# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1b _audit_creation_date 2013-11-18T18:05:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H36 B1 Cl1 N7 Ta1' _chemical_formula_sum 'C21 H36 B Cl N7 Ta' _chemical_formula_weight 613.78 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2722(12) _cell_length_b 14.845(3) _cell_length_c 15.7278(14) _cell_angle_alpha 96.485(9) _cell_angle_beta 94.684(8) _cell_angle_gamma 94.906(12) _cell_volume 2594.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 245 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 16.24 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -2 2 -3 0.154 1 -1 2 0.127 2 -5 -4 0.078 -2 5 4 0.069 -3 -2 -3 0.049 1 3 0 0.128 -1 -8 2 0.114 4 5 -2 0.091 -1 0 2 0.121 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.361 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.162 _exptl_absorpt_correction_T_max 0.208 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1005 _diffrn_reflns_av_unetI/netI 0.1934 _diffrn_reflns_number 15305 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.18 _diffrn_reflns_theta_full 25.18 _diffrn_measured_fraction_theta_full 0.967 _diffrn_measured_fraction_theta_max 0.967 _reflns_number_total 9026 _reflns_number_gt 4897 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 9026 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1416 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1592 _refine_ls_wR_factor_gt 0.1289 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.715 _refine_diff_density_min -1.267 _refine_diff_density_rms 0.198 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta -0.30796(6) 0.72382(5) 0.95894(4) 0.0359(2) Uani 1 1 d . . . Cl1 Cl -0.3036(4) 0.7907(3) 0.8271(2) 0.0505(11) Uani 1 1 d . . . N1 N -0.3269(11) 0.8759(7) 1.0159(8) 0.039(3) Uani 1 1 d . . . N2 N -0.4165(10) 0.8902(8) 1.0745(7) 0.033(3) Uani 1 1 d . . . N3 N -0.5084(11) 0.7187(9) 0.9523(7) 0.043(3) Uani 1 1 d . . . N4 N -0.5691(11) 0.7583(8) 1.0196(8) 0.038(3) Uani 1 1 d . . . N5 N -0.3450(11) 0.6911(9) 1.0915(7) 0.044(3) Uani 1 1 d . . . N6 N -0.4178(11) 0.7421(9) 1.1398(7) 0.039(3) Uani 1 1 d . . . N7 N -0.2846(11) 0.6161(9) 0.9140(8) 0.040(3) Uani 1 1 d . . . B1 B -0.4976(16) 0.8076(12) 1.0985(9) 0.039(4) Uani 1 1 d . . . H1 H -0.5522 0.8299 1.1397 0.046 Uiso 1 1 calc R . . C31 C -0.2962(13) 0.6342(11) 1.1427(9) 0.041(4) Uani 1 1 d . . . C41 C -0.1279(18) 0.5140(14) 0.8950(13) 0.078(7) Uani 1 1 d . . . H41A H -0.123 0.504 0.9544 0.117 Uiso 1 1 calc R . . H41B H -0.0755 0.5667 0.8884 0.117 Uiso 1 1 calc R . . H41C H -0.1046 0.4618 0.861 0.117 Uiso 1 1 calc R . . C50 C -0.1212(14) 0.7568(11) 1.0147(9) 0.043(4) Uani 1 1 d . . . H50A H -0.0876 0.6993 1.0189 0.052 Uiso 1 1 calc R . . H50B H -0.0788 0.7867 0.9728 0.052 Uiso 1 1 calc R . . C23 C -0.6867(14) 0.7421(10) 0.9993(11) 0.043(4) Uani 1 1 d . . . C40 C -0.2579(16) 0.5295(13) 0.8650(10) 0.055(5) Uani 1 1 d . . . C33 C -0.4205(14) 0.7157(11) 1.2187(9) 0.041(4) Uani 1 1 d . . . C21 C -0.5874(18) 0.6843(12) 0.8906(11) 0.056(5) Uani 1 1 d . . . C32 C -0.3428(14) 0.6472(12) 1.2219(10) 0.048(4) Uani 1 1 d . . . H32 H -0.3253 0.616 1.2688 0.058 Uiso 1 1 calc R . . C22 C -0.7059(16) 0.6950(11) 0.9197(11) 0.051(4) Uani 1 1 d . . . H22 H -0.7793 0.6738 0.8898 0.061 Uiso 1 1 calc R . . C13 C -0.4172(14) 0.9807(10) 1.1010(8) 0.037(3) Uani 1 1 d . . . C34 C -0.4913(15) 0.7539(12) 1.2870(10) 0.052(4) Uani 1 1 d . . . H34A H -0.5352 0.801 1.2664 0.079 Uiso 1 1 calc R . . H34B H -0.4385 0.779 1.3365 0.079 Uiso 1 1 calc R . . H34C H -0.5462 0.7066 1.3022 0.079 Uiso 1 1 calc R . . C11 C -0.2757(13) 0.9564(11) 1.0105(9) 0.040(4) Uani 1 1 d . . . C10 C -0.1734(16) 0.9747(11) 0.9572(10) 0.052(4) Uani 1 1 d . . . H10A H -0.1528 0.9181 0.9291 0.078 Uiso 1 1 calc R . . H10B H -0.1056 1.0044 0.9936 0.078 Uiso 1 1 calc R . . H10C H -0.1966 1.0131 0.9148 0.078 Uiso 1 1 calc R . . C12 C -0.3276(16) 1.0264(13) 1.0612(10) 0.055(5) Uani 1 1 d . . . H12 H -0.3063 1.0888 1.0666 0.065 Uiso 1 1 calc R . . C20 C -0.5653(18) 0.6333(12) 0.8068(11) 0.064(5) Uani 1 1 d . . . H20A H -0.4808 0.6354 0.8019 0.096 Uiso 1 1 calc R . . H20B H -0.603 0.6606 0.7605 0.096 Uiso 1 1 calc R . . H20C H -0.5978 0.571 0.8043 0.096 Uiso 1 1 calc R . . C51 C -0.0893(16) 0.8141(13) 1.1000(10) 0.059(5) Uani 1 1 d . . . H51A H -0.0041 0.8204 1.113 0.089 Uiso 1 1 calc R . . H51B H -0.1265 0.7851 1.144 0.089 Uiso 1 1 calc R . . H51C H -0.1171 0.8731 1.0975 0.089 Uiso 1 1 calc R . . C14 C -0.4954(16) 1.0196(13) 1.1605(10) 0.059(5) Uani 1 1 d . . . H14A H -0.5492 0.9721 1.1765 0.088 Uiso 1 1 calc R . . H14B H -0.5404 1.0625 1.1337 0.088 Uiso 1 1 calc R . . H14C H -0.4484 1.0501 1.2109 0.088 Uiso 1 1 calc R . . C30 C -0.2128(15) 0.5682(12) 1.1151(10) 0.055(5) Uani 1 1 d . . . H30A H -0.1948 0.5753 1.0574 0.083 Uiso 1 1 calc R . . H30B H -0.2486 0.5075 1.117 0.083 Uiso 1 1 calc R . . H30C H -0.1403 0.5788 1.1528 0.083 Uiso 1 1 calc R . . C24 C -0.7737(14) 0.7710(12) 1.0587(12) 0.056(5) Uani 1 1 d . . . H24A H -0.7325 0.806 1.1091 0.084 Uiso 1 1 calc R . . H24B H -0.8179 0.7183 1.0746 0.084 Uiso 1 1 calc R . . H24C H -0.8278 0.8076 1.0311 0.084 Uiso 1 1 calc R . . C42 C -0.347(2) 0.4469(13) 0.8792(13) 0.078(6) Uani 1 1 d . . . H42A H -0.4267 0.4585 0.8612 0.117 Uiso 1 1 calc R . . H42B H -0.3408 0.4387 0.939 0.117 Uiso 1 1 calc R . . H42C H -0.3267 0.3929 0.846 0.117 Uiso 1 1 calc R . . C43 C -0.270(2) 0.5395(14) 0.7716(11) 0.082(7) Uani 1 1 d . . . H43A H -0.3515 0.548 0.754 0.122 Uiso 1 1 calc R . . H43B H -0.2477 0.4857 0.7394 0.122 Uiso 1 1 calc R . . H43C H -0.2188 0.5914 0.7611 0.122 Uiso 1 1 calc R . . Ta1A Ta 0.19230(6) 0.79632(4) 0.46907(4) 0.03254(19) Uani 1 1 d . . . Cl1A Cl 0.1927(4) 0.6984(3) 0.3371(2) 0.0509(10) Uani 1 1 d . . . N1A N 0.1906(11) 0.6553(8) 0.5304(8) 0.041(3) Uani 1 1 d . . . N2A N 0.1089(12) 0.6373(10) 0.5867(8) 0.049(4) Uani 1 1 d . . . N3A N -0.0060(10) 0.7636(8) 0.4706(7) 0.033(3) Uani 1 1 d . . . N4A N -0.0565(10) 0.7309(7) 0.5398(7) 0.028(3) Uani 1 1 d . . . N5A N 0.1613(10) 0.8497(8) 0.6027(6) 0.031(3) Uani 1 1 d . . . N6A N 0.0962(11) 0.7996(9) 0.6535(7) 0.042(3) Uani 1 1 d . . . N7A N 0.2010(11) 0.8994(8) 0.4182(7) 0.034(3) Uani 1 1 d . . . B1A B 0.0257(15) 0.7118(13) 0.6156(10) 0.038(4) Uani 1 1 d . . . H1A H -0.0232 0.6896 0.659 0.046 Uiso 1 1 calc R . . C21A C -0.0941(13) 0.7742(11) 0.4130(9) 0.039(4) Uani 1 1 d . . . C31A C 0.2029(13) 0.9283(10) 0.6508(9) 0.037(4) Uani 1 1 d . . . C30A C 0.2811(16) 1.0056(13) 0.6199(10) 0.060(5) Uani 1 1 d . . . H30D H 0.2929 0.99 0.5605 0.089 Uiso 1 1 calc R . . H30E H 0.3571 1.0145 0.6535 0.089 Uiso 1 1 calc R . . H30F H 0.2422 1.0607 0.6264 0.089 Uiso 1 1 calc R . . C32A C 0.1666(15) 0.9275(13) 0.7331(10) 0.052(5) Uani 1 1 d . . . H32A H 0.1836 0.9737 0.7786 0.063 Uiso 1 1 calc R . . C42A C 0.1286(17) 1.0446(13) 0.3885(12) 0.069(6) Uani 1 1 d . . . H42D H 0.0487 1.017 0.3719 0.104 Uiso 1 1 calc R . . H42E H 0.1444 1.0953 0.357 0.104 Uiso 1 1 calc R . . H42F H 0.1369 1.0654 0.449 0.104 Uiso 1 1 calc R . . C41A C 0.2000(19) 0.9373(12) 0.2742(10) 0.068(6) Uani 1 1 d . . . H41D H 0.1194 0.9101 0.2603 0.102 Uiso 1 1 calc R . . H41E H 0.2547 0.8924 0.2621 0.102 Uiso 1 1 calc R . . H41F H 0.2145 0.9864 0.2403 0.102 Uiso 1 1 calc R . . C34A C 0.0353(16) 0.8109(15) 0.8043(10) 0.073(6) Uani 1 1 d . . . H34D H -0.0019 0.7508 0.7842 0.11 Uiso 1 1 calc R . . H34E H -0.0248 0.8503 0.8194 0.11 Uiso 1 1 calc R . . H34F H 0.0901 0.8084 0.8538 0.11 Uiso 1 1 calc R . . C40A C 0.2182(14) 0.9740(11) 0.3690(8) 0.040(4) Uani 1 1 d . . . C22A C -0.2057(13) 0.7483(10) 0.4447(9) 0.036(3) Uani 1 1 d . . . H22A H -0.2817 0.7507 0.4177 0.043 Uiso 1 1 calc R . . C43A C 0.3427(16) 1.0203(13) 0.3921(12) 0.070(6) Uani 1 1 d . . . H43D H 0.3522 1.0434 0.452 0.105 Uiso 1 1 calc R . . H43E H 0.3554 1.0697 0.3584 0.105 Uiso 1 1 calc R . . H43F H 0.4 0.9772 0.3807 0.105 Uiso 1 1 calc R . . C14A C 0.030(2) 0.5077(14) 0.6607(14) 0.087(7) Uani 1 1 d . . . H14D H -0.0226 0.5513 0.6804 0.131 Uiso 1 1 calc R . . H14E H 0.0727 0.4873 0.7093 0.131 Uiso 1 1 calc R . . H14F H -0.0153 0.4567 0.6267 0.131 Uiso 1 1 calc R . . C24A C -0.2581(14) 0.6863(13) 0.5866(9) 0.054(5) Uani 1 1 d . . . H24D H -0.2117 0.6714 0.6361 0.081 Uiso 1 1 calc R . . H24E H -0.3077 0.6332 0.5599 0.081 Uiso 1 1 calc R . . H24F H -0.3075 0.7334 0.6038 0.081 Uiso 1 1 calc R . . C10A C 0.3568(16) 0.5740(12) 0.4684(11) 0.059(5) Uani 1 1 d . . . H10D H 0.3755 0.6289 0.4433 0.088 Uiso 1 1 calc R . . H10E H 0.3361 0.5243 0.4236 0.088 Uiso 1 1 calc R . . H10F H 0.425 0.5614 0.5042 0.088 Uiso 1 1 calc R . . C20A C -0.0771(14) 0.8072(12) 0.3276(9) 0.049(4) Uani 1 1 d . . . H20D H 0.0069 0.8177 0.3214 0.073 Uiso 1 1 calc R . . H20E H -0.1136 0.863 0.3244 0.073 Uiso 1 1 calc R . . H20F H -0.1135 0.7621 0.2824 0.073 Uiso 1 1 calc R . . C51A C 0.4181(13) 0.7822(13) 0.6081(10) 0.051(5) Uani 1 1 d . . . H51D H 0.5031 0.7933 0.6218 0.077 Uiso 1 1 calc R . . H51E H 0.3943 0.7184 0.6072 0.077 Uiso 1 1 calc R . . H51F H 0.3782 0.8164 0.6508 0.077 Uiso 1 1 calc R . . C33A C 0.1023(14) 0.8471(13) 0.7343(9) 0.046(4) Uani 1 1 d . . . C12A C 0.2072(14) 0.5150(12) 0.5692(10) 0.051(4) Uani 1 1 d . . . H12A H 0.234 0.4578 0.5724 0.062 Uiso 1 1 calc R . . C13A C 0.1153(16) 0.5500(11) 0.6089(9) 0.046(4) Uani 1 1 d . . . C11A C 0.2545(15) 0.5853(12) 0.5209(10) 0.049(4) Uani 1 1 d . . . C23A C -0.1770(13) 0.7185(10) 0.5247(9) 0.038(4) Uani 1 1 d . . . C50A C 0.3845(11) 0.8115(10) 0.5200(9) 0.033(3) Uani 1 1 d . . . H50C H 0.4279 0.7772 0.4786 0.039 Uiso 1 1 calc R . . H50D H 0.4137 0.8751 0.5218 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta1 0.0349(4) 0.0464(5) 0.0278(3) 0.0041(3) 0.0028(3) 0.0119(3) Cl1 0.055(3) 0.067(3) 0.0327(19) 0.0100(19) 0.0079(17) 0.019(2) N1 0.032(7) 0.008(6) 0.072(9) 0.005(6) -0.009(6) -0.010(5) N2 0.027(6) 0.046(8) 0.027(6) 0.004(5) 0.008(5) 0.011(6) N3 0.041(8) 0.059(9) 0.032(7) 0.010(6) 0.005(6) 0.017(7) N4 0.031(7) 0.038(8) 0.047(7) 0.006(6) -0.002(6) 0.015(6) N5 0.039(8) 0.058(9) 0.039(7) 0.015(6) 0.004(6) 0.028(7) N6 0.031(7) 0.051(8) 0.035(7) 0.011(6) 0.004(5) 0.003(6) N7 0.030(7) 0.043(8) 0.047(7) 0.008(6) 0.003(6) 0.008(6) B1 0.046(11) 0.049(11) 0.020(7) -0.008(7) -0.004(7) 0.018(9) C31 0.034(9) 0.044(10) 0.042(8) -0.002(7) -0.009(7) 0.009(7) C41 0.077(16) 0.080(16) 0.083(14) 0.001(12) 0.011(11) 0.050(13) C50 0.051(10) 0.050(10) 0.032(8) 0.009(7) 0.018(7) 0.005(8) C23 0.034(9) 0.033(9) 0.064(11) 0.019(8) -0.005(8) 0.009(7) C40 0.051(11) 0.070(13) 0.046(9) 0.007(9) 0.000(8) 0.018(10) C33 0.040(9) 0.048(10) 0.032(8) 0.003(7) -0.004(6) -0.001(8) C21 0.077(14) 0.045(11) 0.046(10) 0.002(8) -0.009(9) 0.027(10) C32 0.044(10) 0.066(12) 0.037(8) 0.014(8) 0.006(7) 0.005(9) C22 0.047(11) 0.038(10) 0.060(11) -0.001(8) -0.019(8) 0.003(8) C13 0.049(10) 0.036(9) 0.023(7) -0.002(6) -0.003(6) 0.004(7) C34 0.046(10) 0.069(12) 0.047(9) 0.010(9) 0.018(8) 0.017(9) C11 0.033(8) 0.055(11) 0.030(7) -0.004(7) -0.002(6) 0.017(8) C10 0.066(12) 0.044(10) 0.047(9) 0.008(8) 0.008(8) 0.005(9) C12 0.054(11) 0.058(12) 0.048(9) 0.009(9) -0.017(8) 0.004(9) C20 0.081(15) 0.062(13) 0.057(11) 0.020(9) 0.015(10) 0.027(11) C51 0.053(12) 0.080(14) 0.047(10) 0.012(9) 0.004(8) 0.015(10) C14 0.063(12) 0.070(13) 0.045(9) -0.002(9) -0.003(8) 0.039(10) C30 0.055(11) 0.062(12) 0.051(10) 0.009(9) 0.002(8) 0.019(9) C24 0.026(9) 0.048(11) 0.093(14) 0.008(10) -0.003(9) 0.000(8) C42 0.090(17) 0.057(13) 0.085(14) -0.004(11) 0.003(12) 0.014(12) C43 0.12(2) 0.071(14) 0.063(13) 0.019(11) 0.024(12) 0.044(14) Ta1A 0.0296(4) 0.0361(4) 0.0320(3) 0.0022(3) 0.0031(3) 0.0057(3) Cl1A 0.058(3) 0.049(3) 0.044(2) -0.0107(19) 0.0119(19) 0.004(2) N1A 0.030(7) 0.030(7) 0.064(8) 0.005(6) 0.005(6) 0.007(6) N2A 0.037(8) 0.069(10) 0.048(8) 0.024(7) 0.010(6) 0.018(7) N3A 0.020(6) 0.046(8) 0.033(6) 0.011(6) -0.004(5) -0.002(5) N4A 0.024(6) 0.027(6) 0.036(6) 0.012(5) 0.003(5) 0.006(5) N5A 0.026(6) 0.045(8) 0.025(6) 0.009(5) 0.004(5) 0.019(6) N6A 0.041(8) 0.047(8) 0.035(7) 0.000(6) -0.003(6) 0.010(6) N7A 0.042(7) 0.031(7) 0.027(6) -0.002(5) -0.003(5) 0.003(6) B1A 0.033(10) 0.058(12) 0.026(8) 0.009(8) 0.004(7) 0.010(9) C21A 0.033(9) 0.048(10) 0.034(8) -0.002(7) -0.003(6) 0.014(7) C31A 0.032(8) 0.042(9) 0.032(8) -0.009(7) -0.008(6) 0.011(7) C30A 0.057(12) 0.071(13) 0.046(10) -0.011(9) -0.009(8) 0.012(10) C32A 0.048(11) 0.068(13) 0.037(9) -0.010(8) -0.011(7) 0.016(9) C42A 0.068(14) 0.077(15) 0.065(12) 0.002(10) 0.000(10) 0.043(11) C41A 0.104(17) 0.056(12) 0.043(10) 0.005(9) 0.011(10) -0.011(11) C34A 0.055(12) 0.13(2) 0.035(9) 0.004(10) -0.003(8) 0.032(12) C40A 0.040(9) 0.046(9) 0.028(7) -0.001(7) 0.004(6) -0.015(7) C22A 0.021(8) 0.040(9) 0.044(8) 0.003(7) -0.003(6) -0.001(6) C43A 0.052(12) 0.072(14) 0.089(14) 0.040(11) -0.002(10) -0.006(10) C14A 0.085(17) 0.079(16) 0.105(17) 0.046(14) 0.016(13) 0.000(13) C24A 0.029(9) 0.092(14) 0.042(9) 0.015(9) 0.002(7) 0.007(9) C10A 0.058(12) 0.052(11) 0.068(11) 0.000(9) 0.009(9) 0.020(9) C20A 0.038(9) 0.062(11) 0.041(8) 0.011(8) -0.008(7) -0.026(8) C51A 0.010(7) 0.083(14) 0.055(10) -0.005(9) -0.006(7) 0.000(8) C33A 0.033(9) 0.081(14) 0.027(8) 0.012(8) -0.004(6) 0.020(9) C12A 0.041(10) 0.054(11) 0.064(11) 0.016(9) 0.008(8) 0.016(8) C13A 0.060(11) 0.041(10) 0.038(8) 0.011(7) 0.005(8) 0.004(8) C11A 0.042(10) 0.054(11) 0.048(9) -0.001(8) -0.005(7) 0.009(8) C23A 0.029(9) 0.041(10) 0.045(9) 0.007(7) 0.001(7) 0.003(7) C50A 0.016(7) 0.031(8) 0.045(8) -0.006(7) -0.012(6) -0.006(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N7 1.725(12) . ? Ta1 C50 2.206(16) . ? Ta1 N3 2.248(13) . ? Ta1 N5 2.257(12) . ? Ta1 N1 2.367(11) . ? Ta1 Cl1 2.400(4) . ? N1 C11 1.297(19) . ? N1 N2 1.436(16) . ? N2 C13 