#------------------------------------------------------------------------------ #$Date: 2015-06-04 14:02:18 +0300 (Thu, 04 Jun 2015) $ #$Revision: 137925 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/34/31/4343171.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_4343171 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 'C49 H55 N3 Nb P Si' _chemical_formula_sum 'C49 H55 N3 Nb P Si' _chemical_formula_weight 837.93 _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_ms10 _audit_creation_date ; 'Tue Apr 15 16:33:27 2014' ; _audit_update_record 'Tue Apr 15 16:35:49 CEST 2014' _cell_angle_alpha 82.8627(15) _cell_angle_beta 88.6467(15) _cell_angle_gamma 70.9964(16) _cell_formula_units_Z 2 _cell_length_a 10.59319(18) _cell_length_b 13.5033(2) _cell_length_c 16.0085(3) _cell_measurement_reflns_used 14287 _cell_measurement_temperature 110(1) _cell_measurement_theta_max 28.0860 _cell_measurement_theta_min 3.5890 _cell_volume 2147.98(7) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET) (compiled Apr 11 2014,15:12:41) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET) (compiled Apr 11 2014,15:12:41) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET) (compiled Apr 11 2014,15:12:41) ; _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 110(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 0.919 _diffrn_measurement_details ; 1 omega -3.00 24.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.6161 57.0000 60.0000 54 2 omega -10.00 89.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.6161 77.0000 -180.0000 198 3 omega -8.00 50.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.6161 77.0000 -60.0000 116 4 omega -43.00 47.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.6161 -77.0000 60.0000 180 5 omega -1.00 88.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.6161 19.0000 0.0000 178 6 omega -54.00 44.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.6161 -38.0000 -90.0000 196 7 omega -11.00 89.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.6161 77.0000 30.0000 200 8 omega -50.00 40.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.6161 -57.0000 120.0000 180 9 omega -3.00 87.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.6161 57.0000 -90.0000 180 10 omega -52.00 49.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.6161 -77.0000 -30.0000 202 11 omega -3.00 87.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.6161 57.0000 120.0000 180 12 omega -52.00 28.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.6161 -77.0000 -180.0000 160 13 omega -50.00 40.00 0.5000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.6161 -57.0000 -150.0000 180 ; _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 -0.0019412000 _diffrn_orient_matrix_UB_12 -0.0022970000 _diffrn_orient_matrix_UB_13 -0.0439580000 _diffrn_orient_matrix_UB_21 -0.0706493000 _diffrn_orient_matrix_UB_22 0.0147644000 _diffrn_orient_matrix_UB_23 0.0009207000 _diffrn_orient_matrix_UB_31 -0.0046572000 _diffrn_orient_matrix_UB_32 0.0539522000 _diffrn_orient_matrix_UB_33 -0.0078379000 _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 0.0592 _diffrn_reflns_av_unetI/netI 0.0564 _diffrn_reflns_laue_measured_fraction_full 0.998 _diffrn_reflns_laue_measured_fraction_max 0.919 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 48569 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.919 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.972 _diffrn_reflns_theta_min 3.197 _diffrn_source 'microfocus X-Ray tube' _exptl_absorpt_coefficient_mu 0.382 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91444 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET) (compiled Apr 11 2014,15:12:41) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. 