Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global # *** Added by check_cif _publ_contact_author_name 'Malcolm L.H.Green' _publ_contact_author_address ; Inorganic Chemistry Laboratory, University of Oxford, South Parks Road, Oxford. OX1 3QR ; _publ_contact_author_phone '(01865) 272649' _publ_contact_author_fax '(01865) 272690 ' _publ_contact_author_email 'Malcolm.Green@chemistry.ox.ac.uk' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _journal_coden_Cambridge 186 loop_ _publ_author_name 'Chen, Chi-Tien' 'Cowley, Andrew R.' 'Green, Malcolm L. H.' 'Rees, Leigh H.' data_str30 _database_code_CSD 155032 _audit_creation_date 1999-09-06T11:43:41-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic _publ_requested_category FO #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C26 H32 Br1 N4' _chemical_formula_structural 'C26 H32 BR1 N4' _chemical_formula_sum 'C22 H32 Br N4' _chemical_formula_weight 432.43 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _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 14.0530(6) _cell_length_b 10.0580(6) _cell_length_c 17.5050(10) _cell_angle_alpha 90 _cell_angle_beta 113.913(3) _cell_angle_gamma 90 _cell_volume 2261.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 124 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 25.28 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow / colourless' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.27 _exptl_crystal_density_method none _exptl_crystal_F_000 908 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.831 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_number 4450 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 26.36 _reflns_number_total 4450 _reflns_number_gt 3373 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Enraf-Nonius DIP2000 Software - XPRESS' _computing_cell_refinement DENZO _computing_data_reduction 'DENZO & SCALEPACK' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.9507P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_extinction_method none _refine_ls_number_reflns 4447 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_gt 0.0932 _refine_ls_wR_factor_all 0.1077 _refine_ls_goodness_of_fit_gt 1.086 _refine_ls_goodness_of_fit_all 1.012 _refine_ls_restrained_S_all 1.083 _refine_ls_restrained_S_obs 1.086 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.595 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.076 #----------------------------------------------------------------------------# # 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' Br Br -0.2901 2.4595 '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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group N1 N 0.3957(2) 0.5122(3) 1.0885(2) 0.0275(6) Uani 1 d . . H1 H 0.4628(2) 0.5023(3) 1.1019(2) 0.033 Uiso 1 calc R . N2 N 0.1982(2) 0.5582(2) 0.9347(2) 0.0249(5) Uani 1 d . . H2 H 0.2493(2) 0.6139(2) 0.9416(2) 0.03 Uiso 1 calc