1.361(18) . ? N2 B1 1.56(2) . ? N3 C21 1.29(2) . ? N3 N4 1.408(16) . ? N4 C23 1.332(19) . ? N4 B1 1.502(19) . ? N5 C31 1.351(18) . ? N5 N6 1.380(16) . ? N6 C33 1.345(18) . ? N6 B1 1.54(2) . ? N7 C40 1.49(2) . ? C31 C32 1.39(2) . ? C31 C30 1.47(2) . ? C41 C40 1.55(2) . ? C50 C51 1.50(2) . ? C23 C22 1.35(2) . ? C23 C24 1.47(2) . ? C40 C43 1.49(2) . ? C40 C42 1.56(3) . ? C33 C32 1.40(2) . ? C33 C34 1.48(2) . ? C21 C22 1.46(2) . ? C21 C20 1.49(2) . ? C13 C12 1.40(2) . ? C13 C14 1.44(2) . ? C11 C12 1.43(2) . ? C11 C10 1.50(2) . ? Ta1A N7A 1.803(11) . ? Ta1A N5A 2.228(10) . ? Ta1A C50A 2.231(12) . ? Ta1A N3A 2.249(11) . ? Ta1A Cl1A 2.396(4) . ? Ta1A N1A 2.401(12) . ? N1A C11A 1.316(19) . ? N1A N2A 1.360(17) . ? N2A C13A 1.39(2) . ? N2A B1A 1.56(2) . ? N3A C21A 1.321(17) . ? N3A N4A 1.385(15) . ? N4A C23A 1.353(17) . ? N4A B1A 1.518(19) . ? N5A C31A 1.343(18) . ? N5A N6A 1.366(17) . ? N6A C33A 1.376(18) . ? N6A B1A 1.50(2) . ? N7A C40A 1.431(18) . ? C21A C22A 1.43(2) . ? C21A C20A 1.50(2) . ? C31A C32A 1.39(2) . ? C31A C30A 1.53(2) . ? C32A C33A 1.35(2) . ? C42A C40A 1.54(2) . ? C41A C40A 1.52(2) . ? C34A C33A 1.51(2) . ? C40A C43A 1.51(2) . ? C22A C23A 1.40(2) . ? C14A C13A 1.46(2) . ? C24A C23A 1.48(2) . ? C10A C11A 1.48(2) . ? C51A C50A 1.53(2) . ? C12A C13A 1.36(2) . ? C12A C11A 1.45(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Ta1 C50 94.1(6) . . ? N7 Ta1 N3 102.8(5) . . ? C50 Ta1 N3 157.6(5) . . ? N7 Ta1 N5 98.6(5) . . ? C50 Ta1 N5 85.2(5) . . ? N3 Ta1 N5 78.0(4) . . ? N7 Ta1 N1 175.6(5) . . ? C50 Ta1 N1 83.0(5) . . ? N3 Ta1 N1 80.8(5) . . ? N5 Ta1 N1 84.5(5) . . ? N7 Ta1 Cl1 95.2(4) . . ? C50 Ta1 Cl1 101.3(4) . . ? N3 Ta1 Cl1 91.7(3) . . ? N5 Ta1 Cl1 164.3(3) . . ? N1 Ta1 Cl1 82.2(3) . . ? C11 N1 N2 105.2(11) . . ? C11 N1 Ta1 137.7(11) . . ? N2 N1 Ta1 117.2(8) . . ? C13 N2 N1 110.3(11) . . ? C13 N2 B1 129.2(12) . . ? N1 N2 B1 120.5(11) . . ? C21 N3 N4 107.8(13) . . ? C21 N3 Ta1 129.5(12) . . ? N4 N3 Ta1 122.6(9) . . ? C23 N4 N3 109.5(13) . . ? C23 N4 B1 131.5(13) . . ? N3 N4 B1 119.0(12) . . ? C31 N5 N6 107.2(11) . . ? C31 N5 Ta1 131.7(10) . . ? N6 N5 Ta1 120.5(9) . . ? C33 N6 N5 110.7(12) . . ? C33 N6 B1 127.6(13) . . ? N5 N6 B1 121.0(11) . . ? C40 N7 Ta1 171.9(11) . . ? N4 B1 N6 109.6(12) . . ? N4 B1 N2 110.4(12) . . ? N6 B1 N2 109.0(13) . . ? N5 C31 C32 108.1(13) . . ? N5 C31 C30 124.1(13) . . ? C32 C31 C30 127.7(15) . . ? C51 C50 Ta1 122.1(11) . . ? N4 C23 C22 108.4(15) . . ? N4 C23 C24 122.3(15) . . ? C22 C23 C24 129.2(16) . . ? N7 C40 C43 108.6(15) . . ? N7 C40 C41 106.9(14) . . ? C43 C40 C41 110.7(16) . . ? N7 C40 C42 112.3(15) . . ? C43 C40 C42 107.5(17) . . ? C41 C40 C42 110.9(16) . . ? N6 C33 C32 106.0(13) . . ? N6 C33 C34 125.6(15) . . ? C32 C33 C34 128.4(14) . . ? N3 C21 C22 108.2(14) . . ? N3 C21 C20 127.1(18) . . ? C22 C21 C20 124.5(17) . . ? C31 C32 C33 107.9(14) . . ? C23 C22 C21 105.9(14) . . ? N2 C13 C12 107.0(13) . . ? N2 C13 C14 125.3(15) . . ? C12 C13 C14 127.7(16) . . ? N1 C11 C12 112.4(15) . . ? N1 C11 C10 124.0(14) . . ? C12 C11 C10 123.6(16) . . ? C13 C12 C11 105.2(15) . . ? N7A Ta1A N5A 101.4(4) . . ? N7A Ta1A C50A 95.0(5) . . ? N5A Ta1A C50A 84.4(5) . . ? N7A Ta1A N3A 102.5(5) . . ? N5A Ta1A N3A 77.5(4) . . ? C50A Ta1A N3A 156.9(5) . . ? N7A Ta1A Cl1A 94.1(3) . . ? N5A Ta1A Cl1A 162.5(3) . . ? C50A Ta1A Cl1A 102.5(4) . . ? N3A Ta1A Cl1A 91.3(3) . . ? N7A Ta1A N1A 176.1(5) . . ? N5A Ta1A N1A 81.9(4) . . ? C50A Ta1A N1A 83.1(5) . . ? N3A Ta1A N1A 80.2(4) . . ? Cl1A Ta1A N1A 83.0(3) . . ? C11A N1A N2A 107.8(13) . . ? C11A N1A Ta1A 133.3(11) . . ? N2A N1A Ta1A 118.9(9) . . ? N1A N2A C13A 110.1(12) . . ? N1A N2A B1A 119.4(13) . . ? C13A N2A B1A 130.5(13) . . ? C21A N3A N4A 107.6(11) . . ? C21A N3A Ta1A 129.7(10) . . ? N4A N3A Ta1A 122.6(8) . . ? C23A N4A N3A 110.6(10) . . ? C23A N4A B1A 130.8(12) . . ? N3A N4A B1A 118.6(11) . . ? C31A N5A N6A 106.9(11) . . ? C31A N5A Ta1A 130.7(10) . . ? N6A N5A Ta1A 122.3(9) . . ? N5A N6A C33A 108.7(13) . . ? N5A N6A B1A 120.1(11) . . ? C33A N6A B1A 131.0(14) . . ? C40A N7A Ta1A 171.4(10) . . ? N6A B1A N4A 108.3(13) . . ? N6A B1A N2A 111.8(13) . . ? N4A B1A N2A 110.4(12) . . ? N3A C21A C22A 109.2(13) . . ? N3A C21A C20A 124.4(14) . . ? C22A C21A C20A 126.4(13) . . ? N5A C31A C32A 109.4(15) . . ? N5A C31A C30A 125.0(13) . . ? C32A C31A C30A 125.6(15) . . ? C33A C32A C31A 107.0(15) . . ? N7A C40A C43A 109.1(13) . . ? N7A C40A C41A 108.5(12) . . ? C43A C40A C41A 110.8(14) . . ? N7A C40A C42A 111.0(13) . . ? C43A C40A C42A 108.2(15) . . ? C41A C40A C42A 109.3(14) . . ? C23A C22A C21A 105.9(12) . . ? C32A C33A N6A 107.9(14) . . ? C32A C33A C34A 130.5(16) . . ? N6A C33A C34A 121.3(17) . . ? C13A C12A C11A 105.7(15) . . ? C12A C13A N2A 107.0(14) . . ? C12A C13A C14A 130.1(17) . . ? N2A C13A C14A 122.8(16) . . ? N1A C11A C12A 109.2(15) . . ? N1A C11A C10A 128.1(16) . . ? C12A C11A C10A 122.7(15) . . ? N4A C23A C22A 106.6(12) . . ? N4A C23A C24A 124.3(13) . . ? C22A C23A C24A 129.0(14) . . ? C51A C50A Ta1A 118.8(9) . . ? _database_code_depnum_ccdc_archive 'CCDC 902489' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2a _audit_creation_date 2013-11-06T13:19:23-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C26 H38 B1 Cl1 N7 Nb1' _chemical_formula_sum 'C26 H38 B Cl N7 Nb' _chemical_formula_weight 587.8 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _space_group_IT_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6170(13) _cell_length_b 11.2000(9) _cell_length_c 14.3110(15) _cell_angle_alpha 96.911(11) _cell_angle_beta 97.518(12) _cell_angle_gamma 107.041(9) _cell_volume 1590.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 223 _cell_measurement_theta_min 3.45 _cell_measurement_theta_max 16.45 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2 4 -3 0.109 4 -3 1 0.151 -4 1 0 0.126 1 -2 -10 0.046 -2 3 13 0.069 -4 -1 3 0.156 4 -7 3 0.162 -5 6 -2 0.137 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.487 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 1.123 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_unetI/netI 0.1634 _diffrn_reflns_number 13551 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 27.4 _diffrn_reflns_theta_full 27.4 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 7195 _reflns_number_gt 3695 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR2002 (Giacovazzo et al, 2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1212P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7195 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1408 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.2268 _refine_ls_wR_factor_gt 0.1816 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.905 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.261 _refine_diff_density_min -1.29 _refine_diff_density_rms 0.126 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 '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' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.73609(6) 0.03448(6) 0.79735(3) 0.0442(2) Uani 1 1 d . . . Cl1 Cl 0.6368(3) 0.1814(3) 0.80592(17) 0.0993(8) Uani 1 1 d . . . B1 B 0.5799(8) -0.2650(8) 0.8375(5) 0.0531(18) Uani 1 1 d . . . N1 N 0.5181(5) -0.1155(5) 0.7373(3) 0.0487(12) Uani 1 1 d . . . N2 N 0.4847(5) -0.2311(5) 0.7648(3) 0.0490(12) Uani 1 1 d . . . N3 N 0.6745(5) -0.0432(5) 0.9296(3) 0.0429(11) Uani 1 1 d . . . N4 N 0.6143(5) -0.1699(5) 0.9296(3) 0.0456(12) Uani 1 1 d . . . N5 N 0.7975(5) -0.1522(5) 0.7840(3) 0.0472(12) Uani 1 1 d . . . N6 N 0.7100(5) -0.2636(5) 0.7995(3) 0.0479(12) Uani 1 1 d . . . N7 N 0.9099(6) 0.1314(5) 0.8463(4) 0.0544(14) Uani 1 1 d . . . C10 C 0.4021(9) 0.0002(10) 0.6343(7) 0.086(3) Uani 1 1 d . . . H10A H 0.4867 0.066 0.6528 0.129 Uiso 1 1 calc R . . H10B H 0.3332 0.0304 0.6558 0.129 Uiso 1 1 calc R . . H10C H 0.3825 -0.0231 0.566 0.129 Uiso 1 1 calc R . . C11 C 0.4083(7) -0.1121(9) 0.6784(5) 0.065(2) Uani 1 1 d . . . C12 C 0.3079(7) -0.2238(9) 0.6693(5) 0.068(2) Uani 1 1 d . . . H12 H 0.2229 -0.2451 0.6329 0.081 Uiso 1 1 calc R . . C13 C 0.3558(7) -0.2987(8) 0.7239(5) 0.0603(18) Uani 1 1 d . . . C14 C 0.2884(9) -0.4285(9) 0.7436(7) 0.089(3) Uani 1 1 d . . . H14A H 0.3505 -0.4542 0.7852 0.133 Uiso 1 1 calc R . . H14B H 0.2586 -0.4873 0.6845 0.133 Uiso 1 1 calc R . . H14C H 0.2129 -0.4273 0.7735 0.133 Uiso 1 1 calc R . . C20 C 0.7398(7) 0.1579(7) 1.0467(4) 0.0556(17) Uani 1 1 d . . . H20A H 0.7693 0.1944 0.9929 0.083 Uiso 1 1 calc R . . H20B H 0.8143 0.1786 1.0983 0.083 Uiso 1 1 calc R . . H20C H 0.6722 0.1911 1.0668 0.083 Uiso 1 1 calc R . . C21 C 0.6836(6) 0.0178(7) 1.0189(4) 0.0463(14) Uani 1 1 d . . . C22 C 0.6299(6) -0.0704(7) 1.0754(4) 0.0500(15) Uani 1 1 d . . . H22 H 0.6243 -0.0537 1.1397 0.06 Uiso 1 1 calc R . . C23 C 0.5874(6) -0.1853(7) 1.0184(4) 0.0531(16) Uani 1 1 d . . . C24 C 0.5234(8) -0.3127(8) 1.0426(5) 0.070(2) Uani 1 1 d . . . H24A H 0.5048 -0.3761 0.9868 0.105 Uiso 1 1 calc R . . H24B H 0.4414 -0.3141 1.0646 0.105 Uiso 1 1 calc R . . H24C H 0.5829 -0.3297 1.092 0.105 Uiso 1 1 calc R . . C30 C 1.0185(7) -0.0855(8) 0.7335(6) 0.0661(19) Uani 1 1 d . . . H30A H 1.0042 -0.0043 0.7404 0.099 Uiso 1 1 calc R . . H30B H 1.0291 -0.1091 0.669 0.099 Uiso 1 1 calc R . . H30C H 1.0977 -0.0808 0.7766 0.099 Uiso 1 1 calc R . . C31 C 0.9013(6) -0.1818(7) 0.7559(4) 0.0506(15) Uani 1 1 d . . . C32 C 0.8834(7) -0.3085(8) 0.7546(5) 0.0603(18) Uani 1 1 d . . . H32 H 0.9424 -0.3514 0.7384 0.072 Uiso 1 1 calc R . . C33 C 0.7628(8) -0.3600(8) 0.7817(5) 0.0607(18) Uani 1 1 d . . . C34 C 0.6946(9) -0.4902(9) 0.7940(7) 0.080(2) Uani 1 1 d . . . H34A H 0.6105 -0.4944 0.8136 0.121 Uiso 1 1 calc R . . H34B H 0.7494 -0.5148 0.842 0.121 Uiso 1 1 calc R . . H34C H 0.6792 -0.5464 0.7346 0.121 Uiso 1 1 calc R . . C40 C 1.0259(6) 0.2420(7) 0.8826(4) 0.0519(15) Uani 1 1 d . . . C41 C 1.0932(8) 0.2271(12) 0.9788(6) 0.097(3) Uani 1 1 d . . . H41A H 1.0306 0.2167 1.0222 0.146 Uiso 1 1 calc R . . H41B H 1.1686 0.3012 1.0039 0.146 Uiso 1 1 calc R . . H41C H 1.123 0.154 0.9711 0.146 Uiso 1 1 calc R . . C42 C 0.9768(10) 0.3567(9) 0.8937(8) 0.093(3) Uani 1 1 d . . . H42A H 0.9343 0.3653 0.8326 0.14 Uiso 1 1 calc R . . H42B H 1.0513 0.4315 0.9189 0.14 Uiso 1 1 calc R . . H42C H 0.9137 0.3457 0.9368 0.14 Uiso 1 1 calc R . . C43 C 1.1228(8) 0.2589(8) 0.8122(5) 0.068(2) Uani 1 1 d . . . H43A H 1.0786 0.2685 0.752 0.101 Uiso 1 1 calc R . . H43B H 1.1526 0.1859 0.8036 0.101 Uiso 1 1 calc R . . H43C H 1.1984 0.333 0.8367 0.101 Uiso 1 1 calc R . . C50 C 0.7492(7) 0.0222(7) 0.6396(4) 0.0541(17) Uani 1 1 d . . . H50A H 0.7816 -0.0482 0.6217 0.065 Uiso 1 1 calc R . . H50B H 0.659 0.0012 0.6042 0.065 Uiso 1 1 calc R . . C51 C 0.8328(7) 0.1334(8) 0.6069(4) 0.0595(18) Uani 1 1 d . . . C52 C 0.8045(9) 0.2470(8) 0.6134(5) 0.070(2) Uani 1 1 d . . . H52 H 0.7302 0.2535 0.639 0.085 Uiso 1 1 calc R . . C53 C 0.9950(11) 0.3394(12) 0.5434(6) 0.104(4) Uani 1 1 d . . . H53 H 1.0505 0.4084 0.5228 0.125 Uiso 1 1 calc R . . C54 C 1.0218(10) 0.2294(12) 0.5353(6) 0.087(3) Uani 1 1 d . . . H54 H 1.095 0.2224 0.5085 0.104 Uiso 1 1 calc R . . C55 C 0.9422(8) 0.1273(9) 0.5663(5) 0.070(2) Uani 1 1 d . . . H55 H 0.9624 0.0516 0.5598 0.084 Uiso 1 1 calc R . . C59 C 0.8851(11) 0.3516(9) 0.5823(6) 0.085(3) Uani 1 1 d . . . H59 H 0.8659 0.4277 0.5875 0.103 Uiso 1 1 calc R . . H1 H 0.5403 -0.3593 0.851 0.04 Uiso 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 Nb1 0.0430(3) 0.0598(4) 0.0272(2) 0.0101(2) 0.00043(18) 0.0131(2) Cl1 0.124(2) 0.1011(19) 0.0682(13) 0.0181(12) 0.0169(13) 0.0261(16) B1 0.047(4) 0.064(5) 0.046(4) 0.008(3) 0.005(3) 0.014(4) N1 0.048(3) 0.061(4) 0.035(2) 0.010(2) 0.001(2) 0.017(3) N2 0.042(3) 0.059(4) 0.037(2) 0.002(2) 0.002(2) 0.007(2) N3 0.037(3) 0.061(3) 0.029(2) 0.010(2) 0.0010(18) 0.014(2) N4 0.040(3) 0.063(4) 0.036(2) 0.019(2) 0.007(2) 0.015(2) N5 0.049(3) 0.059(3) 0.042(3) 0.016(2) 0.009(2) 0.026(3) N6 0.046(3) 0.059(4) 0.040(2) 0.008(2) 0.004(2) 0.020(3) N7 0.058(3) 0.058(4) 0.038(3) 0.003(2) 0.009(2) 0.006(3) C10 0.062(5) 0.125(8) 0.087(6) 0.049(6) 0.007(4) 0.043(5) C11 0.043(4) 0.110(7) 0.044(3) 0.020(4) 0.000(3) 0.027(4) C12 0.041(4) 0.102(6) 0.048(4) -0.002(4) -0.007(3) 0.016(4) C13 0.047(4) 0.075(5) 0.048(3) -0.010(3) 0.006(3) 0.013(3) C14 0.059(5) 0.082(7) 0.094(6) -0.003(5) 0.000(4) -0.011(4) C20 0.057(4) 0.075(5) 0.034(3) 0.001(3) 0.007(3) 0.021(3) C21 0.034(3) 0.071(4) 0.036(3) 0.014(3) 0.001(2) 0.019(3) C22 0.051(4) 0.069(5) 0.032(3) 0.006(3) 0.005(2) 0.023(3) C23 0.044(3) 0.082(5) 0.038(3) 0.022(3) 0.006(3) 0.022(3) C24 0.077(5) 0.076(5) 0.055(4) 0.028(4) 0.012(4) 0.013(4) C30 0.053(4) 0.079(5) 0.074(5) 0.020(4) 0.018(3) 0.025(4) C31 0.046(3) 0.061(4) 0.043(3) 0.008(3) 0.006(3) 0.016(3) C32 0.055(4) 0.075(5) 0.054(4) 0.006(3) 0.007(3) 0.030(4) C33 0.065(5) 0.071(5) 0.047(3) 0.009(3) 0.003(3) 0.024(4) C34 0.074(5) 0.079(6) 0.089(6) 0.021(5) 0.009(5) 0.024(5) C40 0.048(4) 0.064(4) 0.040(3) 0.006(3) -0.001(3) 0.016(3) C41 0.054(5) 0.178(11) 0.054(4) 0.028(5) 0.002(4) 0.028(6) C42 0.083(6) 0.064(6) 0.130(9) 0.009(5) 0.033(6) 0.015(5) C43 0.063(5) 0.076(5) 0.056(4) 0.009(3) 0.009(3) 0.010(4) C50 0.058(4) 0.079(5) 0.020(2) 0.006(3) 0.002(2) 0.016(3) C51 0.061(4) 0.089(6) 0.027(3) 0.013(3) 0.001(3) 0.023(4) C52 0.088(6) 0.086(6) 0.042(3) 0.020(4) 0.012(4) 0.031(5) C53 0.102(8) 0.120(9) 0.054(5) 0.037(5) 0.004(5) -0.024(7) C54 0.073(6) 0.121(9) 0.062(5) 0.034(5) 0.014(4) 0.016(6) C55 0.072(5) 0.093(6) 0.052(4) 0.019(4) 0.016(4) 0.033(5) C59 0.125(8) 0.080(6) 0.047(4) 0.020(4) 0.015(5) 0.021(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 N7 1.838(6) . ? Nb1 Cl1 2.199(3) . ? Nb1 C50 2.270(5) . ? Nb1 N3 2.270(5) . ? Nb1 N5 2.360(5) . ? Nb1 N1 2.402(5) . ? B1 N2 1.514(9) . ? B1 N4 1.521(9) . ? B1 N6 1.545(9) . ? N1 