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 1.296 _exptl_crystal_description irregular _exptl_crystal_F_000 880 _exptl_crystal_size_max 0.2209 _exptl_crystal_size_mid 0.1142 _exptl_crystal_size_min 0.0311 _refine_diff_density_max 0.483 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.080 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 505 _refine_ls_number_reflns 10476 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0438 _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^)+(0.0202P)^2^+2.1398P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.0857 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8991 _reflns_number_total 10476 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL ba_ms10 - #2018 - in P-1 - superflip - nova CELL 0.71073 10.593193 13.503282 16.008527 82.8627 88.6467 70.9964 ZERR 2 0.00018 0.000236 0.000318 0.0015 0.0015 0.0016 LATT 1 SFAC C H N Nb P Si UNIT 98 110 6 2 2 2 L.S. 10 PLAN 25 SIZE 0.1 0.1 0.1 TEMP -154.15 BOND $H CONF fmap 2 acta REM /struk/ba/ba_ms10/ba_ms10.hkl WGHT 0.020200 2.139800 FVAR 1.46236 NB 4 0.760929 0.220787 0.300181 11.00000 0.01133 0.00966 = 0.01312 -0.00116 0.00057 -0.00353 P 5 0.769053 0.023945 0.324816 11.00000 0.01380 0.01096 = 0.01169 -0.00119 -0.00010 -0.00403 SI 6 0.961660 0.371261 0.357253 11.00000 0.01508 0.01730 = 0.02671 -0.00525 0.00229 -0.00812 N1 3 0.610976 0.292347 0.219886 11.00000 0.01610 0.01136 = 0.01631 0.00061 -0.00211 -0.00436 N2 3 0.911965 0.151740 0.226744 11.00000 0.01595 0.01411 = 0.01336 -0.00105 0.00304 -0.00375 N3 3 0.734152 0.202783 0.429349 11.00000 0.01272 0.01228 = 0.01475 -0.00202 -0.00004 -0.00369 C1 1 0.646441 0.021957 0.247348 11.00000 0.01723 0.01568 = 0.01160 -0.00002 -0.00038 -0.00743 C2 1 0.640560 -0.065221 0.210698 11.00000 0.02684 0.01664 = 0.01877 -0.00121 -0.00264 -0.00834 AFIX 43 H2 2 0.703571 -0.133074 0.226774 11.00000 -1.20000 AFIX 0 C3 1 0.542247 -0.052034 0.150778 11.00000 0.04118 0.02235 = 0.02724 -0.00806 -0.01024 -0.01396 AFIX 43 H3 2 0.537442 -0.111051 0.125901 11.00000 -1.20000 AFIX 0 C4 1 0.450943 0.047137 0.127109 11.00000 0.04002 0.02833 = 0.03223 -0.00202 -0.02025 -0.01330 AFIX 43 H4 2 0.383766 0.055876 0.085955 11.00000 -1.20000 AFIX 0 C5 1 0.457114 0.133750 0.163198 11.00000 0.02688 0.01892 = 0.02916 0.00242 -0.01246 -0.00700 AFIX 43 H5 2 0.393737 0.201331 0.146744 11.00000 -1.20000 AFIX 0 C6 1 0.555112 0.122606 0.223187 11.00000 0.01880 0.01451 = 0.01553 0.00163 -0.00247 -0.00703 C7 1 0.564704 0.213929 0.265090 11.00000 0.01387 0.01334 = 0.01475 0.00155 -0.00138 -0.00308 AFIX 13 H7 2 0.492108 0.240964 0.305708 11.00000 -1.20000 AFIX 0 C8 1 0.531331 0.390040 0.178714 11.00000 0.01848 0.01313 = 0.01461 -0.00014 -0.00216 -0.00346 C9 1 0.392037 0.420526 0.179129 11.00000 0.02234 0.01515 = 0.02048 0.00125 -0.00061 -0.00432 AFIX 43 H9 2 0.349540 0.374700 0.208231 11.00000 -1.20000 AFIX 0 C10 1 0.314819 0.517397 0.137327 11.00000 0.02102 0.01732 = 0.02497 -0.00100 -0.00360 -0.00101 C11 1 0.377604 0.584064 0.095548 11.00000 0.03114 0.01383 = 0.02616 0.00388 -0.00575 -0.00219 AFIX 43 H11 2 0.325148 0.650436 0.067373 11.00000 -1.20000 AFIX 0 C12 1 0.516472 0.555402 0.094149 11.00000 0.03367 0.01754 = 0.01947 0.00255 -0.00157 -0.01040 C13 1 0.592393 0.457984 0.134548 11.00000 0.02124 0.01979 = 0.02011 -0.00015 0.00001 -0.00814 AFIX 43 H13 2 0.687033 0.436986 0.132278 11.00000 -1.20000 AFIX 0 C14 1 0.164413 0.547359 0.134716 11.00000 0.02353 0.02710 = 0.04526 0.00605 -0.00610 0.00184 AFIX 137 H14A 2 0.137922 0.507117 0.095508 11.00000 -1.50000 H14B 2 0.125247 0.623020 0.115839 11.00000 -1.50000 H14C 2 0.132519 0.531375 0.191110 11.00000 -1.50000 AFIX 0 C15 1 0.583365 0.628816 0.047853 11.00000 0.04502 0.02326 = 0.03277 0.00811 -0.00078 -0.01532 AFIX 137 H15A 2 0.529974 0.667099 -0.002332 11.00000 -1.50000 H15B 2 0.672706 0.587639 0.030976 11.00000 -1.50000 H15C 2 0.590789 0.679313 0.084896 11.00000 -1.50000 AFIX 0 C16 1 0.927103 -0.074520 0.303218 11.00000 0.01627 0.01311 = 0.00919 -0.00150 -0.00070 -0.00349 C17 1 0.945367 -0.182594 0.313458 11.00000 0.01977 0.01547 = 0.01658 -0.00037 -0.00105 -0.00514 AFIX 43 H17 2 0.873998 -0.206744 0.333324 11.00000 -1.20000 AFIX 0 C18 1 1.066203 -0.255043 0.295024 11.00000 0.02570 0.01151 = 0.02006 -0.00118 -0.00227 -0.00217 AFIX 43 H18 2 1.077255 -0.328302 0.302008 11.00000 -1.20000 AFIX 0 C19 1 1.170654 -0.220372 0.266431 11.00000 0.01917 0.01666 = 0.01957 -0.00399 -0.00269 0.00108 AFIX 43 H19 2 1.252715 -0.269568 0.252042 11.00000 -1.20000 AFIX 0 C20 1 1.155283 -0.113291 0.258786 11.00000 0.01718 0.01963 = 0.01220 -0.00189 -0.00086 -0.00430 AFIX 43 H20 2 1.228256 -0.090236 0.240640 11.00000 -1.20000 AFIX 0 C21 1 1.034972 -0.039413 0.277240 11.00000 0.01751 0.01445 = 0.00882 -0.00088 -0.00088 -0.00326 C22 1 1.027040 0.075401 0.273974 11.00000 0.01579 0.01698 = 0.01378 -0.00257 0.00094 -0.00651 AFIX 23 H22A 2 1.024370 0.092954 0.332362 11.00000 -1.20000 H22B 2 1.109653 0.083527 0.248389 11.00000 -1.20000 AFIX 0 C23 1 0.923548 0.156603 0.137383 11.00000 0.01891 0.01122 = 0.01425 