R . C1 C 0.3391(2) 0.4294(3) 1.0300(2) 0.0231(6) Uani 1 d . . C2 C 0.2222(2) 0.4450(3) 0.9807(2) 0.0238(6) Uani 1 d . . C11 C 0.3730(2) 0.6202(3) 1.1382(2) 0.0329(7) Uani 1 d . . C12 C 0.2616(3) 0.6248(3) 1.1289(2) 0.0326(7) Uani 1 d . . H12A H 0.2169(3) 0.656(2) 1.0727(5) 0.049 Uiso 1 calc R . H12B H 0.2559(4) 0.6856(18) 1.1706(10) 0.049 Uiso 1 calc R . H12C H 0.2396(6) 0.5355(6) 1.1374(14) 0.049 Uiso 1 calc R . C13 C 0.4047(4) 0.7497(4) 1.1125(4) 0.077(2) Uani 1 d . . H13A H 0.398(3) 0.8215(8) 1.1478(17) 0.116 Uiso 1 calc R . H13B H 0.360(2) 0.7681(19) 1.0539(8) 0.116 Uiso 1 calc R . H13C H 0.4773(10) 0.7439(14) 1.119(2) 0.116 Uiso 1 calc R . C14 C 0.4418(3) 0.5840(6) 1.2291(3) 0.071(2) Uani 1 d . . H14A H 0.432(2) 0.6502(19) 1.2665(3) 0.107 Uiso 1 calc R . H14B H 0.5150(4) 0.583(3) 1.2370(6) 0.107 Uiso 1 calc R . H14C H 0.4221(18) 0.4960(15) 1.2419(7) 0.107 Uiso 1 calc R . N21 N 0.3877(2) 0.3285(2) 1.0128(2) 0.0254(6) Uani 1 d . . H21 H 0.4548(2) 0.3223(2) 1.0437(2) 0.031 Uiso 1 calc R . C22 C 0.3447(2) 0.2288(3) 0.9504(2) 0.0256(7) Uani 1 d . . C23 C 0.3738(3) 0.0981(3) 0.9742(2) 0.0335(8) Uani 1 d . . H23 H 0.4200(3) 0.0777(3) 1.0300(2) 0.04 Uiso 1 calc R . C24 C 0.3342(3) -0.0016(4) 0.9154(3) 0.0416(9) Uani 1 d . . H24 H 0.3545(3) -0.0912(4) 0.9308(3) 0.05 Uiso 1 calc R . C25 C 0.2665(3) 0.0270(4) 0.8357(2) 0.0422(9) Uani 1 d . . H25 H 0.2384(3) -0.0427(4) 0.7963(2) 0.051 Uiso 1 calc R . C26 C 0.2386(3) 0.1576(4) 0.8122(2) 0.0374(8) Uani 1 d . . H26 H 0.1912(3) 0.1771(4) 0.7566(2) 0.045 Uiso 1 calc R . C27 C 0.2795(2) 0.2598(3) 0.8691(2) 0.0296(7) Uani 1 d . . H27 H 0.2629(2) 0.3497(3) 0.8525(2) 0.035 Uiso 1 calc R . C31 C 0.0928(2) 0.5955(3) 0.8738(2) 0.0285(7) Uani 1 d . . C32 C 0.0172(2) 0.6041(4) 0.9160(2) 0.0377(8) Uani 1 d . . H32A H 0.0069(15) 0.5153(5) 0.9344(14) 0.057 Uiso 1 calc R . H32B H -0.0496(7) 0.639(2) 0.8763(5) 0.057 Uiso 1 calc R . H32C H 0.0458(9) 0.664(2) 0.9644(9) 0.057 Uiso 1 calc R . C33 C 0.0543(3) 0.4967(4) 0.8014(2) 0.0414(9) Uani 1 d . . H33A H -0.0153(9) 0.5229(14) 0.7614(8) 0.062 Uiso 1 calc R . H33B H 0.0513(18) 0.4076(6) 0.8229(3) 0.062 Uiso 1 calc R . H33C H 0.1022(11) 0.4964(18) 0.7734(10) 0.062 Uiso 1 calc R . C34 C 0.1042(3) 0.7329(4) 0.8415(3) 0.0420(9) Uani 1 d . . H34A H 0.0364(5) 0.7630(11) 0.8006(12) 0.063 Uiso 1 calc R . H34B H 0.1534(15) 0.7281(6) 0.8148(14) 0.063 Uiso 1 calc R . H34C H 0.1302(18) 0.7957(7) 0.8883(3) 0.063 Uiso 1 calc R . N41 N 0.1550(2) 0.3606(3) 0.9811(2) 0.0253(5) Uani 1 d . . H41 H 0.0894(2) 0.3761(3) 0.9484(2) 0.03 Uiso 1 calc R . C42 C 0.1780(2) 0.2444(3) 1.0299(2) 0.0274(7) Uani 1 d . . C43 C 0.2446(3) 0.2380(3) 1.1136(2) 0.0320(7) Uani 1 d . . H43 H 0.2822(3) 0.3149(3) 1.1409(2) 0.038 Uiso 1 calc R . C44 C 0.2569(3) 0.1202(3) 1.1580(2) 0.0381(8) Uani 1 d . . H44 H 0.3025(3) 0.1173(3) 1.2155(2) 0.046 Uiso 1 calc R . C45 C 0.2036(3) 0.0079(4) 1.1194(3) 0.0446(10) Uani 1 d . . H45 H 