N2 1.359(8) . ? N1 C11 1.360(8) . ? N2 C13 1.366(8) . ? N3 C21 1.352(7) . ? N3 N4 1.375(7) . ? N4 C23 1.359(7) . ? N5 C31 1.335(8) . ? N5 N6 1.382(8) . ? N6 C33 1.368(9) . ? N7 C40 1.452(8) . ? C10 C11 1.488(12) . ? C11 C12 1.364(11) . ? C12 C13 1.371(11) . ? C13 C14 1.498(12) . ? C20 C21 1.489(10) . ? C21 C22 1.391(9) . ? C22 C23 1.354(10) . ? C23 C24 1.493(10) . ? C30 C31 1.489(10) . ? C31 C32 1.372(10) . ? C32 C33 1.368(11) . ? C33 C34 1.470(12) . ? C40 C41 1.517(10) . ? C40 C43 1.520(10) . ? C40 C42 1.520(12) . ? C50 C51 1.469(10) . ? C51 C55 1.380(11) . ? C51 C52 1.386(11) . ? C52 C59 1.392(12) . ? C53 C54 1.338(16) . ? C53 C59 1.392(15) . ? C54 C55 1.368(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Nb1 Cl1 100.2(2) . . ? N7 Nb1 C50 98.3(2) . . ? Cl1 Nb1 C50 97.2(2) . . ? N7 Nb1 N3 99.9(2) . . ? Cl1 Nb1 N3 96.39(14) . . ? C50 Nb1 N3 154.9(2) . . ? N7 Nb1 N5 91.2(2) . . ? Cl1 Nb1 N5 168.21(16) . . ? C50 Nb1 N5 84.2(2) . . ? N3 Nb1 N5 78.41(18) . . ? N7 Nb1 N1 172.5(2) . . ? Cl1 Nb1 N1 86.97(15) . . ? C50 Nb1 N1 82.8(2) . . ? N3 Nb1 N1 76.97(17) . . ? N5 Nb1 N1 81.57(19) . . ? N2 B1 N4 109.4(6) . . ? N2 B1 N6 110.8(5) . . ? N4 B1 N6 109.2(5) . . ? N2 N1 C11 106.3(6) . . ? N2 N1 Nb1 120.0(4) . . ? C11 N1 Nb1 133.7(5) . . ? N1 N2 C13 109.7(6) . . ? N1 N2 B1 121.1(5) . . ? C13 N2 B1 128.9(6) . . ? C21 N3 N4 106.8(5) . . ? C21 N3 Nb1 130.2(4) . . ? N4 N3 Nb1 123.0(3) . . ? C23 N4 N3 108.7(5) . . ? C23 N4 B1 130.8(6) . . ? N3 N4 B1 120.4(5) . . ? C31 N5 N6 106.4(5) . . ? C31 N5 Nb1 133.8(5) . . ? N6 N5 Nb1 119.6(4) . . ? C33 N6 N5 109.2(5) . . ? C33 N6 B1 129.6(6) . . ? N5 N6 B1 121.1(5) . . ? C40 N7 Nb1 160.2(5) . . ? N1 C11 C12 109.7(7) . . ? N1 C11 C10 123.4(7) . . ? C12 C11 C10 126.9(7) . . ? C11 C12 C13 107.2(6) . . ? N2 C13 C12 107.1(7) . . ? N2 C13 C14 122.3(7) . . ? C12 C13 C14 130.6(7) . . ? N3 C21 C22 109.1(6) . . ? N3 C21 C20 123.0(5) . . ? C22 C21 C20 127.9(6) . . ? C23 C22 C21 106.6(5) . . ? C22 C23 N4 108.7(6) . . ? C22 C23 C24 129.2(6) . . ? N4 C23 C24 122.1(6) . . ? N5 C31 C32 110.1(6) . . ? N5 C31 C30 122.4(7) . . ? C32 C31 C30 127.4(7) . . ? C33 C32 C31 107.4(6) . . ? N6 C33 C32 106.9(7) . . ? N6 C33 C34 122.3(7) . . ? C32 C33 C34 130.8(7) . . ? N7 C40 C41 109.2(6) . . ? N7 C40 C43 110.3(5) . . ? C41 C40 C43 110.7(6) . . ? N7 C40 C42 107.5(6) . . ? C41 C40 C42 110.1(7) . . ? C43 C40 C42 109.0(7) . . ? C51 C50 Nb1 118.6(4) . . ? C55 C51 C52 117.3(8) . . ? C55 C51 C50 120.6(8) . . ? C52 C51 C50 122.1(7) . . ? C51 C52 C59 121.3(9) . . ? C54 C53 C59 120.7(9) . . ? C53 C54 C55 120.5(10) . . ? C54 C55 C51 121.8(9) . . ? C53 C59 C52 118.4(10) . . ? # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.500 0.500 0.500 225 29 ' ' _platon_squeeze_details ? _database_code_depnum_ccdc_archive 'CCDC 902490' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2b _audit_creation_date 2013-11-06T17:15:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C26 H38 B1 Cl1 N7 Ta1' _chemical_formula_sum 'C26 H38 B Cl N7 Ta' _chemical_formula_weight 675.84 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7131(10) _cell_length_b 11.1795(10) _cell_length_c 14.3633(7) _cell_angle_alpha 96.882(5) _cell_angle_beta 97.911(5) _cell_angle_gamma 107.181(7) _cell_volume 1604.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 243 _cell_measurement_theta_min 3.47 _cell_measurement_theta_max 12.25 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 6 -7 -12 0.071 -7 6 9 0.066 -9 1 0 0.101 3 -1 -1 0.097 -1 4 7 0.152 1 1 2 0.225 5 1 -7 0.061 -5 -1 6 0.113 0 1 2 0.119 -12 -13 -7 0.122 -3 -2 5 0.071 -3 1 -5 0.095 1 -2 7 0.188 9 -10 1 0.087 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.534 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.213 _exptl_absorpt_correction_T_max 0.276 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1321 _diffrn_reflns_av_unetI/netI 0.0654 _diffrn_reflns_number 37885 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 _reflns_number_total 7230 _reflns_number_gt 6332 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+8.3294P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7230 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1236 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.824 _refine_diff_density_min -2.496 _refine_diff_density_rms 0.171 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta 0.75991(3) 0.47226(2) 0.204631(19) 0.02947(10) Uani 1 1 d . . . Cl1 Cl 0.87080(19) 0.32074(17) 0.19354(15) 0.0450(4) Uani 1 1 d . . . B1 B 0.9176(8) 0.7682(7) 0.1621(6) 0.0382(18) Uani 1 1 d . . . N1 N 0.9803(6) 0.6204(5) 0.2660(5) 0.0393(13) Uani 1 1 d . . . N2 N 1.0158(6) 0.7354(5) 0.2356(5) 0.0388(13) Uani 1 1 d . . . N3 N 0.8231(5) 0.5445(5) 0.0718(4) 0.0291(11) Uani 1 1 d . . . N4 N 0.8829(5) 0.6704(5) 0.0711(4) 0.0334(12) Uani 1 1 d . . . N5 N 0.7035(6) 0.6511(5) 0.2158(4) 0.0350(13) Uani 1 1 d . . . N6 N 0.7900(6) 0.7643(5) 0.2012(4) 0.0341(12) Uani 1 1 d . . . N7 N 0.5983(6) 0.3653(5) 0.1575(4) 0.0335(12) Uani 1 1 d . . . C10 C 1.0981(9) 0.5100(9) 0.3747(7) 0.065(3) Uani 1 1 d . . . H10A H 1.0142 0.4434 0.3598 0.097 Uiso 1 1 calc R . . H10B H 1.1209 0.539 0.4423 0.097 Uiso 1 1 calc R . . H10C H 1.1655 0.4783 0.3538 0.097 Uiso 1 1 calc R . . C11 C 1.0884(7) 0.6177(8) 0.3253(6) 0.0453(18) Uani 1 1 d . . . C12 C 1.1921(8) 0.7299(8) 0.3307(6) 0.052(2) Uani 1 1 d . . . H12 H 1.2778 0.7516 0.3656 0.062 Uiso 1 1 calc R . . C13 C 1.1424(8) 0.8017(7) 0.2740(6) 0.0475(19) Uani 1 1 d . . . C14 C 1.2143(9) 0.9300(8) 0.2507(8) 0.069(3) Uani 1 1 d . . . H14A H 1.1536 0.9569 0.2091 0.103 Uiso 1 1 calc R . . H14B H 1.2865 0.9235 0.2197 0.103 Uiso 1 1 calc R . . H14C H 1.2484 0.991 0.3085 0.103 Uiso 1 1 calc R . . C20 C 0.7581(8) 0.3432(7) -0.0455(6) 0.0425(17) Uani 1 1 d . . . H20A H 0.7281 0.3055 0.0073 0.064 Uiso 1 1 calc R . . H20B H 0.8258 0.3109 -0.0651 0.064 Uiso 1 1 calc R . . H20C H 0.6847 0.3227 -0.0977 0.064 Uiso 1 1 calc R . . C21 C 0.8125(6) 0.4815(6) -0.0168(5) 0.0314(14) Uani 1 1 d . . . C22 C 0.8662(7) 0.5699(7) -0.0731(5) 0.0383(15) Uani 1 1 d . . . H22 H 0.8725 0.5527 -0.1369 0.046 Uiso 1 1 calc R . . C23 C 0.9080(7) 0.6873(6) -0.0161(5) 0.0358(15) Uani 1 1 d . . . C24 C 0.9689(8) 0.8158(7) -0.0410(6) 0.0462(19) Uani 1 1 d . . . H24A H 0.9876 0.8796 0.0146 0.069 Uiso 1 1 calc R . . H24B H 0.908 0.8313 -0.0901 0.069 Uiso 1 1 calc R . . H24C H 1.0499 0.8186 -0.0634 0.069 Uiso 1 1 calc R . . C30 C 0.4810(8) 0.5805(7) 0.2599(7) 0.0483(19) Uani 1 1 d . . . H30A H 0.4954 0.4994 0.2528 0.072 Uiso 1 1 calc R . . H30B H 0.4035 0.5762 0.2156 0.072 Uiso 1 1 calc R . . H30C H 0.4684 0.6028 0.3238 0.072 Uiso 1 1 calc R . . C31 C 0.5974(7) 0.6775(7) 0.2409(6) 0.0398(16) Uani 1 1 d . . . C32 C 0.6142(8) 0.8050(7) 0.2435(6) 0.0469(19) Uani 1 1 d . . . H32 H 0.5551 0.847 0.2596 0.056 Uiso 1 1 calc R . . C33 C 0.7349(7) 0.8584(6) 0.2177(6) 0.0388(16) Uani 1 1 d . . . C34 C 0.8021(10) 0.9926(7) 0.2060(7) 0.061(2) Uani 1 1 d . . . H34A H 0.8862 0.9988 0.1874 0.092 Uiso 1 1 calc R . . H34B H 0.816 1.0485 0.2654 0.092 Uiso 1 1 calc R . . H34C H 0.7471 1.0164 0.1578 0.092 Uiso 1 1 calc R . . C40 C 0.4772(7) 0.2606(6) 0.1169(6) 0.0385(16) Uani 1 1 d . . . C41 C 0.4110(8) 0.2922(10) 0.0261(6) 0.060(2) Uani 1 1 d . . . H41A H 0.3884 0.3683 0.0415 0.089 Uiso 1 1 calc R . . H41B H 0.3318 0.2233 -0.002 0.089 Uiso 1 1 calc R . . H41C H 0.4712 0.3049 -0.0182 0.089 Uiso 1 1 calc R . . C42 C 0.5153(9) 0.1398(7) 0.0973(9) 0.072(3) Uani 1 1 d . . . H42A H 0.5564 0.1233 0.156 0.108 Uiso 1 1 calc R . . H42B H 0.5764 0.1508 0.0536 0.108 Uiso 1 1 calc R . . H42C H 0.4369 0.0696 0.0699 0.108 Uiso 1 1 calc R . . C43 C 0.3810(8) 0.2420(8) 0.1883(6) 0.0494(19) Uani 1 1 d . . . H43A H 0.3561 0.3173 0.201 0.074 Uiso 1 1 calc R . . H43B H 0.424 0.2263 0.2466 0.074 Uiso 1 1 calc R . . H43C H 0.3031 0.171 0.1617 0.074 Uiso 1 1 calc R . . C50 C 0.7498(7) 0.4806(7) 0.3612(5) 0.0369(15) Uani 1 1 d . . . H50A H 0.8398 0.5008 0.3958 0.044 Uiso 1 1 calc R . . H50B H 0.7188 0.5514 0.3805 0.044 Uiso 1 1 calc R . . C51 C 0.6661(8) 0.3675(7) 0.3942(5) 0.0416(16) Uani 1 1 d . . . C52 C 0.6901(9) 0.2522(7) 0.3846(6) 0.052(2) Uani 1 1 d . . . H52 H 0.7618 0.2441 0.3576 0.062 Uiso 1 1 calc R . . C53 C 0.6079(11) 0.1477(8) 0.4150(7) 0.068(3) Uani 1 1 d . . . H53 H 0.6249 0.0705 0.4072 0.081 Uiso 1 1 calc R . . C54 C 0.5031(10) 0.1576(10) 0.4559(8) 0.071(3) Uani 1 1 d . . . H54 H 0.449 0.0882 0.4768 0.086 Uiso 1 1 calc R . . C55 C 0.4790(10) 0.2712(11) 0.4656(8) 0.069(3) Uani 1 1 d . . . H55 H 0.4075 0.2786 0.4933 0.083 Uiso 1 1 calc R . . C56 C 0.5577(9) 0.3749(9) 0.4356(7) 0.058(2) Uani 1 1 d . . . H56 H 0.5385 0.4509 0.4429 0.069 Uiso 1 1 calc R . . H1 H 0.963(6) 0.858(6) 0.149(4) 0.020(15) Uiso 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 Ta1 0.02819(15) 0.02887(14) 0.03088(17) 0.00745(10) 0.00658(11) 0.00687(10) Cl1 0.0471(10) 0.0429(9) 0.0527(12) 0.0154(8) 0.0185(9) 0.0186(8) B1 0.039(4) 0.027(4) 0.045(5) 0.003(3) 0.013(4) 0.004(3) N1 0.033(3) 0.042(3) 0.043(4) 0.011(3) 0.009(3) 0.010(3) N2 0.034(3) 0.036(3) 0.040(4) 0.003(2) 0.007(3) 0.003(2) N3 0.030(3) 0.029(3) 0.027(3) 0.007(2) 0.006(2) 0.006(2) N4 0.029(3) 0.025(2) 0.045(4) 0.007(2) 0.008(3) 0.005(2) N5 0.038(3) 0.024(3) 0.041(4) 0.002(2) 0.008(3) 0.008(2) N6 0.038(3) 0.026(3) 0.039(3) 0.003(2) 0.010(3) 0.009(2) N7 0.040(3) 0.024(2) 0.037(3) 0.002(2) 0.016(3) 0.008(2) C10 0.044(5) 0.082(6) 0.069(7) 0.035(5) 0.000(4) 0.017(4) C11 0.032(4) 0.064(5) 0.034(4) 0.004(3) -0.002(3) 0.012(3) C12 0.033(4) 0.064(5) 0.045(5) -0.005(4) -0.002(3) 0.004(4) C13 0.036(4) 0.044(4) 0.051(5) -0.008(3) 0.008(4) 0.002(3) C14 0.040(5) 0.048(5) 0.093(8) -0.005(5) 0.011(5) -0.015(4) C20 0.041(4) 0.043(4) 0.047(5) 0.005(3) 0.015(3) 0.016(3) C21 0.028(3) 0.036(3) 0.032(4) 0.006(3) 0.008(3) 0.013(3) C22 0.035(4) 0.050(4) 0.030(4) 0.010(3) 0.011(3) 0.011(3) C23 0.031(3) 0.040(4) 0.042(4) 0.017(3) 0.016(3) 0.012(3) C24 0.048(5) 0.043(4) 0.053(5) 0.020(4) 0.021(4) 0.013(3) C30 0.040(4) 0.047(4) 0.066(6) 0.009(4) 0.020(4) 0.021(3) C31 0.035(4) 0.039(4) 0.047(5) 0.003(3) 0.007(3) 0.015(3) C32 0.050(5) 0.037(4) 0.058(5) 0.001(3) 0.016(4) 0.021(3) C33 0.043(4) 0.028(3) 0.046(5) 0.002(3) 0.007(3) 0.014(3) C34 0.084(7) 0.027(4) 0.076(7) 0.009(4) 0.024(5) 0.021(4) C40 0.030(3) 0.035(3) 0.050(5) 0.006(3) 0.008(3) 0.010(3) C41 0.038(4) 0.094(7) 0.039(5) 0.012(4) 0.004(4) 0.010(4) C42 0.056(6) 0.030(4) 0.121(10) -0.007(5) 0.027(6) 0.004(4) C43 0.039(4) 0.049(4) 0.054(5) 0.011(4) 0.013(4) 0.002(3) C50 0.042(4) 0.047(4) 0.023(4) 0.005(3) 0.008(3) 0.015(3) C51 0.042(4) 0.054(4) 0.027(4) 0.009(3) 0.004(3) 0.014(3) C52 0.068(6) 0.049(4) 0.043(5) 0.012(4) 0.020(4) 0.020(4) C53 0.091(8) 0.046(5) 0.060(6) 0.017(4) 0.019(6) 0.008(5) C54 0.061(6) 0.078(7) 0.056(6) 0.022(5) 0.009(5) -0.009(5) C55 0.056(6) 0.095(8) 0.064(7) 0.033(6) 0.032(5) 0.018(5) C56 0.050(5) 0.079(6) 0.054(6) 0.023(5) 0.021(4) 0.028(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N7 1.773(6) . ? Ta1 N5 2.248(5) . ? Ta1 C50 2.258(7) . ? Ta1 N3 2.269(5) . ? Ta1 Cl1 2.3415(17) . ? Ta1 N1 2.421(6) . ? B1 N4 1.525(10) . ? B1 N6 1.538(10) . ? B1 N2 1.539(11) . ? N1 C11 1.350(9) . ? N1 N2 1.372(8) . ? N2 C13 1.340(10) . ? N3 C21 1.352(8) . ? N3 N4 1.365(7) . ? N4 C23 1.341(9) . ? N5 C31 1.339(9) . ? N5 N6 1.388(7) . ? N6 C33 1.363(8) . ? N7 C40 1.458(9) . ? C10 C11 1.491(11) . ? C11 C12 1.394(11) . ? C12 C13 1.371(12) . ? C13 C14 1.516(11) . ? C20 C21 1.466(9) . ? C21 C22 1.394(9) . ? C22 C23 1.374(10) . ? C23 C24 1.500(9) . ? C30 C31 1.473(10) . ? C31 C32 1.378(10) . ? C32 C33 1.376(11) . ? C33 C34 1.501(10) . ? C40 C41 1.527(11) . ? C40 C42 1.528(10) . ? C40 C43 1.539(10) . ? C50 C51 1.489(10) . ? C51 C52 1.382(11) . ? C51 C56 1.394(11) . ? C52 C53 1.397(12) . ? C53 C54 1.363(15) . ? C54 C55 1.364(15) . ? C55 C56 1.372(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Ta1 N5 96.9(2) . . ? N7 Ta1 C50 98.3(3) . . ? N5 Ta1 C50 86.1(2) . . ? N7 Ta1 N3 101.4(2) . . ? N5 Ta1 N3 79.7(2) . . ? C50 Ta1 N3 156.9(2) . . ? N7 Ta1 Cl1 96.30(17) . . ? N5 Ta1 Cl1 165.85(15) . . ? C50 Ta1 Cl1 96.99(19) . . ? N3 Ta1 Cl1 92.69(14) . . ? N7 Ta1 N1 178.8(2) . . ? N5 Ta1 N1 82.6(2) . . ? C50 Ta1 N1 82.7(2) . . ? N3 Ta1 N1 77.5(2) . . ? Cl1 Ta1 N1 84.14(15) . . ? N4 B1 N6 109.3(6) . . ? N4 B1 N2 108.5(6) . . ? N6 B1 N2 110.2(6) . . ? C11 N1 N2 106.1(6) . . ? C11 N1 Ta1 134.9(5) . . ? N2 N1 Ta1 118.9(4) . . ? C13 N2 N1 110.2(6) . . ? C13 N2 B1 129.4(6) . . ? N1 N2 B1 120.3(6) . . ? C21 N3 N4 107.2(5) . . ? C21 N3 Ta1 130.7(4) . . ? N4 N3 Ta1 122.1(4) . . ? C23 N4 N3 110.0(5) . . ? C23 N4 B1 129.1(6) . . ? N3 N4 B1 120.9(5) . . ? C31 N5 N6 106.8(5) . . ? C31 N5 Ta1 132.2(5) . . ? N6 N5 Ta1 120.9(4) . . ? C33 N6 N5 108.8(5) . . ? C33 N6 B1 129.4(6) . . ? N5 N6 B1 121.5(5) . . ? C40 N7 Ta1 170.0(4) . . ? N1 C11 C12 109.4(7) . . ? N1 C11 C10 125.7(7) . . ? C12 C11 C10 124.9(8) . . ? C13 C12 C11 106.1(7) . . ? N2 C13 C12 108.1(7) . . ? N2 C13 C14 123.4(8) . . ? C12 C13 C14 128.4(8) . . ? N3 C21 C22 108.3(6) . . ? N3 C21 C20 124.7(6) . . ? C22 C21 C20 127.0(7) . . ? C23 C22 C21 106.8(6) . . ? N4 C23 C22 107.7(6) . . ? N4 C23 C24 122.9(7) . . ? C22 C23 C24 129.3(7) . . ? N5 C31 C32 109.9(6) . . ? N5 C31 C30 123.2(6) . . ? C32 C31 C30 126.9(7) . . ? C31 C32 C33 107.1(6) . . ? N6 C33 C32 107.5(6) . . ? N6 C33 C34 122.3(7) . . ? C32 C33 C34 130.2(7) . . ? N7 C40 C41 108.6(6) . . ? N7 C40 C42 107.9(6) . . ? C41 C40 C42 112.1(8) . . ? N7 C40 C43 110.2(6) . . ? C41 C40 C43 109.3(6) . . ? C42 C40 C43 108.7(6) . . ? C51 C50 Ta1 119.4(5) . . ? C52 C51 C56 117.3(7) . . ? C52 C51 C50 122.5(7) . . ? C56 C51 C50 120.1(7) . . ? C51 C52 C53 120.9(8) . . ? C54 C53 C52 120.7(9) . . ? C53 C54 C55 118.7(9) . . ? C54 C55 C56 121.6(9) . . ? C55 C56 C51 120.8(9) . . ? # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.500 235 31 ' ' _platon_squeeze_details ? _database_code_depnum_ccdc_archive 'CCDC 902491' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3a _audit_creation_date 2013-11-14T18:45:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H42 B1 Cl1 N7 Nb1' _chemical_formula_sum 'C24 H42 B Cl N7 Nb' _chemical_formula_weight 567.82 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6587(12) _cell_length_b 14.113(6) _cell_length_c 20.728(4) _cell_angle_alpha 90 _cell_angle_beta 114.993(14) _cell_angle_gamma 90 _cell_volume 2826.