0.00078 0.00249 0.00026 C24 1 0.835479 0.129190 0.090045 11.00000 0.03207 0.01670 = 0.01634 -0.00019 0.00489 -0.01208 AFIX 43 H24 2 0.765015 0.109647 0.117382 11.00000 -1.20000 AFIX 0 C25 1 0.847602 0.129541 0.003192 11.00000 0.03584 0.01574 = 0.01677 -0.00121 0.00047 -0.00751 C26 1 0.951089 0.159318 -0.035641 11.00000 0.03110 0.02421 = 0.01307 0.00277 0.00383 0.00324 AFIX 43 H26 2 0.961124 0.159550 -0.094785 11.00000 -1.20000 AFIX 0 C27 1 1.039436 0.188520 0.010056 11.00000 0.01703 0.03660 = 0.01958 0.00833 0.00281 0.00007 C28 1 1.025398 0.187382 0.096966 11.00000 0.01553 0.02914 = 0.01863 0.00376 -0.00031 -0.00358 AFIX 43 H28 2 1.085435 0.207649 0.128806 11.00000 -1.20000 AFIX 0 C29 1 0.751907 0.097212 -0.046083 11.00000 0.06637 0.04150 = 0.01933 -0.00498 0.00295 -0.03365 AFIX 137 H29A 2 0.801090 0.034885 -0.073059 11.00000 -1.50000 H29B 2 0.706287 0.155218 -0.089304 11.00000 -1.50000 H29C 2 0.685851 0.080421 -0.008064 11.00000 -1.50000 AFIX 0 C30 1 1.149473 0.222698 -0.033730 11.00000 0.02569 0.09410 = 0.02644 0.01474 0.00373 -0.01936 AFIX 137 H30A 2 1.218135 0.161045 -0.051721 11.00000 -1.50000 H30B 2 1.189359 0.255128 0.005244 11.00000 -1.50000 H30C 2 1.112117 0.274033 -0.083041 11.00000 -1.50000 AFIX 0 C31 1 0.720809 -0.024071 0.427180 11.00000 0.01070 0.01143 = 0.01277 0.00025 -0.00074 -0.00169 C32 1 0.657066 -0.100150 0.440494 11.00000 0.01269 0.01338 = 0.01863 -0.00238 -0.00297 -0.00309 AFIX 43 H32 2 0.634860 -0.128972 0.393928 11.00000 -1.20000 AFIX 0 C33 1 0.625951 -0.133918 0.521434 11.00000 0.01498 0.01562 = 0.02189 0.00252 -0.00088 -0.00621 AFIX 43 H33 2 0.583787 -0.186506 0.530351 11.00000 -1.20000 AFIX 0 C34 1 0.656395 -0.090944 0.588788 11.00000 0.01401 0.01907 = 0.01667 0.00120 0.00184 -0.00404 AFIX 43 H34 2 0.634998 -0.113883 0.644213 11.00000 -1.20000 AFIX 0 C35 1 0.718401 -0.014022 0.575934 11.00000 0.01394 0.01850 = 0.01354 -0.00327 -0.00163 -0.00356 AFIX 43 H35 2 0.738456 0.015267 0.622881 11.00000 -1.20000 AFIX 0 C36 1 0.751508 0.020705 0.495555 11.00000 0.00890 0.01040 = 0.01585 -0.00156 -0.00084 -0.00050 C37 1 0.816483 0.106587 0.481420 11.00000 0.01318 0.01467 = 0.01439 -0.00277 -0.00137 -0.00446 AFIX 23 H37A 2 0.834529 0.125351 0.536732 11.00000 -1.20000 H37B 2 0.903274 0.078380 0.453823 11.00000 -1.20000 AFIX 0 C38 1 0.624427 0.268753 0.469206 11.00000 0.01312 0.01413 = 0.02150 -0.00801 0.00309 -0.00701 C39 1 0.532997 0.354661 0.420714 11.00000 0.01788 0.01420 = 0.02212 -0.00682 0.00092 -0.00769 AFIX 43 H39 2 0.548467 0.367839 0.362331 11.00000 -1.20000 AFIX 0 C40 1 0.420771 0.420930 0.455330 11.00000 0.01638 0.01468 = 0.03585 -0.00981 0.00050 -0.00789 C41 1 0.398295 0.402364 0.540829 11.00000 0.01615 0.02408 = 0.03840 -0.01749 0.00814 -0.00820 AFIX 43 H41 2 0.321479 0.447404 0.564959 11.00000 -1.20000 AFIX 0 C42 1 0.486465 0.319057 0.591237 11.00000 0.02036 0.02590 = 0.02766 -0.01487 0.00873 -0.01368 C43 1 0.598702 0.252622 0.555590 11.00000 0.01865 0.01744 = 0.02072 -0.00701 0.00137 -0.00780 AFIX 43 H43 2 0.658961 0.195366 0.590295 11.00000 -1.20000 AFIX 0 C44 1 0.325085 0.511250 0.400184 11.00000 0.01635 0.02041 = 0.05195 -0.01084 -0.00031 -0.00243 AFIX 137 H44A 2 0.370769 0.528908 0.349399 11.00000 -1.50000 H44B 2 0.293048 0.572805 0.431037 11.00000 -1.50000 H44C 2 0.249116 0.490865 0.384197 11.00000 -1.50000 AFIX 0 C45 1 0.461855 0.301058 0.684302 11.00000 0.02881 0.03861 = 0.02757 -0.01571 0.01090 -0.01382 AFIX 137 H45A 2 0.488639 0.351000 0.713354 11.00000 -1.50000 H45B 2 0.514239 0.228727 0.706769 11.00000 -1.50000 H45C 2 0.366711 0.311762 0.693189 11.00000 -1.50000 AFIX 0 C46 1 0.806319 0.370257 0.307908 11.00000 0.01696 0.01303 = 0.02696 -0.00051 -0.00043 -0.00506 AFIX 23 H46A 2 0.803033 0.405395 0.249538 11.00000 -1.20000 H46B 2 0.731303 0.416287 0.337743 11.00000 -1.20000 AFIX 0 C47 1 0.996354 0.293697 0.464285 11.00000 0.02759 0.03763 = 0.02585 -0.00661 0.00006 -0.01632 AFIX 137 H47A 2 0.915934 0.314207 0.498274 11.00000 -1.50000 H47B 2 1.069221 0.308058 0.491681 11.00000 -1.50000 H47C 2 1.022077 0.218200 0.458959 11.00000 -1.50000 AFIX 0 C48 1 1.109535 0.317219 0.290048 11.00000 0.02288 0.02178 = 0.03530 -0.00303 0.00504 -0.00928 AFIX 137 H48A 2 1.124444 0.242155 0.287370 11.00000 -1.50000 H48B 2 1.188820 0.325647 0.314496 11.00000 -1.50000 H48C 2 1.092637 0.355604 0.233147 11.00000 -1.50000 AFIX 0 C49 1 0.953835 0.510173 0.367777 11.00000 0.01958 0.02516 = 0.06409 -0.01503 0.00551 -0.01226 AFIX 137 H49A 2 0.931224 0.553423 0.312945 11.00000 -1.50000 H49B 2 1.040783 0.510099 0.387436 11.00000 -1.50000 H49C 2 0.885417 0.539450 0.408441 11.00000 -1.50000 AFIX 0 HKLF 4 REM ba_ms10 - #2018 - in P-1 - superflip - nova REM R1 = 0.0438 for 8991 Fo > 4sig(Fo) and 0.0569 for all 10476 data REM 505 parameters refined using 0 restraints END WGHT 0.0203 2.1375 REM Highest difference peak 0.483, deepest hole -0.436, 1-sigma level 0.080 Q1 1 0.7443 0.0067 0.3805 11.00000 0.05 0.48 Q2 1 0.7545 0.2122 0.3799 11.00000 0.05 0.47 Q3 1 0.8793 0.3719 0.3294 11.00000 0.05 0.46 Q4 1 0.7834 0.3060 0.3006 11.00000 0.05 0.45 Q5 1 0.4023 0.4005 0.4910 11.00000 0.05 0.42 Q6 1 0.2271 0.5447 0.4237 11.00000 0.05 0.40 Q7 1 1.0283 0.0163 0.2815 11.00000 0.05 0.39 Q8 1 0.3024 0.4796 0.3507 11.00000 0.05 0.38 Q9 1 0.9128 0.4592 0.3604 11.00000 0.05 0.37 Q10 1 1.1544 0.2190 -0.0926 11.00000 0.05 0.37 Q11 1 0.6051 0.2533 0.5107 11.00000 0.05 0.37 Q12 1 0.9974 0.3413 0.4208 11.00000 0.05 0.36 Q13 1 1.0270 0.3675 0.3074 11.00000 0.05 0.36 Q14 1 0.4838 0.0030 0.1681 11.00000 0.05 0.36 Q15 1 0.8051 0.0510 0.4904 11.00000 0.05 0.35 Q16 1 0.5564 0.4275 0.1486 11.00000 0.05 0.35 Q17 1 0.6091 0.6023 -0.0310 11.00000 0.05 0.35 Q18 1 0.5909 0.3206 0.4539 11.00000 0.05 0.34 Q19 1 0.7590 -0.0128 0.4633 11.00000 0.05 0.34 Q20 1 0.5774 0.1621 0.2394 11.00000 0.05 0.34 Q21 1 1.0829 0.1763 0.1162 11.00000 0.05 0.34 Q22 1 0.6600 0.2096 0.2751 11.00000 0.05 0.34 Q23 1 0.7076 0.0173 0.2794 11.00000 0.05 0.34 Q24 1 1.1700 -0.1666 0.2547 11.00000 0.05 0.33 Q25 1 0.3609 0.4630 0.1431 11.00000 0.05 0.33 ; _cod_data_source_file ic5b00333_si_001.cif _cod_data_source_block ba_ms10 _cod_database_code 4343171 _audit_block_refno 2018 _audit_block_usercomment 'MS261, irregular, orange' _shelxl_version_number 2014-3 _chemical_oxdiff_formula 'C49 H55 N3 Nb P Si' _chemical_oxdiff_usercomment 'MS261, 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 0.963 _shelx_estimated_absorpt_t_min 0.963 _reflns_odcompleteness_completeness 99.83 _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: C7(H7) 2.b Secondary CH2 refined with riding coordinates: C22(H22A,H22B), C37(H37A,H37B), C46(H46A,H46B) 2.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C13(H13), C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C26(H26), C28(H28), C32(H32), C33(H33), C34(H34), C35(H35), 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), C47(H47A,H47B,H47C), C48(H48A, H48B,H48C), C49(H49A,H49B,H49C) ; _shelx_res_checksum 75453 _cell_oxdiff_length_a 10.59319(18) _cell_oxdiff_length_b 13.5033(2) _cell_oxdiff_length_c 16.0085(3) _cell_oxdiff_angle_alpha 82.8627(15) _cell_oxdiff_angle_beta 88.6467(15) _cell_oxdiff_angle_gamma 70.9964(16) _cell_oxdiff_volume 2147.98(7) _cell_oxdiff_measurement_reflns_used 14287 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 0.76093(2) 0.22079(2) 0.30018(2) 0.01137(6) Uani 1 1 d . P P 0.76905(6) 0.02394(4) 0.32482(4) 0.01216(12) Uani 1 1 d . Si Si 0.96166(6) 0.37126(5) 0.35725(4) 0.01880(15) Uani 1 1 d . N1 N 0.61098(18) 0.29235(14) 0.21989(12) 0.0148(4) Uani 1 1 d . N2 N 0.91196(19) 0.15174(15) 0.22674(12) 0.0149(4) Uani 1 1 d . N3 N 0.73415(18) 0.20278(14) 0.42935(11) 0.0133(4) Uani 1 1 d . C1 C 0.6464(2) 0.02196(18) 0.24735(14) 0.0145(5) Uani 1 1 d . C2 C 0.6406(3) -0.06522(19) 0.21070(15) 0.0205(5) Uani 1 1 d . H2 H 0.7036 -0.1331 0.2268 0.025 Uiso 1 1 calc R C3 C 0.5422(3) -0.0520(2) 0.15078(17) 0.0287(6) Uani 1 1 d . H3 H 0.5374 -0.1111 0.1259 0.034 Uiso 1 1 calc R C4 C 0.4509(3) 0.0471(2) 0.12711(18) 0.0328(7) Uani 1 1 d . H4 H 0.3838 0.0559 0.0860 0.039 Uiso 1 1 calc R C5 C 0.4571(3) 0.1338(2) 0.16320(16) 0.0254(6) Uani 1 1 d . H5 H 0.3937 0.2013 0.1467 0.030 Uiso 1 1 calc R C6 C 0.5551(2) 0.12261(18) 0.22319(14) 0.0161(5) Uani 1 1 d . C7 C 0.5647(2) 0.21393(17) 0.26509(14) 0.0146(5) Uani 1 1 d . H7 H 0.4921 0.2410 0.3057 0.017 Uiso 1 1 calc R C8 C 0.5313(2) 0.39004(18) 0.17871(14) 0.0159(5) Uani 1 1 d . C9 C 0.3920(2) 0.42053(18) 0.17913(15) 0.0200(5) Uani 1 1 d . H9 H 0.3495 0.3747 0.2082 0.024 Uiso 1 1 calc R C10 C 0.3148(2) 0.51740(19) 0.13733(16) 0.0225(5) Uani 1 1 d . C11 C 0.3776(3) 0.58406(19) 0.09555(16) 0.0254(6) Uani 1 1 d . H11 H 0.3251 0.6504 0.0674 0.031 Uiso 1 1 calc R C12 C 0.5165(3) 0.55540(19) 0.09415(16) 0.0235(5) Uani 1 1 d . C13 C 0.5924(2) 0.45798(19) 0.13455(15) 0.0202(5) Uani 1 1 d . H13 H 0.6870 0.4370 0.1323 0.024 Uiso 1 1 calc R C14 C 0.1644(3) 0.5474(2) 0.1347(2) 0.0353(7) Uani 1 1 d . H14A H 0.1379 0.5071 0.0955 0.053 Uiso 1 1 calc GR H14B H 0.1252 0.6230 0.1158 0.053 Uiso 1 1 calc GR H14C H 0.1325 0.5314 0.1911 0.053 Uiso 1 1 calc GR C15 C 0.5834(3) 0.6288(2) 0.04785(18) 0.0337(7) Uani 1 1 d . H15A H 0.5300 0.6671 -0.0023 0.050 Uiso 1 1 calc GR H15B H 0.6727 0.5876 0.0310 0.050 Uiso 1 1 calc GR H15C H 0.5908 0.6793 0.0849 0.050 Uiso 1 1 calc GR C16 C 0.9271(2) -0.07452(17) 0.30322(13) 0.0131(4) Uani 1 1 d . C17 C 0.9454(2) -0.18259(18) 0.31346(14) 0.0175(5) Uani 1 1 d . H17 H 0.8740 -0.2067 0.3333 0.021 Uiso 1 1 calc R C18 C 1.0662(2) -0.25504(18) 0.29502(15) 0.0201(5) Uani 1 1 d . H18 H 1.0773 -0.3283 0.3020 0.024 Uiso 1 1 calc R C19 C 1.1707(2) -0.22037(19) 0.26643(15) 0.0200(5) Uani 1 1 d . H19 H 1.2527 -0.2696 0.2520 0.024 Uiso 1 1 calc R C20 C 1.1553(2) -0.11329(18) 0.25879(14) 0.0167(5) Uani 1 1 d . H20 H 1.2283 -0.0902 0.2406 0.020 Uiso 1 1 calc R C21 C 1.0350(2) -0.03941(17) 0.27724(13) 0.0141(5) Uani 1 1 d . C22 C 1.0270(2) 0.07540(17) 0.27397(14) 0.0152(5) Uani 1 1 d . H22A H 1.0244 0.0930 0.3324 0.018 Uiso 1 1 calc R H22B H 1.1097 0.0835 0.2484 0.018 Uiso 1 1 calc R C23 C 0.9235(2) 0.15660(17) 0.13738(14) 0.0163(5) Uani 1 1 d . C24 C 0.8355(3) 0.12919(18) 0.09005(15) 0.0209(5) Uani 1 1 d . H24 H 0.7650 0.1096 0.1174 0.025 Uiso 1 1 calc R C25 C 0.8476(3) 0.12954(19) 0.00319(15) 0.0231(5) Uani 1 1 d . C26 C 0.9511(3) 0.1593(2) -0.03564(16) 0.0263(6) Uani 1 1 d . H26 H 0.9611 0.1595 -0.0948 0.032 Uiso 1 1 calc R C27 C 1.0394(2) 0.1885(2) 0.01006(16) 0.0276(6) Uani 1 1 d . C28 C 1.0254(2) 0.1874(2) 0.09697(15) 0.0226(5) Uani 1 1 d . H28 H 1.0854 0.2076 0.1288 0.027 Uiso 1 1 calc R C29 C 0.7519(3) 0.0972(2) -0.04608(17) 0.0384(7) Uani 1 1 d . H29A H 0.8011 0.0349 -0.0731 0.058 Uiso 1 1 calc GR H29B H 0.7063 0.1552 -0.0893 0.058 Uiso 1 1 calc GR H29C H 0.6859 0.0804 -0.0081 0.058 Uiso 1 1 calc GR C30 C 1.1495(3) 0.2227(3) -0.03373(19) 0.0508(10) Uani 1 1 d . H30A H 1.2181 0.1610 -0.0517 0.076 Uiso 1 1 calc GR H30B H 1.1894 0.2551 0.0052 0.076 Uiso 1 1 calc GR H30C H 1.1121 0.2740 -0.0830 0.076 Uiso 1 1 calc GR C31 C 0.7208(2) -0.02407(17) 0.42718(13) 0.0122(4) Uani 1 1 d . C32 C 0.6571(2) -0.10015(17) 0.44049(14) 0.0151(5) Uani 1 1 d . H32 H 0.6349 -0.1290 0.3939 0.018 Uiso 1 1 calc R C33 C 0.6260(2) -0.13392(18) 0.52143(15) 0.0176(5) Uani 1 1 d . H33 H 0.5838 -0.1865 0.5304 0.021 Uiso 1 1 calc R C34 C 0.6564(2) -0.09094(18) 0.58879(15) 0.0172(5) Uani 1 1 d . H34 H 0.6350 -0.1139 0.6442 0.021 Uiso 1 1 calc R C35 C 0.7184(2) -0.01402(18) 0.57593(14) 0.0156(5) Uani 1 1 d . H35 H 0.7385 0.0153 0.6229 0.019 Uiso 1 1 calc R C36 C 0.7515(2) 0.02070(17) 0.49555(14) 0.0124(4) Uani 1 1 d . C37 C 0.8165(2) 0.10659(17) 0.48142(14) 0.0140(5) Uani 1 1 d . H37A H 0.8345 0.1254 0.5367 0.017 Uiso 1 1 calc R H37B H 0.9033 0.0784 0.4538 0.017 Uiso 1 1 calc R C38 C 0.6244(2) 0.26875(17) 0.46921(15) 0.0151(5) Uani 1 1 d . C39 C 0.5330(2) 0.35466(18) 0.42071(15) 0.0171(5) Uani 1 1 d . H39 H 0.5485 0.3678 0.3623 0.020 Uiso 1 1 calc R C40 C 0.4208(2) 0.42093(18) 0.45533(17) 0.0210(5) Uani 1 1 d . C41 C 0.3983(2) 0.4024(2) 0.54083(17) 0.0247(6) Uani 1 1 d . H41 H 0.3215 0.4474 0.5650 0.030 Uiso 1 1 calc R C42 C 0.4865(2) 0.3191(2) 0.59124(16) 0.0222(5) Uani 1 1 d . C43 C 0.5987(2) 0.25262(19) 0.55559(15) 0.0181(5) Uani 1 1 d . H43 H 0.6590 0.1954 0.5903 0.022 Uiso 1 1 calc R C44 C 0.3251(2) 0.5113(2) 0.40018(19) 0.0299(6) Uani 1 1 d . H44A H 0.3708 0.5289 0.3494 0.045 Uiso 1 1 calc GR H44B H 0.2930 0.5728 0.4310 0.045 Uiso 1 1 calc GR H44C H 0.2491 0.4909 0.3842 0.045 Uiso 1 1 calc GR C45 C 0.4619(3) 0.3011(2) 0.68430(17) 0.0301(6) Uani 1 1 d . H45A H 0.4886 0.3510 0.7134 0.045 Uiso 1 1 calc GR H45B H 0.5142 0.2287 0.7068 0.045 Uiso 1 1 calc GR H45C H 0.3667 0.3118 0.6932 0.045 Uiso 1 1 calc GR C46 C 0.8063(2) 0.37026(18) 0.30791(16) 0.0191(5) Uani 1 1 d . H46A H 0.8030 0.4054 0.2495 0.023 Uiso 1 1 calc R H46B H 0.7313 0.4163 0.3377 0.023 Uiso 1 1 calc R C47 C 0.9964(3) 0.2937(2) 0.46429(16) 0.0287(6) Uani 1 1 d . H47A H 0.9159 0.3142 0.4983 0.043 Uiso 1 1 calc GR H47B H 1.0692 0.3081 0.4917 0.043 Uiso 1 1 calc GR H47C H 1.0221 0.2182 0.4590 0.043 Uiso 1 1 calc GR C48 C 1.1095(3) 0.3172(2) 0.29005(17) 0.0263(6) Uani 1 1 d . H48A H 1.1244 0.2422 0.2874 0.039 Uiso 1 1 calc GR H48B H 1.1888 0.3256 