0.2123(3) -0.0726(4) 1.1499(3) 0.054 Uiso 1 calc R . C46 C 0.1374(3) 0.0127(4) 1.0361(3) 0.0468(10) Uani 1 d . . H46 H 0.1009(3) -0.0650(4) 1.0091(3) 0.056 Uiso 1 calc R . C47 C 0.1236(3) 0.1301(4) 0.9912(2) 0.0362(7) Uani 1 d . . H47 H 0.0769(3) 0.1326(4) 0.9340(2) 0.043 Uiso 1 calc R . Br1 Br 0.37249(2) 0.63117(3) 0.85165(2) 0.02854(11) Uani 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 N1 0.0209(12) 0.0296(15) 0.0317(15) -0.0071(12) 0.0105(12) 0.0038(10) N2 0.0233(12) 0.0220(13) 0.0266(14) 0.0008(11) 0.0072(11) 0.0002(10) C1 0.0252(15) 0.024(2) 0.021(2) -0.0008(13) 0.0104(13) 0.0004(12) C2 0.0231(14) 0.024(2) 0.023(2) -0.0031(13) 0.0084(13) 0.0027(12) C11 0.031(2) 0.031(2) 0.036(2) -0.014(2) 0.0127(15) 0.0002(14) C12 0.038(2) 0.030(2) 0.035(2) -0.005(2) 0.019(2) 0.0062(15) C13 0.097(4) 0.035(2) 0.143(5) -0.031(3) 0.093(4) -0.022(2) C14 0.049(2) 0.107(4) 0.040(2) -0.036(3) 0.000(2) 0.027(3) N21 0.0231(12) 0.0254(14) 0.0251(14) -0.0034(11) 0.0070(11) 0.0022(10) C22 0.0226(14) 0.029(2) 0.030(2) -0.0057(14) 0.0148(14) -0.0012(12) C23 0.039(2) 0.030(2) 0.030(2) 0.0007(14) 0.013(2) 0.0064(14) C24 0.056(2) 0.024(2) 0.051(2) -0.005(2) 0.029(2) -0.003(2) C25 0.057(2) 0.034(2) 0.045(2) -0.019(2) 0.030(2) -0.017(2) C26 0.040(2) 0.045(2) 0.027(2) -0.007(2) 0.013(2) -0.009(2) C27 0.033(2) 0.028(2) 0.030(2) -0.0008(14) 0.0146(15) 0.0007(13) C31 0.0251(15) 0.032(2) 0.027(2) 0.0090(14) 0.0096(14) 0.0072(12) C32 0.027(2) 0.050(2) 0.038(2) 0.011(2) 0.014(2) 0.0118(15) C33 0.035(2) 0.049(2) 0.032(2) -0.001(2) 0.005(2) 0.008(2) C34 0.041(2) 0.037(2) 0.047(2) 0.019(2) 0.017(2) 0.010(2) N41 0.0198(11) 0.0258(14) 0.0276(13) 0.0022(12) 0.0067(11) 0.0033(10) C42 0.0255(15) 0.026(2) 0.034(2) 0.0031(14) 0.0155(14) 0.0034(12) C43 0.034(2) 0.028(2) 0.035(2) 0.0035(15) 0.015(2) 0.0042(14) C44 0.041(2) 0.034(2) 0.043(2) 0.010(2) 0.022(2) 0.012(2) C45 0.057(2) 0.028(2) 0.062(3) 0.014(2) 0.037(2) 0.013(2) C46 0.058(2) 0.021(2) 0.070(3) -0.005(2) 0.035(2) -0.006(2) C47 0.039(2) 0.034(2) 0.038(2) -0.002(2) 0.018(2) -0.004(2) Br1 0.0233(2) 0.0286(2) 0.0328(2) 0.0005(2) 0.01047(12) 0.00025(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 N1 C1 1.309(4) . ? N1 C11 1.504(4) . ? N2 C2 1.356(4) . ? N2 C31 1.480(4) . ? C1 N21 1.324(4) . ? C1 C2 1.523(4) . ? C2 N41 1.271(4) . ? C11 C13 1.503(5) . ? C11 C12 1.507(4) . ? C11 C14 1.535(6) . ? N21 C22 1.424(4) . ? C22 C27 1.380(5) . ? C22 C23 1.389(5) . ? C23 C24 1.383(5) . ? C24 C25 1.364(6) . ? C25 C26 1.385(5) . ? C26 C27 1.384(5) . ? C31 C32 1.522(4) . ? C31 C33 1.527(5) . ? C31 C34 1.526(5) . ? N41 C42 1.406(4) . ? C42 C43 1.384(5) . ? C42 C47 1.395(5) . ? C43 C44 1.389(5) . ? C44 C45 1.372(5) . ? C45 C46 1.376(6) . ? C46 C47 1.387(5) . ? 