 0.130138 11.00000 0.04118 0.02488 = 0.02835 0.01553 0.01897 0.01144 AFIX 137 H44A 2 0.593866 1.101210 0.155730 11.00000 -1.50000 H44B 2 0.618662 1.052069 0.059990 11.00000 -1.50000 H44C 2 0.725051 1.115968 0.167735 11.00000 -1.50000 AFIX 0 C45 1 0.618802 0.657412 0.009858 11.00000 0.04269 0.03359 = 0.02259 0.01133 0.01803 0.02077 AFIX 137 H45A 2 0.539753 0.596407 -0.027770 11.00000 -1.50000 H45B 2 0.672693 0.627633 0.044303 11.00000 -1.50000 H45C 2 0.646631 0.683423 -0.035616 11.00000 -1.50000 AFIX 0 C46 1 0.275392 0.558017 0.167687 11.00000 0.01790 0.02492 = 0.02031 0.00902 0.00359 0.00869 HKLF 4 REM ba_ms16 - #2089 - in P-1 - superflip - nova REM R1 = 0.0596 for 10404 Fo > 4sig(Fo) and 0.0648 for all 10965 data REM 529 parameters refined using 0 restraints END WGHT 0.0357 4.4885 REM Highest difference peak 0.822, deepest hole -1.035, 1-sigma level 0.097 Q1 1 0.6493 0.7518 0.4438 11.00000 0.05 0.82 Q2 1 0.5995 0.7637 0.3311 11.00000 0.05 0.69 Q3 1 0.5855 0.6649 0.3079 11.00000 0.05 0.65 Q4 1 0.6308 0.6579 0.4120 11.00000 0.05 0.65 Q5 1 0.2966 0.5325 0.0873 11.00000 0.05 0.59 Q6 1 0.9200 0.8791 0.8802 11.00000 0.05 0.54 Q7 1 0.6656 0.7917 0.4135 11.00000 0.05 0.54 Q8 1 0.9746 1.0209 0.9269 11.00000 0.05 0.51 Q9 1 0.6985 0.8206 0.4945 11.00000 0.05 0.51 Q10 1 0.5695 0.9548 0.4100 11.00000 0.05 0.50 Q11 1 0.7041 0.9391 0.5034 11.00000 0.05 0.48 Q12 1 0.5807 0.6372 0.3470 11.00000 0.05 0.46 Q13 1 0.6934 0.8649 0.5769 11.00000 0.05 0.46 Q14 1 0.3257 0.5380 0.2080 11.00000 0.05 0.46 Q15 1 0.5853 0.7165 0.5847 11.00000 0.05 0.45 Q16 1 0.8797 0.8180 -0.0584 11.00000 0.05 0.44 Q17 1 1.0261 0.9611 0.9271 11.00000 0.05 0.44 Q18 1 0.3365 0.4595 0.2324 11.00000 0.05 0.44 Q19 1 0.7964 1.1808 0.5919 11.00000 0.05 0.43 Q20 1 0.9038 0.6664 0.2152 11.00000 0.05 0.43 Q21 1 0.8931 0.8994 0.5390 11.00000 0.05 0.42 Q22 1 0.7202 0.3989 0.1035 11.00000 0.05 0.42 Q23 1 0.7606 0.4817 0.4473 11.00000 0.05 0.41 Q24 1 0.9165 0.9431 -0.0027 11.00000 0.05 0.41 Q25 1 0.3990 0.6140 0.3011 11.00000 0.05 0.41 ; _cod_data_source_file ic5b00333_si_001.cif _cod_data_source_block ba_ms16_sq _cod_original_cell_volume 2208.08(7) _cod_chemical_formula_sum_orig 'C49.50 H48 F3 N3 Nb O3 P S' _cod_database_code 4343170 _audit_block_refno 2089 _audit_block_usercomment 'MS260, plate, orange' _shelxl_version_number 2014-3 _chemical_oxdiff_formula 'C53 H52 F3 N3 Nb O3 P S' _chemical_oxdiff_usercomment 'MS260, plate, 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 0.960 _shelx_estimated_absorpt_t_min 0.960 _reflns_odcompleteness_completeness 99.79 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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: C1(H1) 2.b Secondary CH2 refined with riding coordinates: C16(H16A,H16B), C31(H31A,H31B) 2.c Aromatic/amide H refined with riding coordinates: C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C11(H11), C13(H13), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C26(H26), C28(H28), C34(H34), C35(H35), C36(H36), C37(H37), 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) ; _shelx_res_checksum 14341 _olex2_submission_special_instructions 'No special instructions were received' _cell_oxdiff_length_a 12.93050(18) _cell_oxdiff_length_b 13.1452(2) _cell_oxdiff_length_c 15.4214(3) _cell_oxdiff_angle_alpha 106.3805(17) _cell_oxdiff_angle_beta 107.6771(15) _cell_oxdiff_angle_gamma 105.6233(15) _cell_oxdiff_volume 2208.09(6) _cell_oxdiff_measurement_reflns_used 23309 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 Nb Nb 0.62148(2) 0.71198(2) 0.37493(2) 0.01078(7) Uani 1 1 d . S S 0.38136(6) 0.53960(6) 0.26657(5) 0.01491(15) Uani 1 1 d . P P 0.71920(6) 0.88825(6) 0.53486(6) 0.01317(15) Uani 1 1 d . F1 F 0.18401(19) 0.5602(2) 0.18969(18) 0.0411(6) Uani 1 1 d . F2 F 0.3200(2) 0.6535(2) 0.1575(2) 0.0478(7) Uani 1 1 d . F3 F 0.2351(2) 0.4691(2) 0.08370(16) 0.0460(6) Uani 1 1 d . O1 O 0.41881(18) 0.64218(19) 0.35590(16) 0.0173(4) Uani 1 1 d . O2 O 0.48391(18) 0.54580(18) 0.24096(16) 0.0164(4) Uani 1 1 d . O3 O 0.3166(2) 0.4314(2) 0.26354(18) 0.0232(5) Uani 1 1 d . N1 N 0.7496(2) 0.6929(2) 0.33581(19) 0.0153(5) Uani 1 1 d . N2 N 0.6362(2) 0.6456(2) 0.48183(18) 0.0142(5) Uani 1 1 d . N3 N 0.5623(2) 0.8173(2) 0.31455(18) 0.0144(5) Uani 1 1 d . C1 C 0.8032(3) 0.8096(3) 0.3991(2) 0.0159(6) Uani 1 1 d . H1 H 0.8104 0.8640 0.3650 0.019 Uiso 1 1 calc R C2 C 0.8984(3) 0.8530(3) 0.5008(2) 0.0164(6) Uani 1 1 d . C3 C 0.8731(3) 0.9068(3) 0.5795(2) 0.0165(6) Uani 1 1 d . C4 C 0.9563(3) 0.9566(3) 0.6773(2) 0.0213(6) Uani 1 1 d . H4 H 0.9377 0.9925 0.7300 0.026 Uiso 1 1 calc R C5 C 1.0679(3) 0.9526(3) 0.6965(3) 0.0250(7) Uani 1 1 d . H5 H 1.1269 0.9882 0.7624 0.030 Uiso 1 1 calc R C6 C 1.0923(3) 0.8967(3) 0.6190(3) 0.0261(7) Uani 1 1 d . H6 H 1.1675 0.8927 0.6327 0.031 Uiso 1 1 calc R C7 C 1.0090(3) 0.8468(3) 0.5223(3) 0.0223(7) Uani 1 1 d . H7 H 1.0270 0.8082 0.4702 0.027 Uiso 1 1 calc R C8 C 0.7798(3) 0.6348(3) 0.2621(2) 0.0165(6) Uani 1 1 d . C9 C 0.7194(3) 0.5164(3) 0.2073(2) 0.0182(6) Uani 1 1 d . H9 H 0.6542 0.4757 0.2173 0.022 Uiso 1 1 calc R C10 C 0.7536(3) 0.4573(3) 0.1384(2) 0.0200(6) Uani 1 1 d . C11 C 0.8469(3) 0.5190(3) 0.1221(2) 0.0209(6) Uani 1 1 d . H11 H 0.8714 0.4789 0.0759 0.025 Uiso 1 1 calc R C12 C 0.9046(3) 0.6377(3) 0.1720(2) 0.0196(6) Uani 1 1 d . C13 C 0.8719(3) 0.6957(3) 0.2435(2) 0.0177(6) Uani 1 1 d . H13 H 0.9123 0.7765 0.2795 0.021 Uiso 1 1 calc R C14 C 0.6910(3) 0.3288(3) 0.0814(3) 0.0275(7) Uani 1 1 d . H14A H 0.6350 0.2982 0.1075 0.041 Uiso 1 1 calc GR H14B H 0.7488 0.2930 0.0885 0.041 Uiso 1 1 calc GR H14C H 0.6486 0.3117 0.0111 0.041 Uiso 1 1 calc GR C15 C 1.0004(3) 