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 234 _cell_measurement_theta_min 3.45 _cell_measurement_theta_max 15.32 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.26 _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 -2 -12 0.158 -3 2 -1 0.161 1 3 14 0.138 5 -3 1 0.161 15 -16 2 0.145 -17 7 -1 0.084 -8 -11 1 0.156 10 11 -1 0.152 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.545 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.752 _exptl_absorpt_correction_T_max 1.223 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.2398 _diffrn_reflns_av_unetI/netI 0.2784 _diffrn_reflns_number 15126 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 26.05 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.959 _diffrn_measured_fraction_theta_max 0.959 _reflns_number_total 5349 _reflns_number_gt 1859 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5349 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1959 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.1954 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 0.831 _refine_ls_restrained_S_all 0.831 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.99 _refine_diff_density_min -1.019 _refine_diff_density_rms 0.142 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.65219(8) 0.33339(7) 0.21282(4) 0.0501(3) Uani 1 1 d . . . B1 B 0.3337(11) 0.3325(9) 0.0693(5) 0.047(3) Uani 1 1 d . . . Cl1 Cl 0.8557(2) 0.35374(19) 0.19373(11) 0.0617(7) Uani 1 1 d . . . N1 N 0.5572(7) 0.2458(6) 0.0996(3) 0.055(2) Uani 1 1 d . . . N2 N 0.4202(7) 0.2550(6) 0.0564(3) 0.048(2) Uani 1 1 d . . . N3 N 0.5354(7) 0.4464(5) 0.1282(3) 0.0423(18) Uani 1 1 d . . . N4 N 0.4023(7) 0.4297(6) 0.0756(3) 0.051(2) Uani 1 1 d . . . N5 N 0.4341(7) 0.3165(6) 0.2030(3) 0.049(2) Uani 1 1 d . . . N6 N 0.3191(7) 0.3128(5) 0.1387(3) 0.0451(19) Uani 1 1 d . . . N7 N 0.7090(7) 0.4046(7) 0.2911(3) 0.076(3) Uani 1 1 d . . . C10 C 0.7519(9) 0.1415(8) 0.1015(5) 0.082(4) Uani 1 1 d . . . H10A H 0.8054 0.1778 0.1434 0.122 Uiso 1 1 calc R . . H10B H 0.7885 0.1505 0.0668 0.122 Uiso 1 1 calc R . . H10C H 0.7565 0.0756 0.1137 0.122 Uiso 1 1 calc R . . C11 C 0.6033(9) 0.1741(8) 0.0710(4) 0.056(3) Uani 1 1 d . . . C12 C 0.4946(10) 0.1410(7) 0.0098(4) 0.057(3) Uani 1 1 d . . . H12 H 0.4988 0.093 -0.02 0.069 Uiso 1 1 calc R . . C13 C 0.3815(10) 0.1919(7) 0.0017(4) 0.053(3) Uani 1 1 d . . . C14 C 0.2360(9) 0.1835(7) -0.0532(4) 0.068(3) Uani 1 1 d . . . H14A H 0.1797 0.2305 -0.0446 0.103 Uiso 1 1 calc R . . H14B H 0.2011 0.1215 -0.0507 0.103 Uiso 1 1 calc R . . H14C H 0.2334 0.193 -0.0996 0.103 Uiso 1 1 calc R . . C20 C 0.7023(9) 0.5816(8) 0.1629(5) 0.069(3) Uani 1 1 d . . . H20A H 0.7581 0.5381 0.1994 0.103 Uiso 1 1 calc R . . H20B H 0.6859 0.6376 0.1845 0.103 Uiso 1 1 calc R . . H20C H 0.7497 0.5984 0.1342 0.103 Uiso 1 1 calc R . . C21 C 0.5656(9) 0.5354(8) 0.1168(5) 0.056(3) Uani 1 1 d . . . C22 C 0.4578(10) 0.5741(8) 0.0586(4) 0.055(3) Uani 1 1 d . . . H22 H 0.455 0.6342 0.0396 0.066 Uiso 1 1 calc R . . C23 C 0.3560(10) 0.5069(8) 0.0343(4) 0.055(3) Uani 1 1 d . . . C24 C 0.2144(9) 0.5139(8) -0.0255(4) 0.069(3) Uani 1 1 d . . . H24A H 0.1659 0.4553 -0.0295 0.103 Uiso 1 1 calc R . . H24B H 0.2223 0.5262 -0.0692 0.103 Uiso 1 1 calc R . . H24C H 0.1643 0.5645 -0.0161 0.103 Uiso 1 1 calc R . . C30 C 0.4696(9) 0.3058(8) 0.3301(4) 0.076(4) Uani 1 1 d . . . H30A H 0.5646 0.3151 0.3386 0.114 Uiso 1 1 calc R . . H30B H 0.4607 0.2473 0.3514 0.114 Uiso 1 1 calc R . . H30C H 0.4401 0.3574 0.3506 0.114 Uiso 1 1 calc R . . C31 C 0.3825(9) 0.3024(7) 0.2525(4) 0.046(2) Uani 1 1 d . . . C32 C 0.2410(9) 0.2907(7) 0.2202(4) 0.053(3) Uani 1 1 d . . . H32 H 0.1825 0.2808 0.2425 0.064 Uiso 1 1 calc R . . C33 C 0.2045(8) 0.2966(7) 0.1493(4) 0.049(2) Uani 1 1 d . . . C34 C 0.0620(8) 0.2895(8) 0.0880(4) 0.065(3) Uani 1 1 d . . . H34A H 0.0694 0.2986 0.0439 0.097 Uiso 1 1 calc R . . H34B H 0.0029 0.3374 0.0931 0.097 Uiso 1 1 calc R . . H34C H 0.0236 0.2281 0.0883 0.097 Uiso 1 1 calc R . . C40 C 0.7740(9) 0.4701(7) 0.3515(4) 0.055(3) Uani 1 1 d . . . C41 C 0.8080(11) 0.4257(10) 0.4224(4) 0.107(5) Uani 1 1 d . . . H41A H 0.7254 0.3996 0.4232 0.161 Uiso 1 1 calc R . . H41B H 0.8457 0.4728 0.459 0.161 Uiso 1 1 calc R . . H41C H 0.8746 0.3761 0.4306 0.161 Uiso 1 1 calc R . . C42 C 0.6652(12) 0.5497(9) 0.3424(6) 0.112(5) Uani 1 1 d . . . H42A H 0.6422 0.5821 0.2981 0.168 Uiso 1 1 calc R . . H42B H 0.7036 0.594 0.381 0.168 Uiso 1 1 calc R . . H42C H 0.5832 0.5217 0.3425 0.168 Uiso 1 1 calc R . . C43 C 0.9053(9) 0.5139(9) 0.3494(5) 0.089(4) Uani 1 1 d . . . H43A H 0.8812 0.5446 0.3044 0.134 Uiso 1 1 calc R . . H43B H 0.9718 0.4649 0.3555 0.134 Uiso 1 1 calc R . . H43C H 0.9445 0.5596 0.387 0.134 Uiso 1 1 calc R . . C50 C 0.6856(10) 0.1896(8) 0.2573(4) 0.071(3) Uani 1 1 d . . . H50A H 0.6126 0.1812 0.2731 0.086 Uiso 1 1 calc R . . H50B H 0.6608 0.1488 0.2161 0.086 Uiso 1 1 calc R . . C51 C 0.8067(10) 0.1423(7) 0.3130(5) 0.058(3) Uani 1 1 d . . . C52 C 0.9327(11) 0.1403(11) 0.2996(6) 0.138(7) Uani 1 1 d . . . H52A H 1.006 0.1089 0.3383 0.207 Uiso 1 1 calc R . . H52B H 0.9603 0.204 0.2956 0.207 Uiso 1 1 calc R . . H52C H 0.9134 0.1067 0.2561 0.207 Uiso 1 1 calc R . . C53 C 0.8449(13) 0.1844(11) 0.3867(5) 0.142(7) Uani 1 1 d . . . H53A H 0.9243 0.152 0.4209 0.213 Uiso 1 1 calc R . . H53B H 0.7685 0.1772 0.3993 0.213 Uiso 1 1 calc R . . H53C H 0.8659 0.2504 0.3862 0.213 Uiso 1 1 calc R . . C54 C 0.7740(13) 0.0381(10) 0.3196(7) 0.147(6) Uani 1 1 d . . . H54A H 0.8534 0.0082 0.3558 0.221 Uiso 1 1 calc R . . H54B H 0.7511 0.0066 0.2749 0.221 Uiso 1 1 calc R . . H54C H 0.6971 0.034 0.3321 0.221 Uiso 1 1 calc R . . H1 H 0.231(7) 0.329(6) 0.030(3) 0.05(2) Uiso 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 Nb1 0.0508(5) 0.0540(7) 0.0470(4) 0.0061(5) 0.0221(4) 0.0003(5) B1 0.047(6) 0.054(9) 0.043(5) 0.000(6) 0.021(5) -0.002(6) Cl1 0.0580(14) 0.066(2) 0.0723(14) 0.0065(14) 0.0382(12) 0.0031(13) N1 0.054(5) 0.058(7) 0.050(4) -0.005(4) 0.019(4) 0.006(4) N2 0.054(5) 0.051(6) 0.041(4) 0.002(4) 0.023(4) 0.007(4) N3 0.043(4) 0.034(5) 0.049(4) 0.000(4) 0.018(3) 0.003(4) N4 0.053(5) 0.061(7) 0.041(4) 0.008(4) 0.022(4) 0.005(4) N5 0.049(4) 0.060(6) 0.038(4) 0.006(4) 0.018(3) -0.003(4) N6 0.045(4) 0.042(6) 0.050(4) 0.002(4) 0.021(3) 0.004(4) N7 0.066(5) 0.126(10) 0.030(4) -0.016(5) 0.014(4) -0.019(6) C10 0.072(7) 0.085(11) 0.080(7) -0.010(7) 0.024(6) 0.022(7) C11 0.061(6) 0.058(8) 0.055(5) 0.001(5) 0.030(5) 0.013(6) C12 0.080(7) 0.051(8) 0.050(5) -0.009(5) 0.035(5) -0.004(6) C13 0.061(6) 0.054(8) 0.052(5) -0.005(5) 0.030(5) -0.005(5) C14 0.069(6) 0.066(9) 0.067(6) -0.013(6) 0.025(5) -0.009(6) C20 0.069(7) 0.056(9) 0.086(7) -0.001(6) 0.039(6) -0.001(6) C21 0.061(6) 0.057(8) 0.057(6) 0.000(6) 0.032(5) -0.004(6) C22 0.071(7) 0.045(8) 0.054(5) 0.008(5) 0.032(5) 0.007(6) C23 0.075(7) 0.057(8) 0.050(5) 0.009(5) 0.042(5) 0.016(6) C24 0.070(6) 0.078(9) 0.044(5) 0.010(5) 0.010(5) 0.018(6) C30 0.091(8) 0.086(11) 0.060(6) 0.008(6) 0.042(6) -0.021(7) C31 0.057(6) 0.044(7) 0.042(4) 0.001(4) 0.025(4) -0.006(5) C32 0.055(6) 0.061(8) 0.050(5) 0.000(5) 0.028(4) -0.005(5) C33 0.045(5) 0.035(7) 0.071(6) -0.003(5) 0.030(5) 0.007(5) C34 0.042(5) 0.077(9) 0.075(6) 0.016(6) 0.024(5) 0.000(5) C40 0.058(6) 0.047(8) 0.058(5) -0.005(5) 0.023(5) -0.006(5) C41 0.111(9) 0.138(15) 0.052(6) 0.006(7) 0.016(6) -0.039(9) C42 0.145(12) 0.075(12) 0.142(11) -0.001(9) 0.085(10) 0.005(9) C43 0.074(7) 0.098(12) 0.092(8) -0.020(7) 0.031(6) -0.022(7) C50 0.084(7) 0.081(10) 0.059(6) 0.023(6) 0.041(5) 0.039(7) C51 0.059(6) 0.044(8) 0.076(6) 0.011(6) 0.032(5) 0.005(5) C52 0.074(8) 0.23(2) 0.110(9) 0.076(11) 0.039(7) 0.048(10) C53 0.159(13) 0.170(18) 0.063(7) 0.009(9) 0.015(8) 0.064(12) C54 0.160(14) 0.057(12) 0.183(14) 0.039(11) 0.031(11) 0.010(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 N7 1.783(7) . ? Nb1 C50 2.196(10) . ? Nb1 N5 2.259(6) . ? Nb1 N3 2.308(7) . ? Nb1 Cl1 2.381(2) . ? Nb1 N1 2.461(7) . ? B1 N2 1.525(13) . ? B1 N4 1.534(13) . ? B1 N6 1.535(10) . ? N1 N2 1.359(8) . ? N1 C11 1.363(11) . ? N2 C13 1.361(10) . ? N3 C21 1.341(11) . ? N3 N4 1.396(8) . ? N4 C23 1.344(11) . ? N5 C31 1.368(9) . ? N5 N6 1.379(8) . ? N6 C33 1.349(9) . ? N7 C40 1.472(11) . ? C10 C11 1.509(11) . ? C11 C12 1.389(11) . ? C12 C13 1.351(12) . ? C13 C14 1.491(11) . ? C20 C21 1.512(11) . ? C21 C22 1.380(11) . ? C22 C23 1.367(12) . ? C23 C24 1.498(11) . ? C30 C31 1.479(10) . ? C31 C32 1.377(10) . ? C32 C33 1.354(10) . ? C33 C34 1.516(10) . ? C40 C41 1.495(12) . ? C40 C43 1.548(12) . ? C40 C42 1.567(14) . ? C50 C51 1.478(11) . ? C51 C52 1.482(13) . ? C51 C53 1.525(13) . ? C51 C54 1.531(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Nb1 C50 101.9(4) . . ? N7 Nb1 N5 94.7(3) . . ? C50 Nb1 N5 85.3(3) . . ? N7 Nb1 N3 99.7(3) . . ? C50 Nb1 N3 153.9(3) . . ? N5 Nb1 N3 78.5(2) . . ? N7 Nb1 Cl1 95.8(2) . . ? C50 Nb1 Cl1 100.6(2) . . ? N5 Nb1 Cl1 166.63(15) . . ? N3 Nb1 Cl1 91.54(17) . . ? N7 Nb1 N1 174.8(3) . . ? C50 Nb1 N1 82.2(3) . . ? N5 Nb1 N1 82.4(2) . . ? N3 Nb1 N1 75.5(3) . . ? Cl1 Nb1 N1 86.47(18) . . ? N2 B1 N4 110.7(7) . . ? N2 B1 N6 110.1(8) . . ? N4 B1 N6 108.4(7) . . ? N2 N1 C11 105.6(7) . . ? N2 N1 Nb1 118.3(5) . . ? C11 N1 Nb1 135.1(6) . . ? N1 N2 C13 110.4(7) . . ? N1 N2 B1 120.9(7) . . ? C13 N2 B1 128.5(8) . . ? C21 N3 N4 105.1(7) . . ? C21 N3 Nb1 133.5(6) . . ? N4 N3 Nb1 121.4(6) . . ? C23 N4 N3 109.8(8) . . ? C23 N4 B1 129.6(8) . . ? N3 N4 B1 120.5(7) . . ? C31 N5 N6 104.2(6) . . ? C31 N5 Nb1 132.3(5) . . ? N6 N5 Nb1 123.5(4) . . ? C33 N6 N5 110.1(6) . . ? C33 N6 B1 129.9(7) . . ? N5 N6 B1 119.9(7) . . ? C40 N7 Nb1 169.8(6) . . ? N1 C11 C12 109.4(8) . . ? N1 C11 C10 123.4(8) . . ? C12 C11 C10 127.1(9) . . ? C13 C12 C11 106.8(8) . . ? C12 C13 N2 107.7(8) . . ? C12 C13 C14 129.6(9) . . ? N2 C13 C14 122.6(9) . . ? N3 C21 C22 110.6(9) . . ? N3 C21 C20 122.1(9) . . ? C22 C21 C20 127.3(10) . . ? C23 C22 C21 106.6(9) . . ? N4 C23 C22 107.9(9) . . ? N4 C23 C24 123.4(10) . . ? C22 C23 C24 128.7(10) . . ? N5 C31 C32 110.9(7) . . ? N5 C31 C30 122.9(7) . . ? C32 C31 C30 126.1(7) . . ? C33 C32 C31 105.9(8) . . ? N6 C33 C32 108.9(7) . . ? N6 C33 C34 122.0(7) . . ? C32 C33 C34 129.2(8) . . ? N7 C40 C41 113.8(9) . . ? N7 C40 C43 109.5(7) . . ? C41 C40 C43 110.4(8) . . ? N7 C40 C42 106.8(8) . . ? C41 C40 C42 106.2(8) . . ? C43 C40 C42 110.0(9) . . ? C51 C50 Nb1 132.7(8) . . ? C50 C51 C52 115.1(8) . . ? C50 C51 C53 112.4(9) . . ? C52 C51 C53 108.4(9) . . ? C50 C51 C54 110.3(9) . . ? C52 C51 C54 104.9(10) . . ? C53 C51 C54 105.0(10) . . ? _database_code_depnum_ccdc_archive 'CCDC 902492' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3b _audit_creation_date 2013-11-06T17:56:00-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H42 B1 Cl1 N7 Ta1' _chemical_formula_sum 'C24 H42 B Cl N7 Ta' _chemical_formula_weight 655.86 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _space_group_IT_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5914(16) _cell_length_b 14.0905(14) _cell_length_c 18.9936(19) _cell_angle_alpha 90 _cell_angle_beta 95.365(9) _cell_angle_gamma 90 _cell_volume 2822.