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 C1 N1 C11 135.1(2) . . ? C2 N2 C31 125.2(3) . . ? N1 C1 N21 117.4(3) . . ? N1 C1 C2 123.5(3) . . ? N21 C1 C2 119.1(3) . . ? N41 C2 N2 123.8(3) . . ? N41 C2 C1 124.2(3) . . ? N2 C2 C1 112.0(2) . . ? C13 C11 N1 107.2(3) . . ? C13 C11 C12 111.2(3) . . ? N1 C11 C12 114.5(3) . . ? C13 C11 C14 112.1(4) . . ? N1 C11 C14 103.7(3) . . ? C12 C11 C14 108.0(3) . . ? C1 N21 C22 128.1(3) . . ? C27 C22 C23 121.0(3) . . ? C27 C22 N21 122.0(3) . . ? C23 C22 N21 117.0(3) . . ? C24 C23 C22 118.8(3) . . ? C25 C24 C23 120.8(3) . . ? C24 C25 C26 120.0(3) . . ? C27 C26 C25 120.4(3) . . ? C22 C27 C26 118.9(3) . . ? N2 C31 C32 110.9(3) . . ? N2 C31 C33 110.3(3) . . ? C32 C31 C33 111.0(3) . . ? N2 C31 C34 105.8(3) . . ? C32 C31 C34 109.1(3) . . ? C33 C31 C34 109.7(3) . . ? C2 N41 C42 124.7(3) . . ? C43 C42 C47 118.5(3) . . ? C43 C42 N41 124.9(3) . . ? C47 C42 N41 116.4(3) . . ? C42 C43 C44 120.7(3) . . ? C45 C44 C43 120.5(4) . . ? C44 C45 C46 119.5(3) . . ? C45 C46 C47 120.6(4) . . ? C46 C47 C42 120.2(3) . . ? #=END data_Compound_6 _database_code_CSD 155033 _audit_creation_date 00-22-06 _audit_creation_method CRYSTALS_ver_12-03-99 #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Enraf-nonius DIP2000 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; DIP2000 software 'Xpress' (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SHELXS86 (Sheldrick, 1986)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** _cell_length_a 11.2870(7) _cell_angle_alpha 90 _cell_length_b 10.705(1) _cell_angle_beta 96.282(6) _cell_length_c 12.5560(11) _cell_angle_gamma 90 _cell_volume 1508.0(5) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,y+1/2,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'Ta ' -1.2580 6.5230 29.2024 1.7733 15.2293 9.3705 14.5135 0.2960 4.7649 63.3644 9.2435 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum 'C26 H39 Cl3 N5 Ta' _chemical_formula_moiety 'C26 H39 Cl3 N5 Ta' _chemical_compound_source ; ? ; _chemical_formula_weight 708.94 _cell_measurement_reflns_used 24613 _cell_measurement_theta_min 0 _cell_measurement_theta_max 26.57 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.10 _exptl_crystal_density_diffrn 1.56 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 706.37 _exptl_absorpt_coefficient_mu 3.93 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'refined from delta-F (Walker & Stuart , 1983)' _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 0.67 #diffrn_ambient_temperature 150 _diffrn_reflns_number 24613 _reflns_number_total 3245 _diffrn_reflns_av_R_equivalents 0.05 _diffrn_measured_fraction_theta_max 1.000 _reflns_number_gt 2603 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _refine_diff_density_min -3.72 _refine_diff_density_max 1.70 _reflns_threshold_expression >4.00\s(I) _refine_ls_number_reflns 2603 _refine_ls_number_parameters 316 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.0382 _refine_ls_goodness_of_fit_ref 0.8379 _refine_ls_shift/su_max 0.006453 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 5 parameters, Carruthers & Watkin , 1979, 1.25 -1.96 0.333 -.318 -.413 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Ta1 0.23394(4) 0.00368(19) 0.10375(4) 0.0261 1.0000 Uani Cl1 0.1991(4) 0.2035(4) 0.0259(3) 0.0457 1.0000 Uani Cl2 0.0799(3) -0.0763(4) -0.0231(3) 0.0424 1.0000 Uani Cl3 0.3585(3) 0.0957(4) 0.2439(3) 0.0438 1.0000 Uani N1 0.3536(9) -0.0715(11) 0.0220(8) 0.0323 1.0000 Uani N2 0.0903(8) -0.0109(16) 0.2139(7) 0.0196 1.0000 Uani N4 0.2139(9) -0.157(1) 0.1956(8) 0.0301 1.0000 Uani N6 -0.0561(9) -0.2370(11) 0.2727(9) 0.0362 1.0000 Uani N7 0.1021(9) -0.250(1) 0.4033(8) 0.0309 1.0000 Uani C3 0.1157(12) -0.1174(13) 0.2412(11) 0.0361 1.0000 Uani C5 0.0552(12) -0.2051(14) 0.3135(11) 0.0245 1.0000 Uani C11 0.4605(11) 0.006(3) 0.017(1) 0.0452 1.0000 Uani C12 0.5717(15) -0.0477(17) 0.0778(17) 0.0654 1.0000 Uani C13 0.3543(14) -0.1927(14) -0.0306(12) 0.0430 1.0000 Uani C14 0.3632(14) -0.1865(15) -0.1503(14) 0.0520 1.0000 Uani C21 -0.0030(11) 0.0824(13) 0.2484(11) 0.0381 1.0000 Uani C22 0.052(2) 0.2142(18) 0.2642(15) 0.0531 1.0000 Uani C23 -0.1055(16) 0.0866(19) 0.1575(15) 0.0668 1.0000 Uani C24 -0.0495(15) 0.0439(13) 0.3530(12) 0.0518 1.0000 Uani C41 0.2531(11) -0.2789(12) 0.1994(9) 0.0271 1.0000 Uani C42 0.1766(11) -0.3756(13) 0.157(1) 0.0344 1.0000 Uani C43 0.2149(11) -0.496(3) 0.1607(9) 0.0439 1.0000 Uani C44 0.3297(15) -0.5257(11) 0.2071(12) 0.0460 1.0000 Uani C45 0.4050(13) -0.4334(15) 0.2484(12) 0.0425 1.0000 Uani C46 0.3677(12) -0.3100(12) 0.2437(11) 0.0348 1.0000 Uani C61 -0.1370(13) -0.3245(14) 0.3224(11) 0.0421 1.0000 Uani C62 -0.2531(17) -0.330(2) 0.2483(15) 0.0776 1.0000 Uani C63 -0.1616(13) -0.2751(14) 0.4314(12) 0.0432 1.0000 Uani C64 -0.0827(16) -0.4544(14) 0.3325(13) 0.0543 1.0000 Uani C71 0.2187(12) -0.2180(15) 0.4477(11) 0.0419 1.0000 Uani C72 0.2864(12) -0.3144(15) 0.4984(11) 0.0429 1.0000 Uani C73 0.3974(14) -0.2930(18) 0.5493(12) 0.0541 1.0000 Uani C74 0.4481(13) -0.1758(18) 0.5531(11) 0.0482 1.0000 Uani C75 0.3816(15) -0.0785(17) 0.5054(13) 0.0544 1.0000 Uani C76 0.2676(12) -0.0970(13) 0.4535(9) 0.0350 1.0000 Uani H61 -0.0870 -0.1984 0.2032 0.0600 1.0000 Uiso H111 0.4746 0.0211 -0.0580 0.0600 1.0000 Uiso H112 0.4459 0.0914 0.0502 0.0600 1.0000 Uiso H121 0.6406 0.0077 0.0734 0.0600 1.0000 Uiso H122 0.5876 -0.1303 0.0461 0.0600 1.0000 Uiso H123 0.5589 -0.0600 0.1543 0.0600 1.0000 Uiso H131 0.4225 -0.2412 0.0034 0.0600 1.0000 Uiso H132 0.2788 -0.2364 -0.0192 0.0600 1.0000 Uiso H141 0.3625 -0.2717 -0.1801 0.0600 1.0000 Uiso H142 0.4379 -0.1435 -0.1630 0.0600 1.0000 Uiso H143 0.2942 -0.1387 -0.1856 0.0600 1.0000 Uiso H421 0.0936 -0.3560 0.1215 0.0600 1.0000 Uiso H431 0.1601 -0.5664 0.1311 0.0600 1.0000 Uiso H461 0.4242 -0.2435 0.2713 0.0600 1.0000 Uiso H451 0.4859 -0.4547 0.2814 0.0600 1.0000 Uiso H441 0.3577 -0.6135 0.2102 0.0600 1.0000 Uiso H641 -0.1376 -0.5112 0.3653 0.0600 1.0000 Uiso H642 -0.0057 -0.4505 0.3776 0.0600 1.0000 Uiso H643 -0.0704 -0.4856 0.2602 0.0600 1.0000 Uiso H621 -0.3104 -0.3863 