0.7037(3) 0.1484(3) 0.0270(7) Uani 1 1 d . H15A H 1.0773 0.7123 0.1936 0.040 Uiso 1 1 calc GR H15B H 0.9990 0.7799 0.1565 0.040 Uiso 1 1 calc GR H15C H 0.9870 0.6615 0.0799 0.040 Uiso 1 1 calc GR C16 C 0.5766(3) 0.6571(3) 0.5498(2) 0.0168(6) Uani 1 1 d . H16A H 0.5810 0.5992 0.5787 0.020 Uiso 1 1 calc R H16B H 0.4922 0.6357 0.5093 0.020 Uiso 1 1 calc R C17 C 0.6195(3) 0.7727(3) 0.6351(2) 0.0166(6) Uani 1 1 d . C18 C 0.6785(3) 0.8801(3) 0.6369(2) 0.0158(6) Uani 1 1 d . C19 C 0.7083(3) 0.9809(3) 0.7186(2) 0.0215(6) Uani 1 1 d . H19 H 0.7497 1.0536 0.7204 0.026 Uiso 1 1 calc R C20 C 0.6780(3) 0.9756(3) 0.7967(3) 0.0272(7) Uani 1 1 d . H20 H 0.6987 1.0443 0.8514 0.033 Uiso 1 1 calc R C21 C 0.6174(3) 0.8693(3) 0.7942(3) 0.0269(7) Uani 1 1 d . H21 H 0.5953 0.8651 0.8468 0.032 Uiso 1 1 calc R C22 C 0.5893(3) 0.7695(3) 0.7148(2) 0.0223(7) Uani 1 1 d . H22 H 0.5487 0.6972 0.7142 0.027 Uiso 1 1 calc R C23 C 0.7225(3) 0.5971(3) 0.5066(2) 0.0159(6) Uani 1 1 d . C24 C 0.7192(3) 0.5043(3) 0.4324(2) 0.0172(6) Uani 1 1 d . H24 H 0.6600 0.4749 0.3671 0.021 Uiso 1 1 calc R C25 C 0.8011(3) 0.4543(3) 0.4524(3) 0.0214(7) Uani 1 1 d . C26 C 0.8862(3) 0.4977(3) 0.5492(3) 0.0242(7) Uani 1 1 d . H26 H 0.9432 0.4650 0.5636 0.029 Uiso 1 1 calc R C27 C 0.8896(3) 0.5879(3) 0.6251(3) 0.0224(7) Uani 1 1 d . C28 C 0.8076(3) 0.6381(3) 0.6028(2) 0.0193(6) Uani 1 1 d . H28 H 0.8100 0.7007 0.6538 0.023 Uiso 1 1 calc R C29 C 0.7942(3) 0.3535(3) 0.3705(3) 0.0301(8) Uani 1 1 d . H29A H 0.7188 0.2891 0.3457 0.045 Uiso 1 1 calc GR H29B H 0.8589 0.3300 0.3962 0.045 Uiso 1 1 calc GR H29C H 0.8004 0.3761 0.3163 0.045 Uiso 1 1 calc GR C30 C 0.9798(3) 0.6324(4) 0.7300(3) 0.0314(8) Uani 1 1 d . H30A H 1.0223 0.5813 0.7349 0.047 Uiso 1 1 calc GR H30B H 0.9402 0.6347 0.7751 0.047 Uiso 1 1 calc GR H30C H 1.0357 0.7100 0.7482 0.047 Uiso 1 1 calc GR C31 C 0.5180(3) 0.8960(3) 0.3667(2) 0.0150(6) Uani 1 1 d . H31A H 0.4746 0.8572 0.3989 0.018 Uiso 1 1 calc R H31B H 0.4612 0.9107 0.3171 0.018 Uiso 1 1 calc R C32 C 0.6130(3) 1.0116(3) 0.4453(2) 0.0148(6) Uani 1 1 d . C33 C 0.7099(3) 1.0196(3) 0.5238(2) 0.0144(6) Uani 1 1 d . C34 C 0.7963(3) 1.1276(3) 0.5917(2) 0.0178(6) Uani 1 1 d . H34 H 0.8633 1.1323 0.6426 0.021 Uiso 1 1 calc R C35 C 0.7856(3) 1.2284(3) 0.5859(2) 0.0195(6) Uani 1 1 d . H35 H 0.8443 1.3014 0.6328 0.023 Uiso 1 1 calc R C36 C 0.6884(3) 1.2210(3) 0.5108(2) 0.0201(6) Uani 1 1 d . H36 H 0.6792 1.2891 0.5070 0.024 Uiso 1 1 calc R C37 C 0.6042(3) 1.1140(3) 0.4410(2) 0.0173(6) Uani 1 1 d . H37 H 0.5389 1.1103 0.3890 0.021 Uiso 1 1 calc R C38 C 0.5829(2) 0.8347(3) 0.2343(2) 0.0152(6) Uani 1 1 d . C39 C 0.5976(3) 0.9378(3) 0.2200(2) 0.0171(6) Uani 1 1 d . H39 H 0.5908 0.9993 0.2651 0.021 Uiso 1 1 calc R C40 C 0.6218(3) 0.9517(3) 0.1409(2) 0.0197(6) Uani 1 1 d . C41 C 0.6316(3) 0.8616(3) 0.0744(2) 