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 245 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 17.23 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 3 -5 0.112 1 -6 14 0.086 8 -5 -6 0.153 -3 1 4 0.275 -1 3 -5 0.108 -1 -19 0 0.089 0 15 -1 0.104 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.086 _exptl_absorpt_correction_T_max 0.136 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0818 _diffrn_reflns_av_unetI/netI 0.1287 _diffrn_reflns_number 19594 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 6432 _reflns_number_gt 4103 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6432 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1008 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.061 _refine_diff_density_min -2.488 _refine_diff_density_rms 0.166 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta 0.56489(3) 0.16713(2) 0.215337(15) 0.03272(12) Uani 1 1 d . . . Cl1 Cl 0.33914(15) 0.14560(12) 0.19413(10) 0.0342(4) Uani 1 1 d . . . B1 B 0.7376(7) 0.1667(6) 0.0711(4) 0.0325(18) Uani 1 1 d . . . N1 N 0.5462(6) 0.2549(4) 0.1037(3) 0.0388(15) Uani 1 1 d . . . N2 N 0.6371(5) 0.2443(4) 0.0587(3) 0.0341(14) Uani 1 1 d . . . N3 N 0.5948(5) 0.0539(4) 0.1308(3) 0.0316(13) Uani 1 1 d . . . N4 N 0.6717(5) 0.0703(4) 0.0781(3) 0.0317(13) Uani 1 1 d . . . N5 N 0.7717(5) 0.1841(4) 0.2037(3) 0.0376(15) Uani 1 1 d . . . N6 N 0.8205(5) 0.1868(4) 0.1399(3) 0.0313(13) Uani 1 1 d . . . N7 N 0.5847(6) 0.0926(5) 0.2941(3) 0.0530(18) Uani 1 1 d . . . C10 C 0.3550(8) 0.3609(6) 0.1082(5) 0.059(2) Uani 1 1 d . . . H10A H 0.3448 0.3259 0.1507 0.088 Uiso 1 1 calc R . . H10B H 0.281 0.3528 0.0755 0.088 Uiso 1 1 calc R . . H10C H 0.366 0.427 0.1194 0.088 Uiso 1 1 calc R . . C11 C 0.4696(7) 0.3249(5) 0.0754(4) 0.0439(19) Uani 1 1 d . . . C12 C 0.5127(7) 0.3587(5) 0.0152(4) 0.045(2) Uani 1 1 d . . . H12 H 0.4772 0.4072 -0.0134 0.054 Uiso 1 1 calc R . . C13 C 0.6199(8) 0.3067(5) 0.0047(4) 0.0420(19) Uani 1 1 d . . . C14 C 0.7056(8) 0.3141(6) -0.0527(5) 0.055(2) Uani 1 1 d . . . H14A H 0.772 0.2679 -0.0453 0.083 Uiso 1 1 calc R . . H14B H 0.742 0.3766 -0.0524 0.083 Uiso 1 1 calc R . . H14C H 0.6582 0.3028 -0.0975 0.083 Uiso 1 1 calc R . . C20 C 0.4621(7) -0.0812(5) 0.1671(5) 0.049(2) Uani 1 1 d . . . H20A H 0.4424 -0.0379 0.2035 0.073 Uiso 1 1 calc R . . H20B H 0.5026 -0.1365 0.1882 0.073 Uiso 1 1 calc R . . H20C H 0.3854 -0.0994 0.1395 0.073 Uiso 1 1 calc R . . C21 C 0.5488(6) -0.0343(5) 0.1207(4) 0.0379(18) Uani 1 1 d . . . C22 C 0.5981(7) -0.0734(5) 0.0618(4) 0.045(2) Uani 1 1 d . . . H22 H 0.5818 -0.1338 0.0433 0.053 Uiso 1 1 calc R . . C23 C 0.6743(7) -0.0068(5) 0.0364(4) 0.0369(17) Uani 1 1 d . . . C24 C 0.7533(8) -0.0132(5) -0.0250(4) 0.051(2) Uani 1 1 d . . . H24A H 0.7959 0.0461 -0.0305 0.077 Uiso 1 1 calc R . . H24B H 0.6995 -0.027 -0.0673 0.077 Uiso 1 1 calc R . . H24C H 0.8149 -0.0629 -0.0166 0.077 Uiso 1 1 calc R . . C30 C 0.8601(7) 0.1942(6) 0.3308(4) 0.055(2) Uani 1 1 d . . . H30A H 0.7727 0.1855 0.3389 0.082 Uiso 1 1 calc R . . H30B H 0.8904 0.2529 0.3518 0.082 Uiso 1 1 calc R . . H30C H 0.9095 0.1426 0.3518 0.082 Uiso 1 1 calc R . . C31 C 0.8723(7) 0.1967(5) 0.2532(4) 0.0366(17) Uani 1 1 d . . . C32 C 0.9803(7) 0.2079(5) 0.2206(4) 0.0367(18) Uani 1 1 d . . . H32 H 1.0615 0.2179 0.2425 0.044 Uiso 1 1 calc R . . C33 C 0.9462(6) 0.2014(5) 0.1485(4) 0.0326(17) Uani 1 1 d . . . C34 C 1.0253(7) 0.2084(6) 0.0891(4) 0.051(2) Uani 1 1 d . . . H34A H 0.9729 0.2012 0.0453 0.077 Uiso 1 1 calc R . . H34B H 1.0883 0.1592 0.093 0.077 Uiso 1 1 calc R . . H34C H 1.0661 0.2692 0.09 0.077 Uiso 1 1 calc R . . C40 C 0.5802(8) 0.0288(5) 0.3532(4) 0.046(2) Uani 1 1 d . . . C41 C 0.6180(11) 0.0758(7) 0.4235(5) 0.086(3) Uani 1 1 d . . . H41A H 0.7021 0.1012 0.4236 0.129 Uiso 1 1 calc R . . H41B H 0.6161 0.0299 0.4608 0.129 Uiso 1 1 calc R . . H41C H 0.5597 0.1262 0.431 0.129 Uiso 1 1 calc R . . C42 C 0.4454(8) -0.0126(7) 0.3513(5) 0.067(3) Uani 1 1 d . . . H42A H 0.4232 -0.042 0.3063 0.1 Uiso 1 1 calc R . . H42B H 0.3864 0.0374 0.3584 0.1 Uiso 1 1 calc R . . H42C H 0.4426 -0.0591 0.3881 0.1 Uiso 1 1 calc R . . C43 C 0.6760(10) -0.0524(7) 0.3443(6) 0.093(4) Uani 1 1 d . . . H43A H 0.6541 -0.0842 0.3001 0.139 Uiso 1 1 calc R . . H43B H 0.6735 -0.0967 0.3824 0.139 Uiso 1 1 calc R . . H43C H 0.7599 -0.0264 0.3447 0.139 Uiso 1 1 calc R . . C50 C 0.5698(8) 0.3057(6) 0.2599(5) 0.060(3) Uani 1 1 d . . . H50A H 0.6595 0.315 0.2737 0.072 Uiso 1 1 calc R . . H50B H 0.5513 0.3458 0.2188 0.072 Uiso 1 1 calc R . . C51 C 0.5083(7) 0.3587(5) 0.3165(5) 0.046(2) Uani 1 1 d . . . C52 C 0.5450(15) 0.4591(8) 0.3215(9) 0.153(6) Uani 1 1 d . . . H52A H 0.5203 0.4901 0.2773 0.23 Uiso 1 1 calc R . . H52B H 0.6352 0.4639 0.332 0.23 Uiso 1 1 calc R . . H52C H 0.5034 0.489 0.3584 0.23 Uiso 1 1 calc R . . C53 C 0.3671(9) 0.3542(10) 0.3060(7) 0.119(5) Uani 1 1 d . . . H53A H 0.3385 0.3792 0.2602 0.179 Uiso 1 1 calc R . . H53B H 0.3318 0.391 0.3419 0.179 Uiso 1 1 calc R . . H53C H 0.34 0.2894 0.309 0.179 Uiso 1 1 calc R . . C54 C 0.5503(13) 0.3205(9) 0.3882(6) 0.116(5) Uani 1 1 d . . . H54A H 0.5314 0.2539 0.3896 0.173 Uiso 1 1 calc R . . H54B H 0.5065 0.3531 0.423 0.173 Uiso 1 1 calc R . . H54C H 0.64 0.3298 0.398 0.173 Uiso 1 1 calc R . . H1 H 0.795(6) 0.161(4) 0.025(3) 0.029(17) Uiso 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 Ta1 0.03201(19) 0.03266(19) 0.03395(19) -0.00511(14) 0.00550(12) -0.00292(13) Cl1 0.0217(8) 0.0337(10) 0.0463(11) -0.0084(8) -0.0015(7) 0.0002(7) B1 0.027(4) 0.038(5) 0.032(4) -0.004(4) 0.002(3) -0.001(4) N1 0.040(4) 0.034(3) 0.042(4) 0.000(3) 0.001(3) 0.009(3) N2 0.033(3) 0.034(3) 0.035(4) 0.000(3) 0.005(3) 0.006(3) N3 0.031(3) 0.029(3) 0.035(3) -0.004(3) 0.007(3) -0.004(2) N4 0.038(3) 0.028(3) 0.029(3) -0.009(3) 0.004(3) 0.002(2) N5 0.024(3) 0.048(4) 0.041(4) -0.012(3) 0.001(3) -0.005(3) N6 0.030(3) 0.033(3) 0.031(3) -0.002(3) 0.004(3) 0.006(2) N7 0.059(5) 0.061(5) 0.039(4) -0.007(3) 0.003(3) -0.017(4) C10 0.058(6) 0.051(5) 0.068(6) 0.012(5) 0.011(5) 0.029(4) C11 0.041(4) 0.044(5) 0.046(5) 0.001(4) -0.003(4) 0.008(4) C12 0.050(5) 0.042(5) 0.042(5) 0.010(4) -0.004(4) 0.006(4) C13 0.052(5) 0.035(4) 0.037(5) 0.003(4) -0.003(4) -0.006(4) C14 0.067(6) 0.048(5) 0.050(5) 0.019(4) 0.009(5) 0.000(4) C20 0.045(5) 0.037(5) 0.065(6) -0.004(4) 0.004(4) -0.012(4) C21 0.031(4) 0.039(4) 0.042(5) -0.006(4) -0.006(3) 0.007(3) C22 0.053(5) 0.029(4) 0.050(5) -0.005(4) -0.001(4) 0.010(4) C23 0.043(4) 0.034(4) 0.033(4) -0.001(3) -0.002(3) 0.011(3) C24 0.070(6) 0.039(5) 0.045(5) -0.005(4) 0.007(4) 0.018(4) C30 0.045(5) 0.079(7) 0.039(5) 0.000(4) -0.002(4) -0.012(4) C31 0.042(5) 0.037(4) 0.031(4) 0.000(3) 0.001(3) -0.010(3) C32 0.026(4) 0.040(4) 0.044(5) -0.009(4) 0.000(3) 0.000(3) C33 0.024(4) 0.032(4) 0.041(5) 0.002(3) 0.001(3) 0.002(3) C34 0.032(4) 0.070(6) 0.053(5) -0.004(4) 0.012(4) 0.000(4) C40 0.060(5) 0.029(4) 0.048(5) 0.004(4) 0.001(4) -0.003(4) C41 0.129(10) 0.078(8) 0.054(6) 0.004(6) 0.023(6) -0.033(6) C42 0.063(6) 0.078(7) 0.064(6) 0.021(5) 0.027(5) -0.003(5) C43 0.080(8) 0.055(7) 0.137(11) 0.008(7) -0.024(7) 0.011(5) C50 0.057(6) 0.075(7) 0.046(5) -0.016(5) -0.003(4) 0.028(5) C51 0.051(5) 0.031(4) 0.058(6) -0.016(4) 0.003(4) 0.005(3) C52 0.228(18) 0.054(8) 0.188(16) -0.019(9) 0.075(13) -0.037(9) C53 0.051(7) 0.199(14) 0.111(10) -0.080(10) 0.023(6) 0.004(7) C54 0.146(12) 0.147(12) 0.055(7) -0.016(7) 0.012(8) 0.056(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N7 1.823(7) . ? Ta1 C50 2.127(8) . ? Ta1 N5 2.235(5) . ? Ta1 N3 2.306(5) . ? Ta1 Cl1 2.4066(16) . ? Ta1 N1 2.447(6) . ? B1 N2 1.529(10) . ? B1 N6 1.530(10) . ? B1 N4 1.539(9) . ? N1 N2 1.354(8) . ? N1 C11 1.356(9) . ? N2 C13 1.350(9) . ? N3 C21 1.343(8) . ? N3 N4 1.368(7) . ? N4 C23 1.345(8) . ? N5 N6 1.361(8) . ? N5 C31 1.365(9) . ? N6 C33 1.342(8) . ? N7 C40 1.443(10) . ? C10 C11 1.503(11) . ? C11 C12 1.357(11) . ? C12 C13 1.381(11) . ? C13 C14 1.486(11) . ? C20 C21 1.485(10) . ? C21 C22 1.391(10) . ? C22 C23 1.356(10) . ? C23 C24 1.501(10) . ? C30 C31 1.493(10) . ? C31 C32 1.360(10) . ? C32 C33 1.387(10) . ? C33 C34 1.470(10) . ? C40 C41 1.512(11) . ? C40 C42 1.540(11) . ? C40 C43 1.549(12) . ? C50 C51 1.506(11) . ? C51 C52 1.468(13) . ? C51 C53 1.492(12) . ? C51 C54 1.492(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Ta1 C50 101.8(3) . . ? N7 Ta1 N5 96.0(3) . . ? C50 Ta1 N5 87.3(3) . . ? N7 Ta1 N3 99.2(3) . . ? C50 Ta1 N3 155.8(3) . . ? N5 Ta1 N3 78.8(2) . . ? N7 Ta1 Cl1 95.8(2) . . ? C50 Ta1 Cl1 99.7(2) . . ? N5 Ta1 Cl1 164.69(16) . . ? N3 Ta1 Cl1 89.73(14) . . ? N7 Ta1 N1 174.7(2) . . ? C50 Ta1 N1 83.0(3) . . ? N5 Ta1 N1 82.0(2) . . ? N3 Ta1 N1 75.63(19) . . ? Cl1 Ta1 N1 85.42(15) . . ? N2 B1 N6 109.6(6) . . ? N2 B1 N4 109.3(6) . . ? N6 B1 N4 108.6(6) . . ? N2 N1 C11 105.3(6) . . ? N2 N1 Ta1 119.1(4) . . ? C11 N1 Ta1 135.1(5) . . ? C13 N2 N1 110.8(6) . . ? C13 N2 B1 128.7(6) . . ? N1 N2 B1 120.4(6) . . ? C21 N3 N4 106.4(6) . . ? C21 N3 Ta1 132.0(5) . . ? N4 N3 Ta1 121.5(4) . . ? C23 N4 N3 110.0(5) . . ? C23 N4 B1 128.8(6) . . ? N3 N4 B1 121.2(5) . . ? N6 N5 C31 105.8(5) . . ? N6 N5 Ta1 123.3(4) . . ? C31 N5 Ta1 130.9(5) . . ? C33 N6 N5 110.5(5) . . ? C33 N6 B1 128.0(6) . . ? N5 N6 B1 121.3(5) . . ? C40 N7 Ta1 171.0(5) . . ? N1 C11 C12 110.6(7) . . ? N1 C11 C10 123.9(7) . . ? C12 C11 C10 125.4(7) . . ? C11 C12 C13 106.4(7) . . ? N2 C13 C12 106.9(7) . . ? N2 C13 C14 123.7(7) . . ? C12 C13 C14 129.4(7) . . ? N3 C21 C22 108.9(7) . . ? N3 C21 C20 124.2(7) . . ? C22 C21 C20 126.9(7) . . ? C23 C22 C21 107.0(7) . . ? N4 C23 C22 107.7(7) . . ? N4 C23 C24 123.4(7) . . ? C22 C23 C24 128.9(7) . . ? C32 C31 N5 109.7(7) . . ? C32 C31 C30 127.3(7) . . ? N5 C31 C30 122.9(6) . . ? C31 C32 C33 106.8(6) . . ? N6 C33 C32 107.1(6) . . ? N6 C33 C34 123.1(7) . . ? C32 C33 C34 129.8(7) . . ? N7 C40 C41 112.9(7) . . ? N7 C40 C42 108.4(6) . . ? C41 C40 C42 110.8(8) . . ? N7 C40 C43 107.8(8) . . ? C41 C40 C43 107.4(8) . . ? C42 C40 C43 109.5(7) . . ? C51 C50 Ta1 138.0(7) . . ? C52 C51 C53 107.8(9) . . ? C52 C51 C54 103.6(10) . . ? C53 C51 C54 108.5(10) . . ? C52 C51 C50 113.2(9) . . ? C53 C51 C50 112.2(7) . . ? C54 C51 C50 111.1(7) . . ? _database_code_depnum_ccdc_archive 'CCDC 902493' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4a _audit_creation_date 2013-11-07T13:58:14-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C23 H42 B1 Cl1 N7 Nb1 Si1),0.5(C6 H14)' _chemical_formula_sum 'C49 H91 B2 Cl2 N14 Nb2 Si2' _chemical_formula_weight 1210.88 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9978(7) _cell_length_b 38.529(5) _cell_length_c 17.280(2) _cell_angle_alpha 90 _cell_angle_beta 98.009(7) _cell_angle_gamma 90 _cell_volume 6591.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 261 _cell_measurement_theta_min 3.48 _cell_measurement_theta_max 16.25 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.22 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2548 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 3 -1 0.061 0 -3 1 0.048 3 7 4 0.15 -3 -6 -4 0.165 0 -2 -1 0.092 1 5 3 0.079 -1 8 3 0.093 1 -18 -7 0.075 8 7 -1 0.136 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.506 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.658 _exptl_absorpt_correction_T_max 0.766 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1379 _diffrn_reflns_av_unetI/netI 0.1897 _diffrn_reflns_number 41498 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 26.8 _diffrn_reflns_theta_full 26.8 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.977 _reflns_number_total 13770 _reflns_number_gt 6528 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR2002 (Giacovazzo et al, 2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 13770 _refine_ls_number_parameters 637 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1781 _refine_ls_R_factor_gt 0.071 _refine_ls_wR_factor_ref 0.1897 _refine_ls_wR_factor_gt 0.1545 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.074 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.107 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.11329(6) 0.192236(16) 0.81014(3) 0.02681(17) Uani 1 1 d . . . Nb1A Nb 0.61098(6) 0.094895(16) 0.39043(4) 0.02864(18) Uani 1 1 d . . . Si1 Si 0.42737(19) 0.24169(5) 0.78271(11) 0.0350(5) Uani 1 1 d . . . Si1A Si 0.5728(2) 0.13568(6) 0.19088(12) 0.0434(5) Uani 1 1 d . . . Cl1 Cl -0.09161(17) 0.21909(5) 0.75003(11) 0.0461(5) Uani 1 1 d . . . Cl1A Cl 0.79454(19) 0.05512(5) 0.41375(12) 0.0564(6) Uani 1 1 d . . . B1 B 0.2309(7) 0.1225(2) 0.7143(4) 0.0276(18) Uani 1 1 d . . . B1A B 0.2940(8) 0.0618(2) 0.3462(5) 0.035(2) Uani 1 1 d . . . N1 N 0.1607(5) 0.18469(13) 0.6768(3) 0.0268(12) Uani 1 1 d . . . N1A N 0.5187(6) 0.05216(14) 0.2964(3) 0.0389(15) Uani 1 1 d . . . N2 N 0.2165(5) 0.15364(13) 0.6582(3) 0.0266(12) Uani 1 1 d . . . N2A N 0.3815(6) 0.04528(14) 0.2913(3) 0.0374(14) Uani 1 1 d . . . N3 N 0.0269(5) 0.13816(14) 0.7799(3) 0.0322(14) Uani 1 1 d . . . N3A N 0.4814(5) 0.06259(13) 0.4610(3) 0.0280(13) Uani 1 1 d . . . N4 N 0.0923(5) 0.11421(14) 0.7389(3) 0.0301(13) Uani 1 1 d . . . N4A N 0.3511(5) 0.05292(13) 0.4305(3) 0.0292(13) Uani 1 1 d . . . N5 N 0.3257(5) 0.13176(13) 0.7893(3) 0.0268(13) Uani 1 1 d . . . N5A N 0.4055(5) 0.12061(13) 0.3615(3) 0.0276(12) Uani 1 1 d . . . N6 N 0.2961(5) 0.15750(13) 0.8391(3) 0.0253(12) Uani 1 1 d . . . N6A N 0.2921(5) 0.10128(14) 0.3375(3) 0.0297(13) Uani 1 1 d . . . N7 N 0.0770(5) 0.19703(14) 0.9064(3) 0.0334(14) Uani 1 1 d . . . N7A N 0.6824(5) 0.12526(14) 0.4601(3) 0.0338(14) Uani 1 1 d . . . C10 C 0.2996(8) 0.1238(2) 0.5457(4) 0.054(2) Uani 1 1 d . . . H10A H 0.3158 0.1052 0.5826 0.081 Uiso 1 1 calc R . . H10B H 0.383 0.1304 0.5282 0.081 Uiso 1 1 calc R . . H10C H 0.2365 0.1164 0.5018 0.081 Uiso 1 1 calc R . . C10A C 0.7077(8) 0.0330(2) 0.2274(5) 0.076(3) Uani 1 1 d . . . H10D H 0.7589 0.0486 0.2633 0.115 Uiso 1 1 calc R . . H10E H 0.7113 0.0406 0.1748 0.115 Uiso 1 1 calc R . . H10F H 0.745 0.0101 0.2343 0.115 Uiso 1 1 calc R . . C11 C 0.2423(6) 0.15437(18) 0.5841(4) 0.0309(16) Uani 1 1 d . . . C11A C 0.5656(8) 0.0325(2) 0.2423(4) 0.050(2) Uani 1 1 d . . . C12 C 0.2048(6) 0.18683(18) 0.5541(4) 0.0344(17) Uani 1 1 d . . . H12 H 0.2124 0.1951 0.5044 0.041 Uiso 1 1 calc R . . C12A C 0.4600(10) 0.0128(2) 0.2034(5) 0.064(3) Uani 1 1 d . . . H12A H 0.4656 -0.003 0.1633 0.077 Uiso 1 1 calc R . . C13 C 0.1537(6) 0.20438(18) 0.6134(4) 0.0318(16) Uani 1 1 d . . . C13A C 0.3457(9) 0.0213(2) 0.2359(5) 0.051(2) Uani 1 1 d . . . C14 C 0.0967(7) 0.24017(17) 0.6070(4) 0.0392(18) Uani 1 1 d . . . H14A H 0.0681 0.2466 0.6558 0.059 Uiso 1 1 calc R . . H14B H 0.0208 0.2408 0.5664 0.059 Uiso 1 1 calc R . . H14C H 0.1645 0.2561 0.5948 0.059 Uiso 1 1 calc R . . C14A C 0.2031(9) 0.0085(2) 0.2149(5) 0.076(3) Uani 1 1 d . . . H14D H 0.1467 0.0189 0.2492 0.114 Uiso 1 1 calc R . . H14E H 0.2012 -0.0163 0.2205 0.114 Uiso 1 1 calc R . . H14F H 0.1704 0.0147 0.1619 0.114 Uiso 1 1 calc R . . C20 C 0.0574(7) 0.05499(18) 0.6806(4) 0.048(2) Uani 1 1 d . . . H20A H 0.1452 0.0592 0.666 0.072 Uiso 1 1 calc R . . H20B H -0.0065 0.0515 0.6344 0.072 Uiso 1 1 calc R . . H20C H 0.0605 0.0347 0.713 0.072 Uiso 1 1 calc R . . C20A C 0.6343(6) 0.05416(19) 0.5862(4) 0.0404(18) Uani 1 1 d . . . H20D H 0.6943 0.068 0.5602 0.061 Uiso 1 1 calc R . . H20E H 0.6741 0.0318 0.5983 0.061 Uiso 1 1 calc R . . H20F H 0.6186 0.0655 0.6336 0.061 Uiso 1 1 calc R . . C21 C 0.0158(7) 0.08541(18) 0.7246(4) 0.0341(17) Uani 1 1 d . . . C21A C 0.5048(6) 0.04982(16) 0.5346(4) 0.0283(15) Uani 1 1 d . . . C22 C -0.1002(7) 0.09084(19) 0.7577(4) 0.0433(19) Uani 1 1 d . . . H22 H -0.1712 0.0753 0.7582 0.052 Uiso 1 1 calc R . . C22A C 0.3908(7) 0.03155(17) 