0.2770 0.0600 1.0000 Uiso H622 -0.2885 -0.2441 0.2405 0.0600 1.0000 Uiso H623 -0.2371 -0.3591 0.1759 0.0600 1.0000 Uiso H631 -0.2156 -0.3330 0.4643 0.0600 1.0000 Uiso H632 -0.0862 -0.2668 0.4784 0.0600 1.0000 Uiso H633 -0.2007 -0.1918 0.4221 0.0600 1.0000 Uiso H761 0.2210 -0.0253 0.4212 0.0600 1.0000 Uiso H751 0.4156 0.0070 0.5080 0.0600 1.0000 Uiso H741 0.5296 -0.1611 0.5889 0.0600 1.0000 Uiso H731 0.4425 -0.3646 0.5848 0.0600 1.0000 Uiso H721 0.2526 -0.3999 0.4977 0.0600 1.0000 Uiso H221 -0.0082 0.2724 0.2866 0.0600 1.0000 Uiso H222 0.1206 0.2098 0.3212 0.0600 1.0000 Uiso H223 0.0802 0.2424 0.1968 0.0600 1.0000 Uiso H241 -0.1091 0.1056 0.3723 0.0600 1.0000 Uiso H242 0.0174 0.0400 0.4108 0.0600 1.0000 Uiso H243 -0.0877 -0.0395 0.3441 0.0600 1.0000 Uiso H231 -0.1673 0.1450 0.1760 0.0600 1.0000 Uiso H232 -0.1400 0.0015 0.1468 0.0600 1.0000 Uiso H233 -0.0741 0.1139 0.0906 0.0600 1.0000 Uiso 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 0.02780(19) 0.02474(19) 0.02580(19) 0.0136(4) 0.00332(13) 0.0015(5) Cl1 0.059(2) 0.0360(19) 0.0427(19) 0.0027(15) 0.0083(16) 0.0041(16) Cl2 0.0358(18) 0.055(2) 0.0354(17) -0.0074(16) -0.0011(13) -0.0060(16) Cl3 0.044(2) 0.0452(19) 0.0409(18) -0.0080(15) -0.0007(15) -0.0114(16) N1 0.026(5) 0.040(6) 0.033(6) -0.002(5) 0.009(4) 0.001(5) N2 0.027(4) 0.005(8) 0.027(4) -0.002(4) 0.004(3) -0.001(5) N4 0.033(6) 0.033(6) 0.025(5) 0.005(4) 0.006(4) 0.000(5) N6 0.030(6) 0.045(7) 0.033(6) 0.012(5) 0.001(4) -0.002(5) N7 0.032(6) 0.032(6) 0.028(5) 0.001(4) 0.002(4) 0.002(5) C3 0.037(7) 0.036(8) 0.033(7) -0.010(6) -0.004(5) -0.011(6) C5 0.019(6) 0.028(7) 0.027(7) -0.004(6) 0.005(6) -0.001(5) C11 0.050(7) 0.039(7) 0.050(7) 0.011(14) 0.021(5) 0.020(15) C12 0.038(9) 0.05(1) 0.104(15) -0.00(1) 0.010(9) -0.001(7) C13 0.050(9) 0.037(8) 0.042(8) -0.011(6) 0.006(6) 0.014(7) C14 0.053(9) 0.044(9) 0.06(1) -0.011(8) 0.020(8) -0.019(7) C21 0.029(7) 0.044(8) 0.042(7) 0.007(6) 0.007(6) 0.009(6) C22 0.080(14) 0.035(9) 0.050(11) -0.007(9) 0.033(11) 0.006(8) C23 0.05(1) 0.082(13) 0.061(11) -0.01(1) -0.002(8) 0.04(1) C24 0.07(1) 0.043(9) 0.051(8) -0.010(6) 0.030(8) 0.005(7) C41 0.033(6) 0.030(6) 0.019(5) -0.002(5) 0.008(5) -0.000(5) C42 0.027(6) 0.040(7) 0.036(7) -0.007(6) 0.005(5) 0.001(6) C43 0.045(7) 0.039(6) 0.048(6) -0.004(15) 0.007(5) 0.021(15) C44 0.059(9) 0.03(1) 0.055(8) 0.004(6) 0.018(7) 0.003(6) C45 0.036(8) 0.052(9) 0.041(8) 0.005(7) 0.006(6) 0.015(7) C46 0.036(7) 0.031(7) 0.039(7) -0.001(5) 0.010(5) -0.004(5) C61 0.046(8) 0.043(8) 0.039(7) 0.004(6) 0.012(6) -0.012(7) C62 0.053(11) 0.13(2) 0.054(11) -0.004(12) 0.018(9) -0.041(12) C63 0.047(8) 0.038(8) 0.046(8) 0.000(6) 0.013(6) -0.005(6) C64 0.06(1) 0.045(9) 0.055(9) -0.001(7) 0.015(8) -0.013(7) C71 0.032(7) 0.06(1) 0.034(7) -0.002(7) 0.003(6) 0.006(7) C72 0.037(7) 0.06(1) 0.032(7) 0.003(7) 0.006(6) 0.005(7) C73 0.049(9) 0.071(12) 0.041(8) 0.003(8) -0.000(7) 0.014(9) C74 0.036(8) 0.077(12) 0.031(7) -0.007(8) -0.005(6) 0.014(8) C75 0.05(1) 0.061(11) 0.048(9) -0.013(8) 0.002(7) -0.018(8) C76 0.038(7) 0.044(8) 0.022(6) -0.006(6) 0.002(5) 0.002(6) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ta1 . Cl1 . 