0.0209(6) Uani 1 1 d . H41 H 0.6501 0.8717 0.0215 0.025 Uiso 1 1 calc R C42 C 0.6147(3) 0.7570(3) 0.0847(2) 0.0200(6) Uani 1 1 d . C43 C 0.5896(3) 0.7443(3) 0.1634(2) 0.0183(6) Uani 1 1 d . H43 H 0.5765 0.6726 0.1697 0.022 Uiso 1 1 calc R C44 C 0.6416(4) 1.0652(3) 0.1301(3) 0.0293(8) Uani 1 1 d . H44A H 0.5939 1.1012 0.1557 0.044 Uiso 1 1 calc GR H44B H 0.6187 1.0521 0.0600 0.044 Uiso 1 1 calc GR H44C H 0.7251 1.1160 0.1677 0.044 Uiso 1 1 calc GR C45 C 0.6188(4) 0.6574(3) 0.0099(3) 0.0303(8) Uani 1 1 d . H45A H 0.5398 0.5964 -0.0278 0.045 Uiso 1 1 calc GR H45B H 0.6727 0.6276 0.0443 0.045 Uiso 1 1 calc GR H45C H 0.6466 0.6834 -0.0356 0.045 Uiso 1 1 calc GR C46 C 0.2754(3) 0.5580(3) 0.1677(2) 0.0221(7) Uani 1 1 d . 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 Nb 0.00960(12) 0.01205(13) 0.01285(13) 0.00562(9) 0.00576(9) 0.00528(9) S 0.0126(3) 0.0168(3) 0.0164(3) 0.0079(3) 0.0059(3) 0.0061(3) P 0.0109(3) 0.0148(4) 0.0151(4) 0.0061(3) 0.0060(3) 0.0058(3) F1 0.0257(11) 0.0643(16) 0.0480(14) 0.0296(13) 0.0169(10) 0.0291(11) F2 0.0301(12) 0.0491(15) 0.0570(16) 0.0421(13) -0.0013(11) 0.0047(11) F3 0.0519(15) 0.0515(15) 0.0211(11) 0.0040(10) -0.0006(10) 0.0292(13) O1 0.0162(10) 0.0215(11) 0.0180(11) 0.0084(9) 0.0089(9) 0.0100(9) O2 0.0147(10) 0.0182(11) 0.0190(11) 0.0073(9) 0.0090(9) 0.0080(8) O3 0.0200(11) 0.0216(12) 0.0286(13) 0.0131(10) 0.0101(10) 0.0057(9) N1 0.0138(11) 0.0162(12) 0.0193(13) 0.0070(10) 0.0094(10) 0.0081(10) N2 0.0137(11) 0.0157(12) 0.0173(12) 0.0091(10) 0.0078(10) 0.0074(10) N3 0.0130(11) 0.0150(12) 0.0170(12) 0.0067(10) 0.0070(10) 0.0067(10) C1 0.0150(13) 0.0172(14) 0.0225(15) 0.0102(12) 0.0115(12) 0.0095(12) C2 0.0125(13) 0.0137(14) 0.0227(15) 0.0079(12) 0.0067(12) 0.0043(11) C3 0.0123(13) 0.0156(14) 0.0227(15) 0.0094(12) 0.0066(12) 0.0057(11) C4 0.0185(15) 0.0194(15) 0.0249(17) 0.0073(13) 0.0079(13) 0.0083(13) C5 0.0169(15) 0.0243(17) 0.0258(17) 0.0089(14) 0.0000(13) 0.0075(13) C6 0.0125(14) 0.0278(18) 0.038(2) 0.0138(15) 0.0081(14) 0.0088(13) C7 0.0156(14) 0.0224(16) 0.0314(18) 0.0113(14) 0.0117(13) 0.0080(13) C8 0.0174(14) 0.0199(15) 0.0163(14) 0.0077(12) 0.0080(12) 0.0116(12) C9 0.0200(15) 0.0174(15) 0.0213(15) 0.0086(12) 0.0112(13) 0.0092(12) C10 0.0216(15) 0.0208(16) 0.0200(15) 0.0088(13) 0.0070(13) 0.0126(13) C11 0.0234(16) 0.0303(17) 0.0159(15) 0.0094(13) 0.0100(13) 0.0180(14) C12 0.0165(14) 0.0292(17) 0.0188(15) 0.0120(13) 0.0088(12) 0.0130(13) C13 0.0137(13) 0.0188(15) 0.0198(15) 0.0070(12) 0.0065(12) 0.0059(12) C14 0.0351(19) 0.0237(17) 0.0272(18) 0.0091(14) 0.0156(15) 0.0145(15) C15 0.0218(16) 0.037(2) 0.0247(17) 0.0106(15) 0.0145(14) 0.0106(15) C16 0.0151(14) 0.0197(15) 0.0193(15) 0.0102(12) 0.0086(12) 0.0080(12) C17 0.0135(13) 0.0237(16) 0.0173(14) 0.0100(12) 0.0067(11) 0.0115(12) C18 0.0119(13) 0.0224(15) 0.0161(14) 