0.3145 0.039 Uiso 1 1 calc GR H48C H 1.0926 0.3556 0.2331 0.039 Uiso 1 1 calc GR C49 C 0.9538(3) 0.5102(2) 0.3678(2) 0.0343(7) Uani 1 1 d . H49A H 0.9312 0.5534 0.3129 0.051 Uiso 1 1 calc GR H49B H 1.0408 0.5101 0.3874 0.051 Uiso 1 1 calc GR H49C H 0.8854 0.5395 0.4084 0.051 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 Nb 0.01133(10) 0.00966(10) 0.01312(10) -0.00116(7) 0.00057(7) -0.00353(8) P 0.0138(3) 0.0110(3) 0.0117(3) -0.0012(2) -0.0001(2) -0.0040(2) Si 0.0151(3) 0.0173(3) 0.0267(4) -0.0053(3) 0.0023(3) -0.0081(3) N1 0.0161(9) 0.0114(9) 0.0163(10) 0.0006(8) -0.0021(8) -0.0044(8) N2 0.0160(9) 0.0141(10) 0.0134(9) -0.0011(8) 0.0030(8) -0.0037(8) N3 0.0127(9) 0.0123(9) 0.0148(9) -0.0020(8) 0.0000(7) -0.0037(8) C1 0.0172(11) 0.0157(11) 0.0116(11) 0.0000(9) -0.0004(9) -0.0074(9) C2 0.0268(13) 0.0166(12) 0.0188(12) -0.0012(10) -0.0026(10) -0.0083(10) C3 0.0412(16) 0.0224(14) 0.0272(14) -0.0081(11) -0.0102(12) -0.0140(12) C4 0.0400(17) 0.0283(15) 0.0322(15) -0.0020(12) -0.0202(13) -0.0133(13) C5 0.0269(14) 0.0189(13) 0.0292(14) 0.0024(11) -0.0125(11) -0.0070(11) C6 0.0188(12) 0.0145(11) 0.0155(11) 0.0016(9) -0.0025(9) -0.0070(10) C7 0.0139(11) 0.0133(11) 0.0147(11) 0.0015(9) -0.0014(9) -0.0031(9) C8 0.0185(11) 0.0131(11) 0.0146(11) -0.0001(9) -0.0022(9) -0.0035(9) C9 0.0223(12) 0.0151(12) 0.0205(12) 0.0012(10) -0.0006(10) -0.0043(10) C10 0.0210(12) 0.0173(12) 0.0250(13) -0.0010(10) -0.0036(10) -0.0010(10) C11 0.0311(14) 0.0138(12) 0.0262(14) 0.0039(10) -0.0058(11) -0.0022(11) C12 0.0337(14) 0.0175(13) 0.0195(12) 0.0026(10) -0.0016(11) -0.0104(11) C13 0.0212(12) 0.0198(13) 0.0201(12) -0.0002(10) 0.0000(10) -0.0081(10) C14 0.0235(14) 0.0271(15) 0.0453(18) 0.0061(13) -0.0061(13) 0.0018(12) C15 0.0450(18) 0.0233(14) 0.0328(16) 0.0081(12) -0.0008(13) -0.0153(13) C16 0.0163(11) 0.0131(11) 0.0092(10) -0.0015(9) -0.0007(9) -0.0035(9) C17 0.0198(12) 0.0155(12) 0.0166(11) -0.0004(9) -0.0010(9) -0.0051(10) C18 0.0257(13) 0.0115(11) 0.0201(12) -0.0012(10) -0.0023(10) -0.0022(10) C19 0.0192(12) 0.0167(12) 0.0196(12) -0.0040(10) -0.0027(10) 0.0011(10) C20 0.0172(11) 0.0196(12) 0.0122(11) -0.0019(9) -0.0009(9) -0.0043(10) C21 0.0175(11) 0.0144(11) 0.0088(10) -0.0009(9) -0.0009(9) -0.0033(9) C22 0.0158(11) 0.0170(12) 0.0138(11) -0.0026(9) 0.0009(9) -0.0065(9) C23 0.0189(12) 0.0112(11) 0.0142(11) 0.0008(9) 0.0025(9) 0.0003(9) C24 0.0321(14) 0.0167(12) 0.0163(12) -0.0002(10) 0.0049(10) -0.0121(11) C25 0.0358(15) 0.0157(12) 0.0168(12) -0.0012(10) 0.0005(11) -0.0075(11) C26 0.0311(14) 0.0242(14) 0.0131(12) 0.0028(10) 0.0038(11) 0.0032(11) C27 0.0170(12) 0.0366(16) 0.0196(13) 0.0083(12) 0.0028(10) 0.0001(11) C28 0.0155(12) 0.0291(14) 0.0186(12) 0.0038(11) -0.0003(10) -0.0036(11) C29 0.066(2) 0.0415(18) 0.0193(14) -0.0050(13) 0.0029(14) -0.0336(17) C30 0.0257(16) 0.094(3) 0.0264(16) 0.0147(17) 0.0037(13) -0.0194(17) C31 0.0107(10) 0.0114(11) 0.0128(11) 0.0002(9) -0.0007(8) -0.0017(9) C32 0.0127(11) 0.0134(11) 0.0186(12) -0.0024(9) -0.0030(9) -0.0031(9) C33 0.0150(11) 0.0156(12) 0.0219(12) 0.0025(10) -0.0009(9) -0.0062(9) C34 0.0140(11) 0.0191(12) 0.0167(11) 0.0012(10) 0.0018(9) -0.0040(9) C35 0.0139(11) 0.0185(12) 0.0135(11) -0.0033(9) -0.0016(9) -0.0036(9) C36 0.0089(10) 0.0104(11) 0.0158(11) -0.0016(9) -0.0008(8) -0.0005(8) C37 0.0132(11) 0.0147(11) 0.0144(11) -0.0028(9) -0.0014(9) -0.0045(9) C38 0.0131(11) 0.0141(11) 0.0215(12) -0.0080(9) 0.0031(9) -0.0070(9) C39 0.0179(11) 0.0142(12) 0.0221(12) -0.0068(10) 0.0009(10) -0.0077(10) C40 0.0164(12) 0.0147(12) 0.0358(15) -0.0098(11) 0.0005(11) -0.0079(10) C41 0.0162(12) 0.0241(14) 0.0384(15) -0.0175(12) 0.0081(11) -0.0082(11) C42 0.0204(12) 0.0259(14) 0.0277(13) -0.0149(11) 0.0087(11) -0.0137(11) C43 0.0187(12) 0.0174(12) 0.0207(12) -0.0070(10) 0.0014(10) -0.0078(10) C44 0.0163(12) 0.0204(14) 0.0520(18) -0.0108(13) -0.0003(12) -0.0024(11) C45 0.0288(14) 0.0386(16) 0.0276(14) -0.0157(13) 0.0109(12) -0.0138(13) C46 0.0170(12) 0.0130(12) 0.0270(13) -0.0005(10) -0.0004(10) -0.0051(10) C47 0.0276(14) 0.0376(16) 0.0259(14) -0.0066(12) 0.0001(11) -0.0163(13) C48 0.0229(13) 0.0218(13) 0.0353(15) -0.0030(12) 0.0050(12) -0.0093(11) C49 0.0196(13) 0.0252(15) 0.064(2) -0.0150(14) 0.0055(13) -0.0123(12) 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' Nb Nb -2.0727 0.6215 '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' Si Si 0.0817 0.0704 '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 -19 2 0.0571 -5.9936 -18.9789 1.9947 -0.0325 0.1451 -1.0117 -13 3 4 0.1068 -12.9809 2.9958 3.9811 -0.1567 0.9650 0.1909 13 -3 -4 0.1068 12.9809 -2.9958 -3.9811 0.1567 -0.9650 -0.1909 6 19 -2 0.0571 5.9936 18.9789 -1.9947 0.0325 -0.1451 1.0117 3 5 22 0.0290 2.9872 4.9935 21.9698 -0.9830 -0.1171 0.0833 2 -17 0 0.0805 1.9949 -16.9806 0.0050 0.0349 -0.3916 -0.9255 -2 17 0 0.0805 -1.9949 16.9806 -0.0050 -0.0349 0.3916 0.9255 -3 -5 -22 0.0020 -2.9872 -4.9935 -21.9698 0.9830 0.1171 -0.0833 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 Nb P 105.25(6) N1 Nb N2 103.77(8) N1 Nb N3 122.27(7) N1 Nb C7 39.31(8) N1 Nb C46 92.49(8) N2 Nb P 77.92(5) N2 Nb N3 132.58(7) N2 Nb C7 115.24(8) N2 Nb C46 98.58(8) N3 Nb P 79.55(5) N3 Nb C7 96.05(8) N3 Nb C46 90.72(8) C7 Nb P 71.71(6) C7 Nb C46 124.51(8) C46 Nb P 162.26(6) C1 P Nb 101.95(7) C16 P Nb 116.42(7) C16 P C1 107.38(10) C31 P Nb 117.39(7) C31 P C1 107.85(10) C31 P C16 105.20(10) C46 Si C47 113.14(12) C46 Si C48 111.12(12) C46 Si C49 110.52(12) C47 Si C48 108.04(12) C47 Si C49 107.86(14) C48 Si C49 105.83(12) C7 N1 Nb 78.94(12) C8 N1 Nb 145.14(16) C8 N1 C7 126.34(19) C22 N2 Nb 113.50(14) C23 N2 Nb 131.89(15) C23 N2 C22 114.37(17) C37 N3 Nb 119.83(13) C38 N3 Nb 122.97(15) C38 N3 C37 116.16(18) C2 C1 P 127.16(18) C2 C1 C6 120.6(2) C6 C1 P 112.17(17) C1 C2 H2 120.2 C3 C2 C1 119.6(2) C3 C2 H2 120.2 C2 C3 H3 120.0 C4 C3 C2 120.1(2) C4 C3 H3 120.0 C3 C4 H4 119.8 C3 C4 C5 120.3(2) C5 C4 H4 119.8 C4 C5 H5 119.7 C4 C5 C6 120.6(2) C6 C5 H5 119.7 C1 C6 C7 118.6(2) C5 C6 C1 118.7(2) C5 C6 C7 122.6(2) Nb C7 H7 114.7 N1 C7 Nb 61.74(11) N1 C7 C6 120.48(19) N1 C7 H7 114.7 C6 C7 Nb 120.21(15) C6 C7 H7 114.7 C9 C8 N1 121.6(2) C9 C8 C13 118.9(2) C13 C8 N1 119.5(2) C8 C9 H9 119.7 C10 C9 C8 120.7(2) C10 C9 H9 119.7 C9 C10 C14 120.2(2) C11 C10 C9 119.3(2) C11 C10 C14 120.4(2) C10 C11 H11 119.4 C10 C11 C12 121.1(2) C12 C11 H11 119.4 C11 C12 C15 120.4(2) C13 C12 C11 119.1(2) C13 C12 C15 120.4(2) C8 C13 H13 119.6 C12 C13 C8 120.8(2) C12 C13 H13 119.6 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 122.48(17) C17 C16 C21 119.3(2) C21 C16 P 118.16(16) C16 C17 H17 119.6 C18 C17 C16 120.9(2) C18 C17 H17 119.6 C17 C18 H18 120.1 C19 C18 C17 119.8(2) C19 C18 H18 120.1 C18 C19 H19 120.1 C18 C19 C20 119.9(2) C20 C19 H19 120.1 C19 C20 H20 119.4 C21 C20 C19 121.2(2) C21 C20 H20 119.4 C16 C21 C22 122.21(19) C20 C21 C16 118.9(2) C20 C21 C22 118.8(2) N2 C22 C21 115.15(18) N2 C22 H22A 108.5 N2 C22 H22B 108.5 C21 C22 H22A 108.5 C21 C22 H22B 108.5 H22A C22 H22B 107.5 C24 C23 N2 120.4(2) C24 C23 C28 119.2(2) C28 C23 N2 120.4(2) C23 C24 H24 119.2 C23 C24 C25 121.5(2) C25 C24 H24 119.2 C24 C25 C26 118.2(2) C24 C25 C29 120.2(2) C26 C25 C29 121.6(2) C25 C26 H26 119.3 C27 C26 C25 121.4(2) C27 C26 H26 119.3 C26 C27 C28 119.3(2) C26 C27 C30 120.5(2) C28 C27 C30 120.2(3) C23 C28 H28 119.9 C27 C28 C23 120.3(2) C27 C28 H28 119.9 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 124.16(17) C32 C31 C36 120.2(2) C36 C31 P 115.60(16) C31 C32 H32 119.8 C33 C32 C31 120.3(2) C33 C32 H32 119.8 C32 C33 H33 120.1 C34 C33 C32 119.8(2) C34 C33 H33 120.1 C33 C34 H34 119.9 C33 C34 C35 120.2(2) C35 C34 H34 119.9 C34 C35 H35 119.4 C36 C35 C34 121.1(2) C36 C35 H35 119.4 C31 C36 C37 120.68(19) C35 C36 C31 118.2(2) C35 C36 C37 121.1(2) N3 C37 C36 113.41(18) N3 C37 H37A 108.9 N3 C37 H37B 108.9 C36 C37 H37A 108.9 C36 C37 H37B 108.9 H37A C37 H37B 107.7 C39 C38 N3 119.0(2) C39 C38 C43 117.2(2) C43 C38 N3 123.8(2) C38 C39 H39 119.0 C40 C39 C38 122.0(2) C40 C39 H39 119.0 C39 C40 C41 119.2(2) C39 C40 C44 119.8(2) C41 C40 C44 121.0(2) C40 C41 H41 119.6 C42 C41 C40 120.8(2) C42 C41 H41 119.6 C41 C42 C43 119.5(2) C41 C42 C45 120.1(2) C43 C42 C45 120.3(2) C38 C43 H43 119.4 C42 C43 C38 121.3(2) C42 C43 H43 119.4 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 Nb C46 H46A 106.7 Nb C46 H46B 106.7 Si C46 Nb 122.33(12) Si C46 H46A 106.7 Si C46 H46B 106.7 H46A C46 H46B 106.6 Si C47 H47A 109.5 Si C47 H47B 109.5 Si C47 H47C 109.5 H47A C47 H47B 109.5 H47A C47 H47C 109.5 H47B C47 H47C 109.5 Si C48 H48A 109.5 Si C48 H48B 109.5 Si C48 H48C 109.5 H48A C48 H48B 109.5 H48A C48 H48C 109.5 H48B C48 H48C 109.5 Si C49 H49A 109.5 Si C49 H49B 109.5 Si C49 H49C 109.5 H49A C49 H49B 109.5 H49A C49 H49C 109.5 H49B C49 H49C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Nb P 2.6115(6) Nb N1 1.9742(19) Nb N2 2.0058(18) Nb N3 2.0755(18) Nb