2.367(4) yes Ta1 . Cl2 . 2.385(3) yes Ta1 . Cl3 . 2.345(3) yes Ta1 . N1 . 1.96(1) yes Ta1 . N2 . 2.249(8) yes Ta1 . N4 . 2.09(1) yes N1 . C11 . 1.47(3) yes N1 . C13 . 1.456(17) yes N2 . C3 . 1.22(2) yes N2 . C21 . 1.547(18) yes N4 . C3 . 1.367(17) yes N4 . C41 . 1.382(16) yes N6 . C5 . 1.349(17) yes N6 . C61 . 1.492(16) yes N6 . H61 . 0.99(1) no N7 . C5 . 1.285(16) yes N7 . C71 . 1.414(17) yes C3 . C5 . 1.519(19) yes C11 . C12 . 1.51(2) yes C11 . H111 . 0.991(12) no C11 . H112 . 1.02(3) no C12 . H121 . 0.985(17) no C12 . H122 . 0.994(18) no C12 . H123 . 1.00(2) no C13 . C14 . 1.52(2) yes C13 . H131 . 0.986(14) no C13 . H132 . 0.996(16) no C14 . H141 . 0.985(15) no C14 . H142 . 0.989(14) no C14 . H143 . 0.995(18) no C21 . C22 . 1.55(2) yes C21 . C23 . 1.53(2) yes C21 . C24 . 1.524(19) yes C22 . H221 . 0.984(19) no C22 . H222 . 1.00(2) no C22 . H223 . 0.984(17) no C23 . H231 . 0.984(16) no C23 . H232 . 0.99(2) no C23 . H233 . 0.99(2) no C24 . H241 . 0.992(14) no C24 . H242 . 0.988(18) no C24 . H243 . 0.992(15) no C41 . C42 . 1.416(17) yes C41 . C46 . 1.391(18) yes C42 . C43 . 1.36(3) yes C42 . H421 . 1.013(12) no C43 . C44 . 1.397(19) yes C43 . H431 . 1.02(3) no C44 . C45 . 1.368(19) yes C44 . H441 . 0.991(12) no C45 . C46 . 1.386(19) yes C45 . H451 . 0.987(14) no C46 . H461 . 0.993(13) no C61 . C62 . 1.52(2) yes C61 . C63 . 1.521(19) yes C61 . C64 . 1.52(2) yes C62 . H621 . 0.985(18) no C62 . H622 . 1.00(3) no C62 . H623 . 0.998(19) no C63 . H631 . 0.990(14) no C63 . H632 . 0.985(15) no C63 . H633 . 0.996(15) no C64 . H641 . 0.990(15) no C64 . H642 . 0.985(18) no C64 . H643 . 0.992(16) no C71 . C72 . 1.39(2) yes C71 . C76 . 1.41(2) yes C72 . C73 . 1.36(2) yes C72 . H721 . 0.992(16) no C73 . C74 . 1.38(2) yes C73 . H731 . 0.999(17) no C74 . C75 . 1.38(2) yes C74 . H741 . 0.991(14) no C75 . C76 . 1.39(2) yes C75 . H751 . 0.991(17) no C76 . H761 . 0.992(14) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ta1 . Cl2 . 88.42(14) yes Cl1 . Ta1 . Cl3 . 89.38(14) yes Cl2 . Ta1 . Cl3 . 170.11(13) yes Cl1 . Ta1 . N1 . 104.4(3) yes Cl2 . Ta1 . N1 . 89.8(3) yes Cl3 . Ta1 . N1 . 100.1(3) yes Cl1 . Ta1 . N2 . 102.6(4) yes Cl2 . Ta1 . N2 . 82.2(3) yes Cl3 . Ta1 . N2 . 88.9(3) yes N1 . Ta1 . N2 . 151.6(6) yes Cl1 . Ta1 . N4 . 160.9(3) yes Cl2 . Ta1 . N4 . 87.6(3) yes Cl3 . Ta1 . N4 . 91.3(3) yes N1 . Ta1 . N4 . 94.3(4) yes N2 . Ta1 . N4 . 58.4(5) yes Ta1 . N1 . C11 . 113.7(11) yes Ta1 . N1 . C13 . 130.0(9) yes C11 . N1 . C13 . 116.2(13) yes Ta1 . N2 . C3 . 94.2(9) yes Ta1 . N2 . C21 . 133.3(10) yes C3 . N2 . C21 . 132.3(12) yes Ta1 . N4 . C3 . 96.9(8) yes Ta1 . N4 . C41 . 137.9(8) yes C3 . N4 . C41 . 123.2(11) yes C5 . N6 . C61 . 126.0(11) yes C5 . N6 . H61 . 