0.5504(4) 0.0354(17) Uani 1 1 d . . . H22A H 0.3812 0.0196 0.5961 0.043 Uiso 1 1 calc R . . C23 C -0.0913(6) 0.1239(2) 0.7902(4) 0.0374(18) Uani 1 1 d . . . C23A C 0.2953(7) 0.03469(17) 0.4847(4) 0.0356(17) Uani 1 1 d . . . C24 C -0.1910(7) 0.1430(2) 0.8332(4) 0.051(2) Uani 1 1 d . . . H24A H -0.1552 0.1654 0.849 0.076 Uiso 1 1 calc R . . H24B H -0.206 0.1299 0.8785 0.076 Uiso 1 1 calc R . . H24C H -0.2749 0.1457 0.7993 0.076 Uiso 1 1 calc R . . C24A C 0.1537(6) 0.0225(2) 0.4706(4) 0.050(2) Uani 1 1 d . . . H24D H 0.1142 0.0288 0.4187 0.074 Uiso 1 1 calc R . . H24E H 0.1035 0.0331 0.5078 0.074 Uiso 1 1 calc R . . H24F H 0.1515 -0.0022 0.4763 0.074 Uiso 1 1 calc R . . C30 C 0.4996(7) 0.08621(19) 0.7788(5) 0.051(2) Uani 1 1 d . . . H30A H 0.443 0.0816 0.7303 0.077 Uiso 1 1 calc R . . H30B H 0.5056 0.0658 0.8109 0.077 Uiso 1 1 calc R . . H30C H 0.5882 0.0926 0.7685 0.077 Uiso 1 1 calc R . . C30A C 0.4619(7) 0.18392(18) 0.3821(5) 0.051(2) Uani 1 1 d . . . H30D H 0.5517 0.1752 0.3974 0.076 Uiso 1 1 calc R . . H30E H 0.4315 0.1956 0.4256 0.076 Uiso 1 1 calc R . . H30F H 0.4622 0.1999 0.3396 0.076 Uiso 1 1 calc R . . C31 C 0.4403(6) 0.11524(18) 0.8203(4) 0.0352(17) Uani 1 1 d . . . C31A C 0.3691(7) 0.15435(17) 0.3568(4) 0.0328(16) Uani 1 1 d . . . C32 C 0.4858(6) 0.13111(18) 0.8921(4) 0.0357(17) Uani 1 1 d . . . H32 H 0.5629 0.1255 0.9264 0.043 Uiso 1 1 calc R . . C32A C 0.2331(7) 0.15602(19) 0.3303(4) 0.0437(19) Uani 1 1 d . . . H32A H 0.1816 0.1761 0.3224 0.052 Uiso 1 1 calc R . . C33 C 0.3941(6) 0.15665(18) 0.9018(4) 0.0328(17) Uani 1 1 d . . . C33A C 0.1872(7) 0.1229(2) 0.3178(4) 0.0406(18) Uani 1 1 d . . . C34 C 0.3974(7) 0.18022(19) 0.9690(4) 0.0406(19) Uani 1 1 d . . . H34A H 0.3219 0.1958 0.9604 0.061 Uiso 1 1 calc R . . H34B H 0.4799 0.1933 0.975 0.061 Uiso 1 1 calc R . . H34C H 0.3925 0.1669 1.0155 0.061 Uiso 1 1 calc R . . C34A C 0.0463(7) 0.1100(2) 0.2882(5) 0.073(3) Uani 1 1 d . . . H34D H 0.0468 0.0851 0.2859 0.109 Uiso 1 1 calc R . . H34E H 0.0177 0.1192 0.2369 0.109 Uiso 1 1 calc R . . H34F H -0.0148 0.1175 0.323 0.109 Uiso 1 1 calc R . . C40 C 0.0352(7) 0.2043(2) 0.9823(4) 0.0436(19) Uani 1 1 d . . . C40A C 0.7719(7) 0.1474(2) 0.5135(5) 0.050(2) Uani 1 1 d . . . C41 C -0.1095(7) 0.2191(2) 0.9691(5) 0.059(2) Uani 1 1 d . . . H41A H -0.1112 0.2399 0.9384 0.088 Uiso 1 1 calc R . . H41B H -0.1379 0.2243 1.0186 0.088 Uiso 1 1 calc R . . H41C H -0.1695 0.2022 0.942 0.088 Uiso 1 1 calc R . . C41A C 0.8950(8) 0.1251(2) 0.5504(5) 0.079(3) Uani 1 1 d . . . H41D H 0.8634 0.106 0.5786 0.119 Uiso 1 1 calc R . . H41E H 0.955 0.1392 0.5855 0.119 Uiso 1 1 calc R . . H41F H 0.9422 0.1163 0.5097 0.119 Uiso 1 1 calc R . . C42 C 0.0424(8) 0.1712(2) 1.0318(4) 0.061(2) Uani 1 1 d . . . H42A H 0.1337 0.1627 1.0399 0.092 Uiso 1 1 calc R . . H42B H -0.0157 0.1538 1.0051 0.092 Uiso 1 1 calc R . . H42C H 0.0139 0.1762 1.0814 0.092 Uiso 1 1 calc R . . C42A C 0.6962(9) 0.1608(2) 0.5799(5) 0.074(3) Uani 1 1 d . . . H42D H 0.6201 0.1745 0.558 0.111 Uiso 1 1 calc R . . H42E H 0.7562 0.1747 0.6154 0.111 Uiso 1 1 calc R . . H42F H 0.6654 0.1414 0.6076 0.111 Uiso 1 1 calc R . . C43 C 0.1256(8) 0.2336(2) 1.0220(4) 0.059(2) Uani 1 1 d . . . H43A H 0.2176 0.2257 1.0313 0.088 Uiso 1 1 calc R . . H43B H 0.096 0.2396 1.0708 0.088 Uiso 1 1 calc R . . H43C H 0.1193 0.2536 0.9886 0.088 Uiso 1 1 calc R . . C43A C 0.8208(8) 0.1786(2) 0.4669(5) 0.071(3) Uani 1 1 d . . . H43D H 0.7441 0.192 0.4443 0.106 Uiso 1 1 calc R . . H43E H 0.868 0.1701 0.4261 0.106 Uiso 1 1 calc R . . H43F H 0.8802 0.193 0.5016 0.106 Uiso 1 1 calc R . . C50 C 0.2564(6) 0.23567(16) 0.8127(4) 0.0294(16) Uani 1 1 d . . . H50A H 0.2031 0.254 0.7848 0.035 Uiso 1 1 calc R . . H50B H 0.269 0.2428 0.8671 0.035 Uiso 1 1 calc R . . C50A C 0.6667(6) 0.12198(18) 0.2873(4) 0.0342(17) Uani 1 1 d . . . H50C H 0.7078 0.1433 0.3087 0.041 Uiso 1 1 calc R . . H50D H 0.7407 0.1082 0.273 0.041 Uiso 1 1 calc R . . C51 C 0.4282(7) 0.2827(2) 0.7272(5) 0.055(2) Uani 1 1 d . . . H51A H 0.3635 0.2812 0.6807 0.083 Uiso 1 1 calc R . . H51B H 0.5166 0.2865 0.7131 0.083 Uiso 1 1 calc R . . H51C H 0.4048 0.3016 0.7589 0.083 Uiso 1 1 calc R . . C51A C 0.5067(9) 0.18062(19) 0.1923(5) 0.062(2) Uani 1 1 d . . . H51D H 0.4583 0.1862 0.1419 0.092 Uiso 1 1 calc R . . H51E H 0.5807 0.1965 0.2045 0.092 Uiso 1 1 calc R . . H51F H 0.4471 0.1824 0.2311 0.092 Uiso 1 1 calc R . . C52 C 0.5567(7) 0.2481(2) 0.8703(4) 0.054(2) Uani 1 1 d . . . H52A H 0.5623 0.2276 0.9021 0.081 Uiso 1 1 calc R . . H52B H 0.5314 0.2675 0.9 0.081 Uiso 1 1 calc R . . H52C H 0.6429 0.2526 0.8538 0.081 Uiso 1 1 calc R . . C52A C 0.4251(8) 0.1079(2) 0.1512(5) 0.070(3) Uani 1 1 d . . . H52D H 0.3834 0.1172 0.1021 0.105 Uiso 1 1 calc R . . H52E H 0.3606 0.1076 0.1875 0.105 Uiso 1 1 calc R . . H52F H 0.4555 0.0847 0.1436 0.105 Uiso 1 1 calc R . . C53 C 0.4881(7) 0.20639(19) 0.7217(4) 0.052(2) Uani 1 1 d . . . H53A H 0.4232 0.2028 0.676 0.078 Uiso 1 1 calc R . . H53B H 0.499 0.1853 0.7516 0.078 Uiso 1 1 calc R . . H53C H 0.5732 0.213 0.7063 0.078 Uiso 1 1 calc R . . C53A C 0.6972(9) 0.1360(3) 0.1194(5) 0.086(3) Uani 1 1 d . . . H53D H 0.6524 0.1428 0.0689 0.129 Uiso 1 1 calc R . . H53E H 0.7348 0.1132 0.1162 0.129 Uiso 1 1 calc R . . H53F H 0.7681 0.1522 0.1364 0.129 Uiso 1 1 calc R . . C72 C 0.2322(16) 0.0545(5) 0.9362(10) 0.066(5) Uiso 0.5 1 d P . . H72A H 0.1901 0.0385 0.8967 0.08 Uiso 0.5 1 calc PR . . H72B H 0.2424 0.0765 0.9106 0.08 Uiso 0.5 1 calc PR . . C75 C -0.0982(16) 0.0546(5) 1.0224(10) 0.068(5) Uiso 0.5 1 d P . . H75A H -0.0876 0.0729 1.0614 0.082 Uiso 0.5 1 calc PR . . H75B H -0.0788 0.033 1.0508 0.082 Uiso 0.5 1 calc PR . . C74 C -0.0009(18) 0.0588(5) 0.9825(11) 0.081(6) Uiso 0.5 1 d P . . H74A H -0.0238 0.0805 0.9555 0.097 Uiso 0.5 1 calc PR . . H74B H -0.0183 0.041 0.9426 0.097 Uiso 0.5 1 calc PR . . C71 C 0.3583(19) 0.0422(6) 0.9633(12) 0.095(7) Uiso 0.5 1 d P . . H71A H 0.4088 0.0394 0.9203 0.142 Uiso 0.5 1 calc PR . . H71B H 0.3508 0.0202 0.9883 0.142 Uiso 0.5 1 calc PR . . H71C H 0.4041 0.0583 1.0001 0.142 Uiso 0.5 1 calc PR . . C73 C 0.1352(18) 0.0599(5) 0.9961(11) 0.083(6) Uiso 0.5 1 d P . . H73A H 0.1614 0.0429 1.0369 0.099 Uiso 0.5 1 calc PR . . H73B H 0.1577 0.0824 1.0193 0.099 Uiso 0.5 1 calc PR . . C76 C -0.2404(16) 0.0535(5) 0.9940(11) 0.076(6) Uiso 0.5 1 d P . . H76A H -0.2901 0.0502 1.0371 0.114 Uiso 0.5 1 calc PR . . H76B H -0.2586 0.0346 0.9578 0.114 Uiso 0.5 1 calc PR . . H76C H -0.2674 0.075 0.9682 0.114 Uiso 0.5 1 calc PR . . H1 H 0.2795 0.0994 0.6966 0.045 Uiso 1 1 d . . . H1A H 0.1942 0.0489 0.332 0.025 Uiso 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 Nb1 0.0235(3) 0.0302(3) 0.0273(3) -0.0020(3) 0.0053(3) 0.0008(3) Nb1A 0.0233(3) 0.0310(4) 0.0312(4) 0.0031(3) 0.0025(3) 0.0001(3) Si1 0.0317(11) 0.0385(12) 0.0347(12) -0.0027(9) 0.0039(9) -0.0058(9) Si1A 0.0503(13) 0.0423(13) 0.0370(13) 0.0020(10) 0.0046(10) -0.0034(11) Cl1 0.0294(10) 0.0558(13) 0.0525(12) 0.0012(10) 0.0036(9) 0.0093(9) Cl1A 0.0433(11) 0.0599(14) 0.0673(14) 0.0216(11) 0.0129(10) 0.0173(10) B1 0.020(4) 0.031(4) 0.032(5) -0.006(4) 0.003(3) -0.005(3) B1A 0.035(5) 0.028(5) 0.040(5) 0.003(4) 0.002(4) -0.007(4) N1 0.030(3) 0.024(3) 0.025(3) -0.002(2) 0.001(2) 0.001(2) N1A 0.052(4) 0.031(3) 0.035(4) -0.008(3) 0.012(3) 0.005(3) N2 0.026(3) 0.027(3) 0.027(3) -0.004(2) 0.002(2) 0.000(2) N2A 0.050(4) 0.027(3) 0.033(4) 0.001(3) 0.000(3) -0.008(3) N3 0.026(3) 0.041(4) 0.030(3) 0.004(3) 0.005(3) 0.001(3) N3A 0.027(3) 0.031(3) 0.027(3) 0.003(3) 0.004(2) 0.000(3) N4 0.027(3) 0.027(3) 0.035(3) 0.005(3) 0.001(3) -0.007(3) N4A 0.025(3) 0.026(3) 0.036(3) 0.003(3) 0.006(3) 0.000(2) N5 0.023(3) 0.030(3) 0.028(3) 0.003(3) 0.005(2) 0.004(2) N5A 0.022(3) 0.025(3) 0.035(3) -0.002(3) 0.000(2) 0.001(2) N6 0.022(3) 0.029(3) 0.025(3) -0.004(2) 0.002(2) 0.002(2) N6A 0.019(3) 0.032(3) 0.036(3) 0.005(3) -0.002(2) 0.000(3) N7 0.032(3) 0.034(3) 0.036(3) -0.002(3) 0.011(3) 0.003(3) N7A 0.030(3) 0.035(3) 0.034(3) 0.008(3) -0.003(3) -0.007(3) C10 0.082(6) 0.050(5) 0.034(4) -0.004(4) 0.024(4) 0.009(5) C10A 0.084(7) 0.077(7) 0.076(7) -0.009(5) 0.039(5) 0.030(6) C11 0.030(4) 0.035(4) 0.028(4) -0.003(3) 0.005(3) 0.005(3) C11A 0.070(6) 0.039(5) 0.045(5) -0.001(4) 0.015(4) 0.009(4) C12 0.037(4) 0.042(5) 0.026(4) -0.001(3) 0.011(3) 0.001(3) C12A 0.117(8) 0.028(5) 0.046(5) -0.010(4) 0.008(5) 0.004(5) C13 0.027(4) 0.037(4) 0.032(4) 0.006(3) 0.004(3) 0.000(3) C13A 0.078(6) 0.028(4) 0.046(5) 0.002(4) 0.004(5) -0.013(4) C14 0.055(5) 0.034(4) 0.028(4) 0.005(3) 0.002(3) 0.006(4) C14A 0.117(8) 0.060(6) 0.048(6) -0.005(5) -0.004(5) -0.054(6) C20 0.052(5) 0.033(4) 0.058(5) -0.005(4) 0.005(4) -0.012(4) C20A 0.036(4) 0.047(5) 0.037(4) 0.000(4) 0.001(3) -0.002(4) C21 0.036(4) 0.035(4) 0.029(4) 0.007(3) -0.001(3) -0.005(3) C21A 0.034(4) 0.024(4) 0.028(4) 0.001(3) 0.006(3) 0.008(3) C22 0.040(5) 0.039(5) 0.050(5) 0.007(4) 0.000(4) -0.013(4) C22A 0.040(4) 0.031(4) 0.038(4) 0.004(3) 0.016(4) 0.001(3) C23 0.020(4) 0.049(5) 0.043(5) 0.006(4) 0.001(3) -0.010(3) C23A 0.038(4) 0.028(4) 0.044(5) -0.002(3) 0.014(4) -0.003(3) C24 0.034(4) 0.060(6) 0.061(5) -0.011(4) 0.019(4) -0.015(4) C24A 0.031(4) 0.053(5) 0.064(6) 0.013(4) 0.008(4) -0.008(4) C30 0.036(4) 0.041(5) 0.076(6) -0.010(4) 0.001(4) 0.015(4) C30A 0.059(5) 0.032(5) 0.057(5) -0.002(4) -0.007(4) 0.001(4) C31 0.024(4) 0.036(4) 0.046(5) 0.010(4) 0.008(3) 0.003(3) C31A 0.034(4) 0.031(4) 0.034(4) 0.002(3) 0.007(3) 0.003(3) C32 0.024(4) 0.044(5) 0.037(4) 0.007(4) -0.004(3) 0.008(3) C32A 0.044(5) 0.037(5) 0.050(5) 0.008(4) 0.004(4) 0.015(4) C33 0.029(4) 0.040(4) 0.029(4) 0.004(3) 0.002(3) -0.001(3) C33A 0.032(4) 0.048(5) 0.039(4) 0.008(4) -0.006(3) 0.000(4) C34 0.040(4) 0.054(5) 0.026(4) -0.002(4) -0.001(3) 0.004(4) C34A 0.025(4) 0.087(7) 0.100(8) 0.027(6) -0.012(4) 0.004(5) C40 0.043(5) 0.053(5) 0.037(5) -0.010(4) 0.015(4) -0.006(4) C40A 0.045(5) 0.048(5) 0.050(5) 0.001(4) -0.017(4) -0.013(4) C41 0.051(5) 0.075(6) 0.056(6) -0.004(5) 0.027(4) 0.014(5) C41A 0.044(5) 0.100(8) 0.084(7) 0.038(6) -0.030(5) -0.024(5) C42 0.078(6) 0.071(6) 0.041(5) 0.014(5) 0.032(4) 0.011(5) C42A 0.088(7) 0.080(7) 0.052(6) -0.022(5) 0.002(5) -0.016(6) C43 0.073(6) 0.059(6) 0.047(5) -0.021(4) 0.015(4) -0.001(5) C43A 0.062(6) 0.064(6) 0.076(7) 0.023(5) -0.020(5) -0.033(5) C50 0.036(4) 0.025(4) 0.028(4) -0.006(3) 0.007(3) -0.004(3) C50A 0.028(4) 0.041(4) 0.034(4) 0.005(3) 0.003(3) -0.004(3) C51 0.043(5) 0.060(6) 0.063(6) 0.012(5) 0.010(4) -0.013(4) C51A 0.096(7) 0.043(5) 0.045(5) 0.014(4) 0.008(5) -0.008(5) C52 0.033(4) 0.073(6) 0.054(5) 0.004(4) 0.001(4) -0.008(4) C52A 0.085(7) 0.059(6) 0.056(6) 0.014(5) -0.026(5) -0.022(5) C53 0.033(4) 0.058(5) 0.070(6) -0.023(4) 0.028(4) -0.008(4) C53A 0.087(7) 0.124(10) 0.049(6) 0.002(6) 0.018(5) 0.012(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 N7 1.760(5) . ? Nb1 C50 2.198(6) . ? Nb1 N6 2.264(5) . ? Nb1 N3 2.288(6) . ? Nb1 Cl1 2.3985(18) . ? Nb1 N1 2.433(5) . ? Nb1A N7A 1.757(5) . ? Nb1A C50A 2.203(6) . ? Nb1A N3A 2.270(5) . ? Nb1A N5A 2.273(5) . ? Nb1A Cl1A 2.3818(19) . ? Nb1A N1A 2.405(6) . ? Si1 C51 1.850(8) . ? Si1 C52 1.865(7) . ? Si1 C50 1.869(6) . ? Si1 C53 1.873(7) . ? Si1A C51A 1.854(8) . ? Si1A C53A 1.871(8) . ? Si1A C50A 1.871(6) . ? Si1A C52A 1.874(7) . ? B1 N5 1.537(8) . ? B1 N2 1.538(9) . ? B1 N4 1.539(8) . ? B1A N2A 1.516(10) . ? B1A N4A 1.527(9) . ? B1A N6A 1.529(9) . ? N1 C13 1.327(8) . ? N1 N2 1.377(7) . ? N1A C11A 1.337(9) . ? N1A N2A 1.388(7) . ? N2 C11 1.341(8) . ? N2A C13A 1.345(9) . ? N3 C23 1.338(7) . ? N3 N4 1.382(7) . ? N3A C21A 1.353(7) . ? N3A N4A 1.386(6) . ? N4 C21 1.351(8) . ? N4A C23A 1.352(8) . ? N5 C31 1.355(7) . ? N5 N6 1.372(7) . ? N5A C31A 1.350(8) . ? N5A N6A 1.372(6) . ? N6 C33 1.356(8) . ? N6A C33A 1.346(8) . ? N7 C40 1.458(8) . ? N7A C40A 1.465(8) . ? C10 C11 1.503(9) . ? C10A C11A 1.479(10) . ? C11 C12 1.385(9) . ? C11A C12A 1.396(11) . ? C12 C13 1.382(8) . ? C12A C13A 1.381(11) . ? C13 C14 1.490(9) . ? C13A C14A 1.504(10) . ? C20 C21 1.488(9) . ? C20A C21A 1.476(8) . ? C21 C22 1.379(9) . ? C21A C22A 1.398(8) . ? C22 C23 1.388(10) . ? C22A C23A 1.383(9) . ? C23 C24 1.514(9) . ? C23A C24A 1.479(8) . ? C30 C31 1.495(9) . ? C30A C31A 1.496(9) . ? C31 C32 1.401(9) . ? C31A C32A 1.374(9) . ? C32 C33 1.371(9) . ? C32A C33A 1.362(10) . ? C33 C34 1.470(9) . ? C33A C34A 1.514(9) . ? C40 C42 1.534(10) . ? C40 C41 1.541(10) . ? C40 C43 1.544(10) . ? C40A C42A 1.549(11) . ? C40A C41A 1.562(10) . ? C40A C43A 1.565(10) . ? C72 C71 1.37(2) . ? C72 C73 1.53(2) . ? C75 C74 1.28(2) . ? C75 C76 1.44(2) . ? C74 C73 1.35(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Nb1 C50 96.9(2) . . ? N7 Nb1 N6 96.9(2) . . ? C50 Nb1 N6 86.7(2) . . ? N7 Nb1 N3 101.0(2) . . ? C50 Nb1 N3 157.2(2) . . ? N6 Nb1 N3 77.26(18) . . ? N7 Nb1 Cl1 95.04(17) . . ? C50 Nb1 Cl1 101.22(18) . . ? N6 Nb1 Cl1 164.81(14) . . ? N3 Nb1 Cl1 91.24(14) . . ? N7 Nb1 N1 178.9(2) . . ? C50 Nb1 N1 84.1(2) . . ? N6 Nb1 N1 83.17(17) . . ? N3 Nb1 N1 78.01(17) . . ? Cl1 Nb1 N1 84.76(13) . . ? N7A Nb1A C50A 96.6(2) . . ? N7A Nb1A N3A 101.8(2) . . ? C50A Nb1A N3A 157.2(2) . . ? N7A Nb1A N5A 97.4(2) . . ? C50A Nb1A N5A 86.5(2) . . ? N3A Nb1A N5A 77.94(18) . . ? N7A Nb1A Cl1A 94.73(18) . . ? C50A Nb1A Cl1A 99.54(18) . . ? N3A Nb1A Cl1A 92.32(14) . . ? N5A Nb1A Cl1A 165.76(14) . . ? N7A Nb1A N1A 178.3(2) . . ? C50A Nb1A N1A 83.9(2) . . ? N3A Nb1A N1A 78.09(19) . . ? N5A Nb1A N1A 84.27(19) . . ? Cl1A Nb1A N1A 83.56(15) . . ? C51 Si1 C52 104.7(4) . . ? C51 Si1 C50 108.7(3) . . ? C52 Si1 C50 110.4(3) . . ? C51 Si1 C53 107.6(4) . . ? C52 Si1 C53 108.1(4) . . ? C50 Si1 C53 116.5(3) . . ? C51A Si1A C53A 105.8(4) . . ? C51A Si1A C50A 112.8(3) . . ? C53A Si1A C50A 107.0(4) . . ? C51A Si1A C52A 105.9(4) . . ? C53A