0.0091(12) 0.0057(11) 0.0095(12) C19 0.0195(15) 0.0241(16) 0.0215(16) 0.0090(13) 0.0081(13) 0.0099(13) C20 0.0349(19) 0.0316(19) 0.0183(16) 0.0085(14) 0.0118(15) 0.0185(16) C21 0.0358(19) 0.0349(19) 0.0209(16) 0.0154(15) 0.0178(15) 0.0179(16) C22 0.0256(16) 0.0271(17) 0.0219(16) 0.0140(14) 0.0127(14) 0.0135(14) C23 0.0148(13) 0.0166(14) 0.0220(15) 0.0117(12) 0.0100(12) 0.0074(12) C24 0.0182(14) 0.0168(14) 0.0215(15) 0.0116(12) 0.0101(12) 0.0074(12) C25 0.0214(15) 0.0209(16) 0.0330(18) 0.0158(14) 0.0183(14) 0.0109(13) C26 0.0191(15) 0.0277(17) 0.040(2) 0.0220(16) 0.0176(15) 0.0152(14) C27 0.0180(15) 0.0280(17) 0.0297(18) 0.0189(15) 0.0116(14) 0.0114(13) C28 0.0185(14) 0.0208(15) 0.0228(16) 0.0102(13) 0.0113(13) 0.0090(12) C29 0.035(2) 0.0293(19) 0.037(2) 0.0149(16) 0.0227(17) 0.0181(16) C30 0.0233(17) 0.048(2) 0.0282(19) 0.0191(17) 0.0078(15) 0.0199(17) C31 0.0128(13) 0.0168(14) 0.0177(14) 0.0066(12) 0.0075(11) 0.0079(11) C32 0.0144(13) 0.0170(14) 0.0173(14) 0.0067(12) 0.0112(12) 0.0070(11) C33 0.0144(13) 0.0159(14) 0.0179(14) 0.0077(12) 0.0106(12) 0.0077(11) C34 0.0160(14) 0.0189(15) 0.0183(15) 0.0057(12) 0.0082(12) 0.0070(12) C35 0.0219(15) 0.0156(14) 0.0211(15) 0.0053(12) 0.0130(13) 0.0046(12) C36 0.0257(16) 0.0189(15) 0.0291(17) 0.0127(13) 0.0208(14) 0.0136(13) C37 0.0168(14) 0.0220(15) 0.0213(15) 0.0114(13) 0.0127(12) 0.0110(12) C38 0.0102(12) 0.0186(14) 0.0159(14) 0.0075(12) 0.0039(11) 0.0053(11) C39 0.0141(13) 0.0189(15) 0.0170(14) 0.0066(12) 0.0057(12) 0.0060(12) C40 0.0171(14) 0.0200(15) 0.0211(15) 0.0099(13) 0.0064(12) 0.0057(12) C41 0.0211(15) 0.0273(17) 0.0171(15) 0.0104(13) 0.0103(13) 0.0088(13) C42 0.0197(15) 0.0245(16) 0.0176(15) 0.0078(13) 0.0086(12) 0.0105(13) C43 0.0215(15) 0.0186(15) 0.0196(15) 0.0100(12) 0.0100(13) 0.0101(12) C44 0.041(2) 0.0249(18) 0.0283(18) 0.0155(15) 0.0190(16) 0.0114(16) C45 0.043(2) 0.034(2) 0.0226(17) 0.0113(15) 0.0180(16) 0.0208(17) C46 0.0179(15) 0.0249(17) 0.0203(16) 0.0090(13) 0.0036(13) 0.0087(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' F F 0.0171 0.0103 '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' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 '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 -6 15 -15 0.0887 -5.9999 15.0029 -15.0018 -0.2997 -0.0965 -0.9517 17 -5 0 0.0767 16.9995 -5.0000 -0.0004 0.8870 0.3705 0.2130 -14 -7 14 0.0785 -13.9996 -7.0027 14.0022 -0.7506 -0.2738 0.6025 6 -15 15 0.0887 5.9999 -15.0029 15.0018 0.2997 0.0965 0.9517 -1 14 6 0.0102 -1.0022 13.9990 6.0025 -0.1755 0.9380 -0.2807 1 -15 -3 0.0387 1.0020 -14.9996 -3.0020 0.1626 -0.8605 0.4024 0 -11 20 0.0993 -0.0007 -11.0038 20.0031 -0.0591 0.2949 0.9522 12 9 -15 0.1177 11.9996 9.0029 -15.0022 0.6439 0.2596 -0.7032 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle P Nb S 132.39(2) O1 Nb S 