C7 2.200(2) Nb C46 2.240(2) P C1 1.826(2) P C16 1.824(2) P C31 1.811(2) Si C46 1.847(2) Si C47 1.871(3) Si C48 1.875(3) Si C49 1.879(3) N1 C7 1.420(3) N1 C8 1.404(3) N2 C22 1.467(3) N2 C23 1.428(3) N3 C37 1.473(3) N3 C38 1.408(3) C1 C2 1.398(3) C1 C6 1.401(3) C2 H2 0.9500 C2 C3 1.386(3) C3 H3 0.9500 C3 C4 1.386(4) C4 H4 0.9500 C4 C5 1.388(4) C5 H5 0.9500 C5 C6 1.390(3) C6 C7 1.507(3) C7 H7 1.0000 C8 C9 1.397(3) C8 C13 1.401(3) C9 H9 0.9500 C9 C10 1.393(3) C10 C11 1.385(4) C10 C14 1.511(4) C11 H11 0.9500 C11 C12 1.394(4) C12 C13 1.386(3) C12 C15 1.511(3) 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 1.397(3) C16 C21 1.409(3) C17 H17 0.9500 C17 C18 1.386(3) C18 H18 0.9500 C18 C19 1.383(3) C19 H19 0.9500 C19 C20 1.391(3) C20 H20 0.9500 C20 C21 1.391(3) C21 C22 1.519(3) C22 H22A 0.9900 C22 H22B 0.9900 C23 C24 1.382(3) C23 C28 1.396(3) C24 H24 0.9500 C24 C25 1.393(3) C25 C26 1.394(4) C25 C29 1.501(4) C26 H26 0.9500 C26 C27 1.382(4) C27 C28 1.394(3) C27 C30 1.515(4) 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 1.395(3) C31 C36 1.407(3) C32 H32 0.9500 C32 C33 1.388(3) C33 H33 0.9500 C33 C34 1.377(3) C34 H34 0.9500 C34 C35 1.392(3) C35 H35 0.9500 C35 C36 1.391(3) C36 C37 1.522(3) C37 H37A 0.9900 C37 H37B 0.9900 C38 C39 1.402(3) C38 C43 1.407(3) C39 H39 0.9500 C39 C40 1.386(3) C40 C41 1.390(4) C40 C44 1.505(4) C41 H41 0.9500 C41 C42 1.384(4) C42 C43 1.394(3) C42 C45 1.510(3) 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 0.9900 C46 H46B 0.9900 C47 H47A 0.9800 C47 H47B 0.9800 C47 H47C 0.9800 C48 H48A 0.9800 C48 H48B 0.9800 C48 H48C 0.9800 C49 H49A 0.9800 C49 H49B 0.9800 C49 H49C 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 P C1 C2 155.50(19) Nb P C1 C6 -21.97(17) Nb P C16 C17 -179.82(16) Nb P C16 C21 1.8(2) Nb P C31 C32 146.95(16) Nb P C31 C36 -32.95(19) Nb N1 C7 C6 -110.27(19) Nb N1 C8 C9 -129.3(3) Nb N1 C8 C13 52.1(4) Nb N2 C22 C21 98.84(19) Nb N2 C23 C24 -57.2(3) Nb N2 C23 C28 123.9(2) Nb N3 C37 C36 -93.24(19) Nb N3 C38 C39 -4.1(3) Nb N3 C38 C43 174.59(17) P C1 C2 C3 -178.18(19) P C1 C6 C5 178.80(19) P C1 C6 C7 -2.9(3) P C16 C17 C18 178.86(18) P C16 C21 C20 -178.63(17) P C16 C21 C22 5.3(3) P C31 C32 C33 178.74(17) P C31 C36 C35 -179.20(16) P C31 C36 C37 2.1(3) N1 C8 C9 C10 -179.5(2) N1 C8 C13 C12 -179.2(2) N2 C23 C24 C25 -177.6(2) N2 C23 C28 C27 177.7(2) N3 C38 C39 C40 178.1(2) N3 C38 C43 C42 -178.3(2) C1 P C16 C17 -66.4(2) C1 P C16 C21 115.20(18) C1 P C31 C32 32.6(2) C1 P C31 C36 -147.27(16) C1 C2 C3 C4 0.4(4) C1 C6 C7 Nb 35.8(3) C1 C6 C7 N1 108.7(2) C2 C1 C6 C5 1.1(3) C2 C1 C6 C7 179.4(2) C2 C3 C4 C5 -0.1(4) C3 C4 C5 C6 0.3(4) C4 C5 C6 C1 -0.9(4) C4 C5 C6 C7 -179.1(2) C5 C6 C7 Nb -146.0(2) C5 C6 C7 N1 -73.0(3) C6 C1 C2 C3 -0.9(4) C7 N1 C8 C9 0.4(3) C7 N1 C8 C13 -178.2(2) C8 N1 C7 Nb -153.4(2) C8 N1 C7 C6 96.3(3) C8 C9 C10 C11 -0.5(4) C8 C9 C10 C14 177.1(2) C9 C8 C13 C12 2.1(4) C9 C10 C11 C12 0.5(4) C10 C11 C12 C13 0.7(4) C10 C11 C12 C15 179.7(2) C11 C12 C13 C8 -2.1(4) C13 C8 C9 C10 -0.8(4) C14 C10 C11 C12 -177.0(3) C15 C12 C13 C8 179.0(2) C16 P C1 C2 32.6(2) C16 P C1 C6 -144.85(16) C16 P C31 C32 -81.7(2) C16 P C31 C36 98.36(17) C16 C17 C18 C19 0.3(4) C16 C21 C22 N2 -52.3(3) C17 C16 C21 C20 2.9(3) C17 C16 C21 C22 -173.2(2) C17 C18 C19 C20 2.0(4) C18 C19 C20 C21 -1.8(4) C19 C20 C21 C16 -0.7(3) C19 C20 C21 C22 175.5(2) C20 C21 C22 N2 131.6(2) C21 C16 C17 C18 -2.7(3) C22 N2 C23 C24 116.7(2) C22 N2 C23 C28 -62.2(3) C23 N2 C22 C21 -76.2(2) C23 C24 C25 C26 -0.5(4) C23 C24 C25 C29 178.8(2) C24 C23 C28 C27 -1.2(4) C24 C25 C26 C27 -0.4(4) C25 C26 C27 C28 0.5(4) C25 C26 C27 C30 -178.8(3) C26 C27 C28 C23 0.3(4) C28 C23 C24 C25 1.3(4) C29 C25 C26 C27 -179.7(3) C30 C27 C28 C23 179.6(3) C31 P C1 C2 -80.3(2) C31 P C1 C6 102.23(17) C31 P C16 C17 48.3(2) C31 P C16 C21 -130.10(18) C31 C32 C33 C34 1.0(3) C31 C36 C37 N3 61.5(3) C32 C31 C36 C35 0.9(3) C32 C31 C36 C37 -177.78(19) C32 C33 C34 C35 -0.1(3) C33 C34 C35 C36 -0.3(3) C34 C35 C36 C31 -0.1(3) C34 C35 C36 C37 178.6(2) C35 C36 C37 N3 -117.1(2) C36 C31 C32 C33 -1.4(3) C37 N3 C38 C39 -172.42(19) C37 N3 C38 C43 6.3(3) C38 N3 C37 C36 75.5(2) C38 C39 C40 C41 0.5(3) C38 C39 C40 C44 -179.3(2) C39 C38 C43 C42 0.4(3) C39 C40 C41 C42 0.1(4) C40 C41 C42 C43 -0.4(4) C40 C41 C42 C45 179.0(2) C41 C42 C43 C38 0.2(4) C43 C38 C39 C40 -0.7(3) C44 C40 C41 C42 179.9(2) C45 C42 C43 C38 -179.2(2) C47 Si C46 Nb -49.97(18) C48 Si C46 Nb 71.77(16) C49 Si C46 Nb -171.04(14)