Si1A C52A 108.9(4) . . ? C50A Si1A C52A 115.9(3) . . ? N5 B1 N2 110.1(5) . . ? N5 B1 N4 106.8(5) . . ? N2 B1 N4 109.1(5) . . ? N2A B1A N4A 109.3(6) . . ? N2A B1A N6A 110.9(6) . . ? N4A B1A N6A 108.3(6) . . ? C13 N1 N2 106.2(5) . . ? C13 N1 Nb1 136.0(4) . . ? N2 N1 Nb1 117.6(4) . . ? C11A N1A N2A 106.7(6) . . ? C11A N1A Nb1A 136.1(5) . . ? N2A N1A Nb1A 117.2(4) . . ? C11 N2 N1 110.1(5) . . ? C11 N2 B1 127.3(5) . . ? N1 N2 B1 122.4(5) . . ? C13A N2A N1A 109.9(6) . . ? C13A N2A B1A 127.9(7) . . ? N1A N2A B1A 122.1(5) . . ? C23 N3 N4 106.4(5) . . ? C23 N3 Nb1 131.1(5) . . ? N4 N3 Nb1 122.3(4) . . ? C21A N3A N4A 106.8(5) . . ? C21A N3A Nb1A 131.9(4) . . ? N4A N3A Nb1A 121.3(4) . . ? C21 N4 N3 110.3(5) . . ? C21 N4 B1 128.9(6) . . ? N3 N4 B1 120.8(5) . . ? C23A N4A N3A 109.4(5) . . ? C23A N4A B1A 129.9(6) . . ? N3A N4A B1A 120.6(5) . . ? C31 N5 N6 109.6(5) . . ? C31 N5 B1 127.8(6) . . ? N6 N5 B1 122.4(5) . . ? C31A N5A N6A 107.4(5) . . ? C31A N5A Nb1A 131.4(4) . . ? N6A N5A Nb1A 120.9(4) . . ? C33 N6 N5 106.8(5) . . ? C33 N6 Nb1 131.4(4) . . ? N5 N6 Nb1 121.8(4) . . ? C33A N6A N5A 108.8(5) . . ? C33A N6A B1A 129.8(6) . . ? N5A N6A B1A 120.8(5) . . ? C40 N7 Nb1 172.9(5) . . ? C40A N7A Nb1A 166.5(5) . . ? N2 C11 C12 107.3(6) . . ? N2 C11 C10 122.7(6) . . ? C12 C11 C10 130.0(6) . . ? N1A C11A C12A 109.3(7) . . ? N1A C11A C10A 123.6(8) . . ? C12A C11A C10A 127.1(8) . . ? C13 C12 C11 105.9(6) . . ? C13A C12A C11A 106.7(7) . . ? N1 C13 C12 110.5(6) . . ? N1 C13 C14 124.4(6) . . ? C12 C13 C14 125.1(6) . . ? N2A C13A C12A 107.4(7) . . ? N2A C13A C14A 123.1(8) . . ? C12A C13A C14A 129.4(8) . . ? N4 C21 C22 106.7(6) . . ? N4 C21 C20 123.3(6) . . ? C22 C21 C20 130.0(7) . . ? N3A C21A C22A 109.1(6) . . ? N3A C21A C20A 123.3(6) . . ? C22A C21A C20A 127.5(6) . . ? C21 C22 C23 107.2(6) . . ? C23A C22A C21A 106.5(6) . . ? N3 C23 C22 109.4(6) . . ? N3 C23 C24 121.2(6) . . ? C22 C23 C24 129.4(6) . . ? N4A C23A C22A 108.0(6) . . ? N4A C23A C24A 121.9(6) . . ? C22A C23A C24A 130.0(6) . . ? N5 C31 C32 107.3(6) . . ? N5 C31 C30 122.1(6) . . ? C32 C31 C30 130.6(6) . . ? N5A C31A C32A 108.2(6) . . ? N5A C31A C30A 124.3(6) . . ? C32A C31A C30A 127.4(6) . . ? C33 C32 C31 106.4(6) . . ? C33A C32A C31A 107.8(6) . . ? N6 C33 C32 109.9(6) . . ? N6 C33 C34 123.4(6) . . ? C32 C33 C34 126.7(6) . . ? N6A C33A C32A 107.9(6) . . ? N6A C33A C34A 122.4(7) . . ? C32A C33A C34A 129.7(7) . . ? N7 C40 C42 110.1(6) . . ? N7 C40 C41 108.6(6) . . ? C42 C40 C41 111.1(6) . . ? N7 C40 C43 108.5(6) . . ? C42 C40 C43 112.4(7) . . ? C41 C40 C43 106.0(6) . . ? N7A C40A C42A 110.0(6) . . ? N7A C40A C41A 108.3(6) . . ? C42A C40A C41A 108.6(7) . . ? N7A C40A C43A 109.3(6) . . ? C42A C40A C43A 110.2(7) . . ? C41A C40A C43A 110.4(6) . . ? Si1 C50 Nb1 135.0(3) . . ? Si1A C50A Nb1A 134.6(3) . . ? C71 C72 C73 117.3(17) . . ? C74 C75 C76 127.6(18) . . ? C75 C74 C73 137(2) . . ? C74 C73 C72 126.7(18) . . ? _database_code_depnum_ccdc_archive 'CCDC 902494' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5a _audit_creation_date 2013-11-07T16:32:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H44 B1 Cl1 N7 Nb1' _chemical_formula_sum 'C29 H44 B Cl N7 Nb' _chemical_formula_weight 629.88 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.820(15) _cell_length_b 20.044(11) _cell_length_c 13.824(11) _cell_angle_alpha 90 _cell_angle_beta 105.81(8) _cell_angle_gamma 90 _cell_volume 3151(5) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 235 _cell_measurement_theta_min 3.56 _cell_measurement_theta_max 16.54 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -4 16 1 0.234 1 1 -3 0.156 1 -5 0 0.22 -3 -2 7 0.173 -7 -3 -1 0.094 3 2 1 0.222 -5 3 4 0.164 5 -3 -4 0.22 9 -18 19 0.183 -2 4 5 0.249 3 -7 -8 0.162 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.497 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.689 _exptl_absorpt_correction_T_max 0.775 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1079 _diffrn_reflns_av_unetI/netI 0.1073 _diffrn_reflns_number 16190 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 5518 _reflns_number_gt 3685 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR2002 (Giacovazzo et al, 2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+16.5092P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5518 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1573 _refine_ls_wR_factor_gt 0.1402 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.261 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.112 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' Cl Cl 0.1484 0.1585 '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' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.23273(5) 0.01938(3) 0.26368(4) 0.02081(17) Uani 1 1 d . . . Cl1 Cl 0.09920(15) -0.07191(8) 0.20027(13) 0.0341(4) Uani 1 1 d . . . B1 B 0.1545(6) 0.1262(4) 0.4262(5) 0.0234(15) Uani 1 1 d . . . N1 N 0.0500(4) 0.0796(3) 0.2532(4) 0.0239(11) Uani 1 1 d . . . N2 N 0.0512(4) 0.1244(3) 0.3292(4) 0.0223(11) Uani 1 1 d . . . N3 N 0.2106(4) 0.0048(2) 0.4199(4) 0.0249(11) Uani 1 1 d . . . N4 N 0.1710(4) 0.0559(3) 0.4703(4) 0.0240(11) Uani 1 1 d . . . N5 N 0.3237(4) 0.1073(2) 0.3500(4) 0.0204(10) Uani 1 1 d . . . N6 N 0.2685(4) 0.1482(2) 0.4027(4) 0.0220(11) Uani 1 1 d . . . N7 N 0.3577(4) -0.0291(3) 0.2660(4) 0.0259(11) Uani 1 1 d . . . C11 C -0.0558(5) 0.0854(3) 0.1860(5) 0.0281(15) Uani 1 1 d . . . C12 C -0.1212(5) 0.1332(3) 0.2196(5) 0.0282(14) Uani 1 1 d . . . H12 H -0.1976 0.1464 0.1872 0.034 Uiso 1 1 calc R . . C13 C -0.0529(5) 0.1574(3) 0.3091(5) 0.0254(14) Uani 1 1 d . . . C14 C -0.0922(6) 0.0467(4) 0.0905(5) 0.0401(17) Uani 1 1 d . . . H14A H -0.0297 0.0172 0.0863 0.06 Uiso 1 1 calc R . . H14B H -0.1091 0.0769 0.0344 0.06 Uiso 1 1 calc R . . H14C H -0.1612 0.0211 0.0892 0.06 Uiso 1 1 calc R . . C15 C -0.0807(6) 0.2089(4) 0.3767(6) 0.0373(17) Uani 1 1 d . . . H15A H -0.0141 0.215 0.4338 0.056 Uiso 1 1 calc R . . H15B H -0.1471 0.1946 0.3989 0.056 Uiso 1 1 calc R . . H15C H -0.0991 0.2503 0.3408 0.056 Uiso 1 1 calc R . . C21 C 0.2562(6) -0.1158(3) 0.4467(5) 0.0319(15) Uani 1 1 d . . . H21A H 0.2768 -0.1112 0.3845 0.048 Uiso 1 1 calc R . . H21B H 0.1932 -0.1474 0.4384 0.048 Uiso 1 1 calc R . . H21C H 0.3233 -0.1312 0.498 0.048 Uiso 1 1 calc R . . C22 C 0.2180(5) -0.0502(3) 0.4763(5) 0.0252(13) Uani 1 1 d . . . C23 C 0.1805(5) -0.0353(3) 0.5617(5) 0.0282(14) Uani 1 1 d . . . H23 H 0.1751 -0.0648 0.6122 0.034 Uiso 1 1 calc R . . C24 C 0.1533(5) 0.0317(3) 0.5558(4) 0.0256(14) Uani 1 1 d . . . C25 C 0.1090(6) 0.0729(4) 0.6280(5) 0.0373(17) Uani 1 1 d . . . H25A H 0.0972 0.118 0.604 0.056 Uiso 1 1 calc R . . H25B H 0.1655 0.0722 0.6927 0.056 Uiso 1 1 calc R . . H25C H 0.0358 0.0548 0.6335 0.056 Uiso 1 1 calc R . . C30 C 0.5212(6) 0.1024(3) 0.3149(5) 0.0292(15) Uani 1 1 d . . . H30A H 0.4897 0.062 0.2807 0.044 Uiso 1 1 calc R . . H30B H 0.5908 0.0923 0.3675 0.044 Uiso 1 1 calc R . . H30C H 0.5403 0.1328 0.268 0.044 Uiso 1 1 calc R . . C31 C 0.4315(5) 0.1338(3) 0.3594(4) 0.0235(13) Uani 1 1 d . . . C32 C 0.4429(5) 0.1921(3) 0.4140(5) 0.0284(14) Uani 1 1 d . . . H32 H 0.5074 0.2206 0.4293 0.034 Uiso 1 1 calc R . . C33 C 0.3396(6) 0.2000(3) 0.4416(5) 0.0259(14) Uani 1 1 d . . . C34 C 0.3078(6) 0.2536(4) 0.5030(6) 0.0394(17) Uani 1 1 d . . . H34A H 0.2301 0.2458 0.5095 0.059 Uiso 1 1 calc R . . H34B H 0.3099 0.2959 0.4709 0.059 Uiso 1 1 calc R . . H34C H 0.3628 0.254 0.5685 0.059 Uiso 1 1 calc R . . C40 C 0.4438(6) -0.0772(4) 0.2526(6) 0.0372(17) Uani 1 1 d . . . C41 C 0.5430(6) -0.0849(4) 0.3512(7) 0.051(2) Uani 1 1 d . . . H41A H 0.5809 -0.0426 0.3696 0.076 Uiso 1 1 calc R . . H41B H 0.5995 -0.1168 0.3417 0.076 Uiso 1 1 calc R . . H41C H 0.5102 -0.0999 0.4037 0.076 Uiso 1 1 calc R . . C42 C 0.4963(9) -0.0530(5) 0.1683(8) 0.066(3) Uani 1 1 d . . . H42A H 0.5345 -0.0108 0.1868 0.099 Uiso 1 1 calc R . . H42B H 0.4346 -0.048 0.1071 0.099 Uiso 1 1 calc R . . H42C H 0.5526 -0.085 0.1584 0.099 Uiso 1 1 calc R . . C43 C 0.3847(9) -0.1441(4) 0.2237(8) 0.066(3) Uani 1 1 d . . . H43A H 0.3525 -0.1594 0.2764 0.098 Uiso 1 1 calc R . . H43B H 0.4414 -0.1758 0.2138 0.098 Uiso 1 1 calc R . . H43C H 0.3227 -0.1395 0.1626 0.098 Uiso 1 1 calc R . . C50 C 0.2343(6) 0.0745(3) 0.1238(5) 0.0277(14) Uani 1 1 d . . . C51 C 0.2296(5) 0.1478(3) 0.0873(5) 0.0259(14) Uani 1 1 d . . . C52 C 0.1763(6) 0.1490(4) -0.0289(5) 0.0388(17) Uani 1 1 d . . . H52A H 0.0982 0.131 -0.0456 0.058 Uiso 1 1 calc R . . H52B H 0.2244 0.1226 -0.0602 0.058 Uiso 1 1 calc R . . H52C H 0.1737 0.1941 -0.0527 0.058 Uiso 1 1 calc R . . C53 C 0.1502(6) 0.1906(3) 0.1332(6) 0.0324(16) Uani 1 1 d . . . H53A H 0.0731 0.1712 0.1177 0.049 Uiso 1 1 calc R . . H53B H 0.1452 0.2348 0.1058 0.049 Uiso 1 1 calc R . . H53C H 0.1826 0.1925 0.2048 0.049 Uiso 1 1 calc R . . C54 C 0.3541(5) 0.1775(3) 0.1097(5) 0.0249(13) Uani 1 1 d . . . C55 C 0.3876(6) 0.2334(3) 0.1690(5) 0.0294(15) Uani 1 1 d . . . H55 H 0.3343 0.2535 0.1984 0.035 Uiso 1 1 calc R . . C56 C 0.5008(6) 0.2602(4) 0.1855(6) 0.0361(17) Uani 1 1 d . . . H56 H 0.522 0.2979 0.2256 0.043 Uiso 1 1 calc R . . C57 C 0.5805(7) 0.2309(4) 0.1423(6) 0.0418(19) Uani 1 1 d . . . H57 H 0.6559 0.2484 0.1537 0.05 Uiso 1 1 calc R . . C58 C 0.5481(6) 0.1757(4) 0.0824(6) 0.0378(17) Uani 1 1 d . . . H58 H 0.6017 0.156 0.0528 0.045 Uiso 1 1 calc R . . C59 C 0.4360(6) 0.1490(4) 0.0656(5) 0.0302(15) Uani 1 1 d . . . H59 H 0.4151 0.1118 0.0245 0.036 Uiso 1 1 calc R . . H1 H 0.139(5) 0.160(3) 0.482(5) 0.025(17) Uiso 1 1 d . . . H50B H 0.157(6) 0.047(3) 0.095(5) 0.031(18) Uiso 1 1 d . . . H50A H 0.281(7) 0.050(4) 0.089(7) 0.06(3) Uiso 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 Nb1 0.0199(3) 0.0222(3) 0.0195(3) -0.0021(3) 0.00389(18) -0.0006(2) Cl1 0.0349(9) 0.0291(8) 0.0348(9) -0.0056(7) 0.0036(7) -0.0080(7) B1 0.013(3) 0.031(4) 0.026(4) -0.002(3) 0.004(3) 0.000(3) N1 0.013(3) 0.030(3) 0.026(3) -0.003(2) 0.002(2) 0.000(2) N2 0.014(3) 0.026(3) 0.026(3) 0.000(2) 0.003(2) -0.001(2) N3 0.025(3) 0.023(3) 0.025(3) -0.003(2) 0.005(2) -0.001(2) N4 0.018(3) 0.030(3) 0.025(3) 0.000(2) 0.006(2) 0.001(2) N5 0.019(3) 0.023(3) 0.018(2) 0.001(2) 0.0023(19) 0.003(2) N6 0.024(3) 0.021(3) 0.023(3) -0.006(2) 0.010(2) -0.001(2) N7 0.024(3) 0.027(3) 0.027(3) -0.001(2) 0.008(2) 0.002(2) C11 0.020(3) 0.037(4) 0.027(3) 0.005(3) 0.005(3) -0.003(3) C12 0.019(3) 0.035(4) 0.030(4) 0.005(3) 0.005(3) 0.004(3) C13 0.021(3) 0.026(3) 0.032(4) 0.002(3) 0.011(3) 0.002(3) C14 0.032(4) 0.053(5) 0.028(4) -0.001(3) -0.006(3) 0.000(3) C15 0.031(4) 0.037(4) 0.044(4) -0.004(3) 0.011(3) 0.004(3) C21 0.040(4) 0.025(3) 0.030(4) 0.005(3) 0.007(3) 0.001(3) C22 0.013(3) 0.030(3) 0.030(3) 0.000(3) 0.003(2) -0.004(3) C23 0.029(3) 0.031(4) 0.026(3) 0.006(3) 0.009(3) -0.005(3) C24 0.021(3) 0.034(4) 0.020(3) 0.000(3) 0.003(2) -0.005(3) C25 0.039(4) 0.045(4) 0.033(4) 0.000(3) 0.019(3) 0.005(3) C30 0.024(3) 0.031(4) 0.033(4) -0.002(3) 0.008(3) -0.001(3) C31 0.019(3) 0.028(3) 0.020(3) 0.002(3) 0.000(2) -0.002(3) C32 0.018(3) 0.029(3) 0.037(4) -0.002(3) 0.005(3) -0.006(3) C33 0.030(4) 0.024(3) 0.023(3) -0.004(3) 0.005(3) -0.002(3) C34 0.037(4) 0.034(4) 0.048(4) -0.017(3) 0.013(3) -0.004(3) C40 0.038(4) 0.029(4) 0.047(4) 0.000(3) 0.016(3) 0.009(3) C41 0.026(4) 0.053(5) 0.071(6) 0.005(4) 0.008(4) 0.013(4) C42 0.083(7) 0.057(6) 0.078(7) 0.004(5) 0.056(6) 0.025(5) C43 0.069(6) 0.039(5) 0.093(8) -0.026(5) 0.030(5) 0.007(4) C50 0.024(4) 0.029(3) 0.032(3) 0.002(3) 0.011(3) -0.001(3) C51 0.026(3) 0.027(3) 0.023(3) 0.004(3) 0.004(3) 0.000(3) C52 0.034(4) 0.047(4) 0.031(4) 0.010(3) 0.000(3) 0.001(3) C53 0.021(3) 0.031(4) 0.046(4) 0.010(3) 0.010(3) 0.004(3) C54 0.023(3) 0.025(3) 0.026(3) 0.007(3) 0.005(3) 0.001(3) C55 0.030(4) 0.025(3) 0.033(4) 0.006(3) 0.008(3) 0.003(3) C56 0.030(4) 0.031(4) 0.043(4) 0.006(3) 0.003(3) -0.007(3) C57 0.031(4) 0.051(5) 0.044(4) 0.014(4) 0.012(3) -0.007(3) C58 0.023(4) 0.051(5) 0.044(4) 0.011(4) 0.016(3) 0.006(3) C59 0.028(4) 0.037(4) 0.027(3) 0.004(3) 0.009(3) 0.002(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 N7 1.761(5) . ? Nb1 C50 2.232(7) . ? Nb1 N5 2.233(5) . ? Nb1 N3 2.264(5) . ? Nb1 Cl1 2.419(2) . ? Nb1 N1 2.444(5) . ? B1 N4 1.527(9) . ? B1 N6 1.534(8) . ? B1 N2 1.550(8) . ? N1 C11 1.344(8) . ? N1 N2 1.379(7) . ? N2 C13 1.357(8) . ? N3 C22 1.340(8) . ? N3 N4 1.390(7) . ? N4 C24 1.346(8) . ? N5 C31 1.354(8) . ? N5 N6 1.374(7) . ? N6 C33 1.351(8) . ? N7 C40 1.451(8) . ? C11 C12 1.389(9) . ? C11 C14 1.490(10) . ? C12 C13 1.368(9) . ? C13 C15 1.488(9) . ? C21 C22 1.483(9) . ? C22 C23 1.401(9) . ? C23 C24 1.379(9) . ? C24 C25 1.495(9) . ? C30 C31 1.501(9) . ? C31 C32 1.377(9) . ? C32 C33 1.384(9) . ? C33 C34 1.480(9) . ? C40 C43 1.514(11) . ? C40 C42 1.541(11) . ? C40 C41 1.544(11) . ? C50 C51 1.550(9) . ? C51 C53 1.529(9) . ? C51 C54 1.539(9) . ? C51 C52 1.558(9) . ? C54 C55 1.382(9) . ? C54 C59 1.398(9) . ? C55 C56 1.401(10) . ? C56 C57 1.377(11) . ? C57 C58 1.374(11) . ? C58 C59 1.388(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Nb1 C50 94.8(2) . . ? N7 Nb1 N5 98.4(2) . . ? C50 Nb1 N5 87.4(2) . . ? N7 Nb1 N3 103.0(2) . . ? C50 Nb1 N3 157.1(2) . . ? N5 Nb1 N3 75.92(18) . . ? N7 Nb1 Cl1 92.89(19) . . ? C50 Nb1 Cl1 102.66(19) . . ? N5 Nb1 Cl1 164.18(13) . . ? N3 Nb1 Cl1 90.82(14) . . ? N7 Nb1 N1 175.6(2) . . ? C50 Nb1 N1 85.4(2) . . ? N5 Nb1 N1 86.02(18) . . ? N3 Nb1 N1 77.92(19) . . ? Cl1 Nb1 N1 82.74(15) . . ? N4 B1 N6 109.1(5) . . ? N4 B1 N2 107.9(5) . . ? N6 B1 N2 110.7(5) . . ? C11 N1 N2 106.5(5) . . ? C11 N1 Nb1 136.4(4) . . ? N2 N1 Nb1 116.8(3) . . ? C13 N2 N1 109.9(5) . . ? C13 N2 B1 128.5(5) . . ? N1 N2 B1 121.1(5) . . ? C22 N3 N4 107.0(5) . . ? C22 N3 Nb1 131.0(4) . . ? N4 N3 Nb1 121.7(4) . . ? C24 N4 N3 109.3(5) . . ? C24 