30.11(5) O1 Nb P 102.36(5) O2 Nb S 30.26(5) O2 Nb P 162.64(5) O2 Nb O1 60.32(7) N1 Nb S 121.32(8) N1 Nb P 105.87(8) N1 Nb O1 151.33(9) N1 Nb O2 91.28(9) N1 Nb N2 102.54(10) N1 Nb N3 107.51(10) N1 Nb C1 38.54(10) N2 Nb S 87.02(7) N2 Nb P 76.41(7) N2 Nb O1 79.22(8) N2 Nb O2 97.60(9) N2 Nb N3 147.70(10) N2 Nb C1 106.30(11) N3 Nb S 87.37(7) N3 Nb P 84.17(7) N3 Nb O1 80.08(9) N3 Nb O2 93.35(9) N3 Nb C1 90.46(10) C1 Nb S 157.13(8) C1 Nb P 69.85(8) C1 Nb O1 168.46(9) C1 Nb O2 127.44(9) O1 S Nb 56.15(9) O1 S O2 107.75(12) O1 S C46 104.81(14) O2 S Nb 51.70(8) O2 S C46 105.74(14) O3 S Nb 137.00(10) O3 S O1 117.77(14) O3 S O2 115.86(13) O3 S C46 103.53(15) C46 S Nb 119.36(11) C3 P Nb 103.63(10) C3 P C18 104.39(14) C18 P Nb 118.14(10) C33 P Nb 115.69(10) C33 P C3 108.54(14) C33 P C18 105.57(14) S O1 Nb 93.74(10) S O2 Nb 98.04(11) C1 N1 Nb 79.65(16) C1 N1 C8 127.8(3) C8 N1 Nb 146.8(2) C16 N2 Nb 125.76(19) C23 N2 Nb 120.66(19) C23 N2 C16 113.0(2) C31 N3 Nb 120.29(19) C38 N3 Nb 122.21(19) C38 N3 C31 116.4(2) Nb C1 H1 115.0 N1 C1 Nb 61.81(15) N1 C1 H1 115.0 N1 C1 C2 122.1(3) C2 C1 Nb 117.6(2) C2 C1 H1 115.0 C3 C2 C1 115.9(3) C7 C2 C1 125.5(3) C7 C2 C3 118.6(3) C2 C3 P 110.3(2) C4 C3 P 127.7(2) C4 C3 C2 121.7(3) C3 C4 H4 120.7 C3 C4 C5 118.6(3) C5 C4 H4 120.7 C4 C5 H5 120.1 C6 C5 C4 119.9(3) C6 C5 H5 120.1 C5 C6 H6 119.4 C7 C6 C5 121.1(3) C7 C6 H6 119.4 C2 C7 H7 119.9 C6 C7 C2 120.1(3) C6 C7 H7 119.9 N1 C8 C13 119.9(3) C9 C8 N1 120.6(3) C9 C8 C13 119.5(3) C8 C9 H9 119.6 C10 C9 C8 120.8(3) C10 C9 H9 119.6 C9 C10 C11 118.9(3) C9 C10 C14 120.9(3) C11 C10 C14 120.2(3) C10 C11 H11 119.2 C12 C11 C10 121.5(3) C12 C11 H11 119.2 C11 C12 C13 119.0(3) C11 C12 C15 120.6(3) C13 C12 C15 120.4(3) C8 C13 H13 119.9 C12 C13 C8 120.2(3) C12 C13 H13 119.9 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 N2 C16 H16A 107.5 N2 C16 H16B 107.5 N2 C16 C17 119.3(2) H16A C16 H16B 107.0 C17 C16 H16A 107.5 C17 C16 H16B 107.5 C18 C17 C16 125.4(3) C18 C17 C22 118.4(3) C22 C17 C16 116.0(3) C17 C18 P 119.9(2) C17 C18 C19 119.6(3) C19 C18 P 120.6(2) C18 C19 H19 119.5 C20 C19 C18 121.0(3) C20 C19 H19 119.5 C19 C20 H20 120.2 C19 C20 C21 119.5(3) C21 C20 H20 120.2 C20 C21 H21 120.0 C22 C21 C20 119.9(3) C22 C21 H21 120.0 C17 C22 H22 119.2 C21 C22 C17 121.5(3) C21 C22 H22 119.2 C24 C23 N2 118.9(3) C28 C23 N2 121.9(3) C28 C23 C24 119.2(3) C23 C24 H24 119.4 C25 C24 C23 121.2(3) C25 C24 H24 119.4 C24 C25 C26 118.5(3) C24 C25 C29 119.7(3) C26 C25 C29 121.8(3) C25 C26 H26 119.2 C27 C26 C25 121.5(3) C27 C26 H26 119.2 C26 C27 C28 118.9(3) C26 C27 C30 121.2(3) C28 C27 C30 119.8(3) C23 C28 C27 120.6(3) C23 C28 H28 119.7 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 N3 C31 H31A 108.6 N3 C31 H31B 108.6 N3 C31 C32 114.8(2) H31A C31 H31B 107.5 C32 C31 H31A 108.6 C32 C31 H31B 108.6 C33 C32 C31 122.3(3) C37 C32 