N4 B1 130.5(5) . . ? N3 N4 B1 120.3(5) . . ? C31 N5 N6 106.6(5) . . ? C31 N5 Nb1 131.7(4) . . ? N6 N5 Nb1 121.7(4) . . ? C33 N6 N5 109.6(5) . . ? C33 N6 B1 128.6(5) . . ? N5 N6 B1 120.8(5) . . ? C40 N7 Nb1 168.2(5) . . ? N1 C11 C12 109.0(6) . . ? N1 C11 C14 123.9(6) . . ? C12 C11 C14 127.1(6) . . ? C13 C12 C11 107.5(6) . . ? N2 C13 C12 107.0(5) . . ? N2 C13 C15 123.5(6) . . ? C12 C13 C15 129.5(6) . . ? N3 C22 C23 109.2(6) . . ? N3 C22 C21 123.0(6) . . ? C23 C22 C21 127.7(6) . . ? C24 C23 C22 106.3(5) . . ? N4 C24 C23 108.2(5) . . ? N4 C24 C25 123.7(6) . . ? C23 C24 C25 128.1(6) . . ? N5 C31 C32 109.5(5) . . ? N5 C31 C30 123.2(6) . . ? C32 C31 C30 127.3(6) . . ? C31 C32 C33 106.7(5) . . ? N6 C33 C32 107.6(5) . . ? N6 C33 C34 123.9(6) . . ? C32 C33 C34 128.5(6) . . ? N7 C40 C43 109.4(6) . . ? N7 C40 C42 109.2(6) . . ? C43 C40 C42 109.4(7) . . ? N7 C40 C41 110.1(6) . . ? C43 C40 C41 109.3(7) . . ? C42 C40 C41 109.5(7) . . ? C51 C50 Nb1 138.0(5) . . ? C53 C51 C54 111.2(5) . . ? C53 C51 C50 111.6(5) . . ? C54 C51 C50 110.6(5) . . ? C53 C51 C52 107.3(6) . . ? C54 C51 C52 107.3(5) . . ? C50 C51 C52 108.6(6) . . ? C55 C54 C59 117.9(6) . . ? C55 C54 C51 122.4(6) . . ? C59 C54 C51 119.6(6) . . ? C54 C55 C56 120.9(6) . . ? C57 C56 C55 120.1(7) . . ? C58 C57 C56 119.6(7) . . ? C57 C58 C59 120.5(7) . . ? C58 C59 C54 120.9(7) . . ? _database_code_depnum_ccdc_archive 'CCDC 902495' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5b _audit_creation_date 2012-03-05T13:07:00-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H44 B1 Cl1 N7 Ta1' _chemical_formula_sum 'C29 H44 B Cl N7 Ta' _chemical_formula_weight 717.92 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7974(7) _cell_length_b 11.6980(7) _cell_length_c 13.9965(11) _cell_angle_alpha 83.471(5) _cell_angle_beta 89.385(6) _cell_angle_gamma 63.341(4) _cell_volume 1568.07(19) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 245 _cell_measurement_theta_min 3.45 _cell_measurement_theta_max 12.23 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 9 5 10 0.127 -12 -8 -13 0.148 2 11 -1 0.114 -1 -11 1 0.173 -3 6 7 0.099 3 -5 -6 0.166 -3 -4 4 0.172 2 1 -4 0.181 -11 -7 -12 0.089 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.62 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.214 _exptl_absorpt_correction_T_max 0.254 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_unetI/netI 0.0611 _diffrn_reflns_number 13499 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 7132 _reflns_number_gt 5832 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+3.1994P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7132 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.029 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 0.835 _refine_ls_restrained_S_all 0.835 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.003 _refine_diff_density_max 2.217 _refine_diff_density_min -1.226 _refine_diff_density_rms 0.11 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Cl Cl 0.1484 0.1585 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta 0.328739(15) 0.406362(15) 0.797537(11) 0.02417(6) Uani 1 1 d . . . Cl1 Cl 0.12800(10) 0.37361(10) 0.82681(7) 0.0347(2) Uani 1 1 d . . . B1 B 0.6418(5) 0.1343(4) 0.8341(3) 0.0287(9) Uani 1 1 d . . . N1 N 0.4195(3) 0.1952(3) 0.7385(2) 0.0290(7) Uani 1 1 d . . . N2 N 0.5565(3) 0.1092(3) 0.7604(2) 0.0279(7) Uani 1 1 d . . . N3 N 0.4380(3) 0.2650(3) 0.9316(2) 0.0265(7) Uani 1 1 d . . . N4 N 0.5634(3) 0.1586(3) 0.9284(2) 0.0273(7) Uani 1 1 d . . . N5 N 0.5471(3) 0.3759(3) 0.7822(2) 0.0269(7) Uani 1 1 d . . . N6 N 0.6588(3) 0.2552(3) 0.7971(2) 0.0269(7) Uani 1 1 d . . . N7 N 0.2653(3) 0.5550(3) 0.8453(2) 0.0276(7) Uani 1 1 d . . . C10 C 0.2267(4) 0.2004(4) 0.6364(4) 0.0441(11) Uani 1 1 d . . . H10A H 0.1746 0.2826 0.6592 0.066 Uiso 1 1 calc R . . H10B H 0.1838 0.1456 0.6554 0.066 Uiso 1 1 calc R . . H10C H 0.2285 0.2121 0.5675 0.066 Uiso 1 1 calc R . . C11 C 0.3715(4) 0.1398(4) 0.6788(3) 0.0327(9) Uani 1 1 d . . . C12 C 0.4763(5) 0.0207(4) 0.6623(3) 0.0361(9) Uani 1 1 d . . . H12 H 0.4693 -0.036 0.6237 0.043 Uiso 1 1 calc R . . C13 C 0.5929(4) 0.0027(4) 0.7143(3) 0.0332(9) Uani 1 1 d . . . C14 C 0.7346(5) -0.1065(4) 0.7226(3) 0.0461(11) Uani 1 1 d . . . H14A H 0.7924 -0.0894 0.7645 0.069 Uiso 1 1 calc R . . H14B H 0.7727 -0.1167 0.6601 0.069 Uiso 1 1 calc R . . H14C H 0.7302 -0.1841 0.7485 0.069 Uiso 1 1 calc R . . C20 C 0.2641(4) 0.3563(4) 1.0556(3) 0.0386(10) Uani 1 1 d . . . H20A H 0.2154 0.4215 1.0029 0.058 Uiso 1 1 calc R . . H20B H 0.2828 0.3951 1.1068 0.058 Uiso 1 1 calc R . . H20C H 0.2081 0.315 1.0783 0.058 Uiso 1 1 calc R . . C21 C 0.3970(4) 0.2590(4) 1.0225(3) 0.0302(8) Uani 1 1 d . . . C22 C 0.4962(4) 0.1504(4) 1.0764(3) 0.0339(9) Uani 1 1 d . . . H22 H 0.4934 0.124 1.1413 0.041 Uiso 1 1 calc R . . C23 C 0.5996(4) 0.0889(4) 1.0157(3) 0.0292(8) Uani 1 1 d . . . C24 C 0.7307(5) -0.0326(4) 1.0367(3) 0.0431(11) Uani 1 1 d . . . H24A H 0.782 -0.0511 0.9793 0.065 Uiso 1 1 calc R . . H24B H 0.7091 -0.1022 1.0586 0.065 Uiso 1 1 calc R . . H24C H 0.7854 -0.0228 1.0858 0.065 Uiso 1 1 calc R . . C30 C 0.5136(4) 0.6006(4) 0.7359(3) 0.0396(10) Uani 1 1 d . . . H30A H 0.4174 0.621 0.7412 0.059 Uiso 1 1 calc R . . H30B H 0.5291 0.6281 0.6715 0.059 Uiso 1 1 calc R . . H30C H 0.5388 0.644 0.7805 0.059 Uiso 1 1 calc R . . C31 C 0.5988(4) 0.4607(4) 0.7579(3) 0.0304(8) Uani 1 1 d . . . C32 C 0.7425(4) 0.3938(4) 0.7579(3) 0.0336(9) Uani 1 1 d . . . H32 H 0.8035 0.4291 0.7439 0.04 Uiso 1 1 calc R . . C33 C 0.7774(4) 0.2654(4) 0.7823(3) 0.0343(9) Uani 1 1 d . . . C34 C 0.9178(5) 0.1518(5) 0.7931(4) 0.0584(14) Uani 1 1 d . . . H34A H 0.9082 0.0746 0.8112 0.088 Uiso 1 1 calc R . . H34B H 0.9725 0.1621 0.8419 0.088 Uiso 1 1 calc R . . H34C H 0.9627 0.1457 0.733 0.088 Uiso 1 1 calc R . . C40 C 0.2057(4) 0.6701(4) 0.8945(3) 0.0310(8) Uani 1 1 d . . . C41 C 0.3061(5) 0.6553(5) 0.9761(3) 0.0444(11) Uani 1 1 d . . . H41A H 0.323 0.5798 1.0197 0.067 Uiso 1 1 calc R . . H41B H 0.2666 0.7298 1.0099 0.067 Uiso 1 1 calc R . . H41C H 0.392 0.6469 0.95 0.067 Uiso 1 1 calc R . . C42 C 0.0666(5) 0.6858(5) 0.9324(4) 0.0511(12) Uani 1 1 d . . . H42A H 0.0806 0.6112 0.976 0.077 Uiso 1 1 calc R . . H42B H 0.0056 0.6952 0.8795 0.077 Uiso 1 1 calc R . . H42C H 0.0261 0.761 0.9654 0.077 Uiso 1 1 calc R . . C43 C 0.1785(5) 0.7909(4) 0.8253(3) 0.0458(11) Uani 1 1 d . . . H43A H 0.2647 0.7836 0.8004 0.069 Uiso 1 1 calc R . . H43B H 0.137 0.8654 0.859 0.069 Uiso 1 1 calc R . . H43C H 0.117 0.7993 0.773 0.069 Uiso 1 1 calc R . . C50 C 0.2993(4) 0.4689(4) 0.6400(3) 0.0286(8) Uani 1 1 d . . . C51 C 0.1799(4) 0.5844(4) 0.5786(3) 0.0294(8) Uani 1 1 d . . . C52 C 0.0424(4) 0.6254(4) 0.6292(3) 0.0380(10) Uani 1 1 d . . . H52A H 0.0241 0.5524 0.6437 0.057 Uiso 1 1 calc R . . H52B H -0.0314 0.6913 0.5878 0.057 Uiso 1 1 calc R . . H52C H 0.0485 0.6583 0.6879 0.057 Uiso 1 1 calc R . . C53 C 0.1607(5) 0.5408(5) 0.4824(3) 0.0415(10) Uani 1 1 d . . . H53A H 0.1387 0.4698 0.4946 0.062 Uiso 1 1 calc R . . H53B H 0.245 0.5145 0.4484 0.062 Uiso 1 1 calc R . . H53C H 0.0866 0.6111 0.4441 0.062 Uiso 1 1 calc R . . C54 C 0.2146(4) 0.6979(4) 0.5537(3) 0.0315(9) Uani 1 1 d . . . C55 C 0.1313(5) 0.8207(4) 0.5763(3) 0.0417(10) Uani 1 1 d . . . H55 H 0.0504 0.8367 0.6084 0.05 Uiso 1 1 calc R . . C56 C 0.1665(6) 0.9213(5) 0.5517(4) 0.0505(12) Uani 1 1 d . . . H56 H 0.1106 1.0025 0.5695 0.061 Uiso 1 1 calc R . . C57 C 0.2828(5) 0.9012(5) 0.5015(3) 0.0490(12) Uani 1 1 d . . . H57 H 0.3059 0.9684 0.4851 0.059 Uiso 1 1 calc R . . C58 C 0.3654(5) 0.7803(5) 0.4757(4) 0.0494(12) Uani 1 1 d . . . H58 H 0.4439 0.7659 0.4409 0.059 Uiso 1 1 calc R . . C59 C 0.3312(5) 0.6796(4) 0.5016(3) 0.0416(10) Uani 1 1 d . . . H59 H 0.3875 0.5986 0.4836 0.05 Uiso 1 1 calc R . . H1 H 0.739(4) 0.056(3) 0.849(2) 0.013(8) Uiso 1 1 d . . . H2B H 0.302(5) 0.401(5) 0.623(4) 0.052(15) Uiso 1 1 d . . . H2A H 0.388(4) 0.467(4) 0.617(3) 0.033(11) Uiso 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 Ta1 0.02309(8) 0.02473(9) 0.02416(8) -0.00021(5) -0.00086(5) -0.01088(6) Cl1 0.0291(5) 0.0393(5) 0.0396(5) -0.0012(4) 0.0020(4) -0.0196(4) B1 0.027(2) 0.025(2) 0.031(2) 0.0014(17) -0.0012(18) -0.0097(19) N1 0.0256(16) 0.0283(17) 0.0315(17) 0.0005(13) -0.0032(13) -0.0116(14) N2 0.0278(16) 0.0256(16) 0.0291(17) -0.0008(13) 0.0018(13) -0.0115(14) N3 0.0253(16) 0.0293(17) 0.0247(16) 0.0030(13) -0.0028(12) -0.0134(14) N4 0.0270(16) 0.0276(17) 0.0270(16) 0.0011(13) -0.0023(13) -0.0130(14) N5 0.0235(15) 0.0320(17) 0.0253(16) 0.0004(13) -0.0007(12) -0.0136(14) N6 0.0212(15) 0.0300(17) 0.0273(16) -0.0003(13) 0.0007(12) -0.0102(14) N7 0.0233(15) 0.0323(18) 0.0259(16) 0.0003(13) -0.0002(13) -0.0122(14) C10 0.037(2) 0.045(3) 0.054(3) -0.012(2) -0.008(2) -0.020(2) C11 0.035(2) 0.033(2) 0.033(2) -0.0017(17) -0.0018(17) -0.0186(19) C12 0.047(2) 0.031(2) 0.033(2) -0.0103(17) 0.0035(19) -0.020(2) C13 0.042(2) 0.027(2) 0.030(2) -0.0019(16) 0.0038(17) -0.0157(18) C14 0.044(3) 0.035(2) 0.046(3) -0.007(2) 0.003(2) -0.006(2) C20 0.038(2) 0.051(3) 0.029(2) 0.0020(19) 0.0053(18) -0.024(2) C21 0.034(2) 0.035(2) 0.027(2) -0.0002(16) 0.0013(16) -0.0218(18) C22 0.043(2) 0.040(2) 0.025(2) 0.0068(17) -0.0034(17) -0.027(2) C23 0.034(2) 0.0252(19) 0.029(2) 0.0018(15) -0.0044(16) -0.0152(17) C24 0.044(3) 0.034(2) 0.043(3) 0.0089(19) -0.013(2) -0.013(2) C30 0.040(2) 0.034(2) 0.047(3) 0.0026(19) 0.003(2) -0.020(2) C31 0.036(2) 0.038(2) 0.0220(18) -0.0002(16) 0.0014(16) -0.0211(19) C32 0.032(2) 0.045(2) 0.032(2) -0.0029(18) 0.0065(17) -0.0247(19) C33 0.027(2) 0.044(2) 0.033(2) -0.0031(18) 0.0027(16) -0.0185(19) C34 0.025(2) 0.053(3) 0.090(4) -0.002(3) 0.013(2) -0.013(2) C40 0.032(2) 0.026(2) 0.032(2) -0.0077(16) 0.0019(16) -0.0095(17) C41 0.057(3) 0.048(3) 0.036(2) -0.008(2) -0.002(2) -0.030(2) C42 0.033(2) 0.048(3) 0.069(3) -0.018(2) 0.015(2) -0.013(2) C43 0.056(3) 0.026(2) 0.044(3) -0.0032(19) 0.000(2) -0.009(2) C50 0.032(2) 0.027(2) 0.026(2) -0.0003(16) -0.0022(16) -0.0134(18) C51 0.031(2) 0.031(2) 0.0245(19) -0.0012(16) -0.0035(15) -0.0124(17) C52 0.028(2) 0.043(2) 0.038(2) -0.0001(19) -0.0039(17) -0.0134(19) C53 0.046(3) 0.050(3) 0.031(2) -0.0041(19) -0.0067(19) -0.023(2) C54 0.031(2) 0.035(2) 0.0254(19) 0.0017(16) -0.0038(16) -0.0126(18) C55 0.045(2) 0.035(2) 0.036(2) -0.0026(18) 0.0020(19) -0.010(2) C56 0.064(3) 0.035(3) 0.047(3) -0.003(2) 0.003(2) -0.017(2) C57 0.067(3) 0.049(3) 0.038(3) 0.007(2) -0.005(2) -0.035(3) C58 0.050(3) 0.051(3) 0.048(3) 0.003(2) 0.010(2) -0.025(2) C59 0.042(2) 0.037(2) 0.039(2) 0.0006(19) 0.0059(19) -0.014(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N7 1.767(3) . ? Ta1 C50 2.222(4) . ? Ta1 N5 2.232(3) . ? Ta1 N3 2.289(3) . ? Ta1 Cl1 2.3881(9) . ? Ta1 N1 2.454(3) . ? B1 N2 1.527(5) . ? B1 N6 1.539(5) . ? B1 N4 1.544(5) . ? N1 C11 1.349(5) . ? N1 N2 1.378(4) . ? N2 C13 1.364(5) . ? N3 C21 1.347(5) . ? N3 N4 1.372(4) . ? N4 C23 1.344(5) . ? N5 C31 1.352(5) . ? N5 N6 1.380(4) . ? N6 C33 1.350(5) . ? N7 C40 1.458(5) . ? C10 C11 1.493(6) . ? C11 C12 1.388(6) . ? C12 C13 1.381(6) . ? C13 C14 1.484(6) . ? C20 C21 1.486(6) . ? C21 C22 1.381(6) . ? C22 C23 1.372(6) . ? C23 C24 1.489(6) . ? C30 C31 1.469(6) . ? C31 C32 1.390(5) . ? C32 C33 1.376(6) . ? C33 C34 1.496(6) . ? C40 C42 1.525(6) . ? C40 C41 1.524(6) . ? C40 C43 1.531(6) . ? C50 C51 1.556(5) . ? C51 C52 1.534(5) . ? C51 C54 1.538(6) . ? C51 C53 1.540(5) . ? C54 C55 1.382(6) . ? C54 C59 1.392(6) . ? C55 C56 1.399(7) . ? C56 C57 1.371(7) . ? C57 C58 1.380(7) . ? C58 C59 1.394(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Ta1 C50 102.12(15) . . ? N7 Ta1 N5 97.01(13) . . ? C50 Ta1 N5 86.49(13) . . ? N7 Ta1 N3 100.84(13) . . ? C50 Ta1 N3 153.78(14) . . ? N5 Ta1 N3 78.29(11) . . ? N7 Ta1 Cl1 96.07(10) . . ? C50 Ta1 Cl1 100.53(11) . . ? N5 Ta1 Cl1 163.51(8) . . ? N3 Ta1 Cl1 89.42(8) . . ? N7 Ta1 N1 177.49(12) . . ? C50 Ta1 N1 80.40(13) . . ? N5 Ta1 N1 82.99(11) . . ? N3 Ta1 N1 76.69(11) . . ? Cl1 Ta1 N1 83.51(8) . . ? N2 B1 N6 110.0(3) . . ? N2 B1 N4 108.6(3) . . ? N6 B1 N4 108.4(3) . . ? C11 N1 N2 105.9(3) . . ? C11 N1 Ta1 135.6(3) . . ? N2 N1 Ta1 118.2(2) . . ? C13 N2 N1 110.4(3) . . ? C13 N2 B1 128.7(3) . . ? N1 N2 B1 120.7(3) . . ? C21 N3 N4 106.5(3) . . ? C21 N3 Ta1 131.1(3) . . ? N4 N3 Ta1 122.3(2) . . ? C23 N4 N3 109.8(3) . . ? C23 N4 B1 129.5(3) . . ? N3 N4 B1 120.7(3) . . ? C31 N5 N6 106.8(3) . . ? C31 N5 Ta1 130.9(3) . . ? N6 N5 Ta1 122.3(2) . . ? C33 N6 N5 109.5(3) . . ? C33 N6 B1 128.3(3) . . ? N5 N6 B1 122.0(3) . . ? C40 N7 Ta1 172.6(3) . . ? N1 C11 C12 110.1(4) . . ? N1 C11 C10 124.1(4) . . ? C12 C11 C10 125.8(4) . . ? C13 C12 C11 106.7(4) . . ? N2 C13 C12 106.9(3) . . ? N2 C13 C14 123.1(4) . . ? C12 C13 C14 130.0(4) . . ? N3 C21 C22 109.3(4) . . ? N3 C21 C20 123.4(4) . . ? C22 C21 C20 127.3(4) . . ? C23 C22 C21 106.8(3) . . ? N4 C23 C22 107.6(3) . . ? N4 C23 C24 123.3(4) . . ? C22 C23 C24 129.0(4) . . ? N5 C31 C32 108.9(4) . . ? N5 C31 C30 124.3(4) . . ? C32 C31 C30 126.8(4) . . ? C33 C32 C31 107.0(3) . . ? N6 C33 C32 107.8(4) . . ? N6 C33 C34 123.0(4) . . ? C32 C33 C34 129.2(4) . . ? N7 C40 C42 108.3(3) . . ? N7 C40 C41 108.9(3) . . ? C42 C40 C41 111.4(4) . . ? N7 C40 C43 111.2(3) . . ? C42 C40 C43 107.7(4) . . ? C41 C40 C43 109.3(4) . . ? C51 C50 Ta1 131.7(3) . . ? C52 C51 C54 111.7(3) . . ? C52 C51 C53 107.1(3) . . ? C54 C51 C53 106.7(3) . . ? C52 C51 C50 110.6(3) . . ? C54 C51 C50 111.8(3) . . ? C53 C51 C50 108.7(3) . . ? C55 C54 C59 117.5(4) . . ? C55 C54 C51 123.1(4) . . ? C59 C54 C51 119.3(4) . . ? C54 C55 C56 121.2(4) . . ? C57 C56 C55 120.5(5) . . ? C56 C57 C58 119.3(5) . . ? C57 C58 C59 120.1(4) . . ? C58 C59 C54 121.4(4) . . ? # END of CIF _database_code_depnum_ccdc_archive 'CCDC 902496'