C31 119.7(3) C37 C32 C33 117.9(3) C32 C33 P 118.8(2) C34 C33 P 121.4(2) C34 C33 C32 119.9(3) C33 C34 H34 119.4 C35 C34 C33 121.1(3) C35 C34 H34 119.4 C34 C35 H35 120.4 C36 C35 C34 119.2(3) C36 C35 H35 120.4 C35 C36 H36 119.9 C35 C36 C37 120.1(3) C37 C36 H36 119.9 C32 C37 H37 119.1 C36 C37 C32 121.7(3) C36 C37 H37 119.1 N3 C38 C43 118.9(3) C39 C38 N3 123.8(3) C39 C38 C43 117.3(3) C38 C39 H39 119.3 C40 C39 C38 121.3(3) C40 C39 H39 119.3 C39 C40 C44 119.8(3) C41 C40 C39 119.5(3) C41 C40 C44 120.6(3) C40 C41 H41 119.6 C40 C41 C42 120.8(3) C42 C41 H41 119.6 C41 C42 C45 121.0(3) C43 C42 C41 118.9(3) C43 C42 C45 120.1(3) C38 C43 H43 119.0 C42 C43 C38 122.0(3) C42 C43 H43 119.0 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 F1 C46 S 108.6(2) F2 C46 S 112.8(2) F2 C46 F1 108.0(3) F2 C46 F3 110.4(3) F3 C46 S 109.7(2) F3 C46 F1 107.1(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Nb S 2.9139(8) Nb P 2.5210(8) Nb O1 2.425(2) Nb O2 2.310(2) Nb N1 1.980(2) Nb N2 2.056(2) Nb N3 2.058(2) Nb C1 2.210(3) S O1 1.465(2) S O2 1.483(2) S O3 1.422(2) S C46 1.838(3) P C3 1.818(3) P C18 1.826(3) P C33 1.814(3) F1 C46 1.330(4) F2 C46 1.307(4) F3 C46 1.313(4) N1 C1 1.400(4) N1 C8 1.402(4) N2 C16 1.477(4) N2 C23 1.435(4) N3 C31 1.475(4) N3 C38 1.408(4) C1 H1 1.0000 C1 C2 1.499(4) C2 C3 1.400(4) C2 C7 1.398(4) C3 C4 1.392(4) C4 H4 0.9500 C4 C5 1.402(4) C5 H5 0.9500 C5 C6 1.387(5) C6 H6 0.9500 C6 C7 1.381(5) C7 H7 0.9500 C8 C9 1.397(4) C8 C13 1.402(4) C9 H9 0.9500 C9 C10 1.391(4) C10 C11 1.395(5) C10 C14 1.509(5) C11 H11 0.9500 C11 C12 1.389(5) C12 C13 1.400(4) C12 C15 1.514(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 H16A 0.9900 C16 H16B 0.9900 C16 C17 1.524(4) C17 C18 1.401(4) C17 C22 1.405(4) C18 C19 1.407(4) C19 H19 0.9500 C19 C20 1.387(5) C20 H20 0.9500 C20 C21 1.389(5) C21 H21 0.9500 C21 C22 1.386(5) C22 H22 0.9500 C23 C24 1.397(4) C23 C28 1.393(4) C24 H24 0.9500 C24 C25 1.394(4) C25 C26 1.396(5) C25 C29 1.511(5) C26 H26 0.9500 C26 C27 1.391(5) C27 C28 1.400(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 H31A 0.9900 C31 H31B 0.9900 C31 C32 1.529(4) C32 C33 1.408(4) C32 C37 1.399(4) C33 C34 1.399(4) C34 H34 0.9500 C34 C35 1.393(4) C35 H35 0.9500 C35 C36 1.385(5) C36 H36 0.9500 C36 C37 1.390(5) C37 H37 0.9500 C38 C39 1.406(4) C38 C43 1.413(4) C39 H39 0.9500 C39 C40 1.396(4) C40 C41 1.394(5) C40 C44 1.510(5) C41 H41 0.9500 C41 C42 1.395(5) C42 C43 1.390(4) C42 C45 1.506(5) 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 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 Nb S C46 F1 -121.8(2) Nb S C46 F2 -2.1(3) Nb S C46 F3 121.5(2) Nb P C3 C2 22.8(2) Nb P C3 C4 -151.5(3) Nb P C18 C17 16.1(3) Nb P C18 C19 -165.3(2) Nb P C33 C32 28.3(3) Nb P C33 C34 -152.1(2) Nb N1 C1 C2 106.5(3) Nb N1 C8 C9 -41.8(5) Nb N1 C8 C13 138.7(3) Nb N2 C16 C17 -73.5(3) Nb N2 C23 C24 -59.0(3) Nb N2 C23 C28 122.5(3) Nb N3 C31 C32 84.8(3) Nb N3 C38 C39 -148.4(2) Nb N3 C38 C43 31.6(4) Nb C1 C2 C3 -46.1(3) Nb C1 C2 C7 135.8(3) P C3 C4 C5 174.0(3) P C18 C19 C20 -179.8(3) P C33 C34 C35 -176.7(2) O1 S O2 Nb 3.59(13) O1 S C46 F1 -62.6(3) O1 S C46 F2 57.1(3) O1 S C46 F3 -179.3(2) O2 S O1 Nb -3.39(13) O2 S C46 F1 -176.3(2) O2 S C46 F2 -56.6(3) O2 S C46 F3 67.0(3) O3 S O1 Nb 129.94(12) O3 S O2 Nb -130.75(12) O3 S C46 F1 61.4(3) O3 S C46 F2 -178.9(3) O3 S C46 F3 -55.3(3) N1 C1 C2 C3 -118.5(3) N1 C1 C2 C7 63.4(4) N1 C8 C9 C10 -176.1(3) N1 C8 C13 C12 178.2(3) N2 C16 C17 C18 25.7(4) N2 C16 C17 C22 -158.8(3) N2 C23 C24 C25 179.8(3) N2 C23 C28 C27 179.0(3) N3 C31 C32 C33 -55.3(4) N3 C31 C32 C37 125.5(3) N3 C38 C39 C40 177.8(3) N3 C38 C43 C42 -177.2(3) C1 N1 C8 C9 177.8(3) C1 N1 C8 C13 -1.7(5) C1 C2 C3 P 8.9(3) C1 C2 C3 C4 -176.4(3) C1 C2 C7 C6 175.8(3) C2 C3 C4 C5 0.3(5) C3 P C18 C17 -98.3(2) C3 P C18 C19 80.3(3) C3 P C33 C32 144.2(2) C3 P C33 C34 -36.1(3) C3 C2 C7 C6 -2.3(5) C3 C4 C5 C6 -2.0(5) C4 C5 C6 C7 1.6(5) C5 C6 C7 C2 0.6(5) C7 C2 C3 P -172.8(2) C7 C2 C3 C4 1.9(5) C8 N1 C1 Nb 159.2(3) C8 N1 C1 C2 -94.3(4) C8 C9 C10 C11 -2.3(5) C8 C9 C10 C14 178.1(3) C9 C8 C13 C12 -1.3(4) C9 C10 C11 C12 -1.0(5) C10 C11 C12 C13 3.1(5) C10 C11 C12 C15 -176.1(3) C11 C12 C13 C8 -1.9(5) C13 C8 C9 C10 3.4(5) C14 C10 C11 C12 178.7(3) C15 C12 C13 C8 177.3(3) C16 N2 C23 C24 129.5(3) C16 N2 C23 C28 -49.0(4) C16 C17 C18 P -4.5(4) C16 C17 C18 C19 176.9(3) C16 C17 C22 C21 -176.3(3) C17 C18 C19 C20 -1.2(5) C18 P C3 C2 147.1(2) C18 P C3 C4 -27.2(3) C18 P C33 C32 -104.4(2) C18 P C33 C34 75.3(3) C18 C17 C22 C21 -0.5(5) C18 C19 C20 C21 0.0(5) C19 C20 C21 C22 1.0(5) C20 C21 C22 C17 -0.8(5) C22 C17 C18 P -179.9(2) C22 C17 C18 C19 1.5(4) C23 N2 C16 C17 97.5(3) C23 C24 C25 C26 1.0(5) C23 C24 C25 C29 179.5(3) C24 C23 C28 C27 0.5(5) C24 C25 C26 C27 0.8(5) C25 C26 C27 C28 -1.9(5) C25 C26 C27 C30 178.4(3) C26 C27 C28 C23 1.3(5) C28 C23 C24 C25 -1.6(4) C29 C25 C26 C27 -177.7(3) C30 C27 C28 C23 -179.1(3) C31 N3 C38 C39 19.4(4) C31 N3 C38 C43 -160.6(3) C31 C32 C33 P -2.5(4) C31 C32 C33 C34 177.8(3) C31 C32 C37 C36 -180.0(3) C32 C33 C34 C35 3.0(4) C33 P C3 C2 -100.7(2) C33 P C3 C4 85.0(3) C33 P C18 C17 147.4(2) C33 P C18 C19 -34.0(3) C33 C32 C37 C36 0.7(4) C33 C34 C35 C36 -0.8(5) C34 C35 C36 C37 -1.5(5) C35 C36 C37 C32 1.5(5) C37 C32 C33 P 176.7(2) C37 C32 C33 C34 -2.9(4) C38 N3 C31 C32 -83.2(3) C38 C39 C40 C41 0.1(5) C38 C39 C40 C44 -177.6(3) C39 C38 C43 C42 2.8(4) C39 C40 C41 C42 1.6(5) C40 C41 C42 C43 -1.0(5) C40 C41 C42 C45 176.7(3) C41 C42 C43 C38 -1.2(5) C43 C38 C39 C40 -2.2(4) C44 C40 C41 C42 179.3(3) C45 C42 C43 C38 -178.9(3) C46 S O1 Nb -115.68(12) C46 S O2 Nb 115.25(13) 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 -0.000 -0.000 -0.000 243 28 toluene