116.8(11) no C61 . N6 . H61 . 117.2(10) no C5 . N7 . C71 . 122.1(12) yes N2 . C3 . N4 . 110.3(12) yes N2 . C3 . C5 . 129.8(13) yes N4 . C3 . C5 . 119.9(12) yes N6 . C5 . N7 . 121.1(13) yes N6 . C5 . C3 . 113.0(12) yes N7 . C5 . C3 . 125.9(12) yes N1 . C11 . C12 . 113.8(20) yes N1 . C11 . H111 . 110.2(17) no C12 . C11 . H111 . 109.2(12) no N1 . C11 . H112 . 108.7(10) no C12 . C11 . H112 . 107.6(16) no H111 . C11 . H112 . 107.0(27) no C11 . C12 . H121 . 111.1(19) no C11 . C12 . H122 . 108.5(19) no H121 . C12 . H122 . 109.6(17) no C11 . C12 . H123 . 109.5(14) no H121 . C12 . H123 . 109.4(19) no H122 . C12 . H123 . 108.7(18) no N1 . C13 . C14 . 114.4(13) yes N1 . C13 . H131 . 108.4(13) no C14 . C13 . H131 . 108.6(13) no N1 . C13 . H132 . 107.8(12) no C14 . C13 . H132 . 108.2(13) no H131 . C13 . H132 . 109.3(15) no C13 . C14 . H141 . 109.7(15) no C13 . C14 . H142 . 109.2(15) no H141 . C14 . H142 . 109.9(15) no C13 . C14 . H143 . 109.3(13) no H141 . C14 . H143 . 109.5(16) no H142 . C14 . H143 . 109.2(15) no N2 . C21 . C22 . 110.5(12) yes N2 . C21 . C23 . 106.9(11) yes C22 . C21 . C23 . 109.1(14) yes N2 . C21 . C24 . 112.1(11) yes C22 . C21 . C24 . 107.9(13) yes C23 . C21 . C24 . 110.3(13) yes C21 . C22 . H221 . 109.6(18) no C21 . C22 . H222 . 108.5(16) no H221 . C22 . H222 . 109.3(17) no C21 . C22 . H223 . 109.5(16) no H221 . C22 . H223 . 110.5(19) no H222 . C22 . H223 . 109.3(20) no C21 . C23 . H231 . 109.9(16) no C21 . C23 . H232 . 109.0(16) no H231 . C23 . H232 . 109.7(19) no C21 . C23 . H233 . 109.3(16) no H231 . C23 . H233 . 109.9(18) no H232 . C23 . H233 . 109.1(17) no C21 . C24 . H241 . 109.7(14) no C21 . C24 . H242 . 109.6(13) no H241 . C24 . H242 . 109.5(14) no C21 . C24 . H243 . 109.4(13) no H241 . C24 . H243 . 109.2(15) no H242 . C24 . H243 . 109.5(15) no N4 . C41 . C42 . 120.0(11) yes N4 . C41 . C46 . 121.4(11) yes C42 . C41 . C46 . 118.6(12) yes C41 . C42 . C43 . 120.1(13) yes C41 . C42 . H421 . 120.7(12) no C43 . C42 . H421 . 119.2(14) no C42 . C43 . C44 . 120.3(21) yes C42 . C43 . H431 . 120.6(12) no C44 . C43 . H431 . 119.1(25) no C43 . C44 . C45 . 120.3(17) yes C43 . C44 . H441 . 120.4(19) no C45 . C44 . H441 . 119.2(15) no C44 . C45 . C46 . 120.0(12) yes C44 . C45 . H451 . 120.0(15) no C46 . C45 . H451 . 120.1(16) no C41 . C46 . C45 . 120.7(13) yes C41 . C46 . H461 . 120.1(13) no C45 . C46 . H461 . 119.3(14) no N6 . C61 . C62 . 106.9(12) yes N6 . C61 . C63 . 109.8(12) yes C62 . C61 . C63 . 109.4(13) yes N6 . C61 . C64 . 110.5(12) yes C62 . C61 . C64 . 109.3(15) yes C63 . C61 . C64 . 110.8(13) yes C61 . C62 . H621 . 110.7(18) no C61 . C62 . H622 . 109.6(18) no H621 . C62 . H622 . 109.2(19) no C61 . C62 . H623 . 109.8(17) no H621 . C62 . H623 . 109.2(20) no H622 . C62 . H623 . 108.2(20) no C61 . C63 . H631 . 109.8(13) no C61 . C63 . H632 . 109.8(13) no H631 . C63 . H632 . 109.8(14) no C61 . C63 . H633 . 109.2(13) no H631 . C63 . H633 . 109.0(13) no H632 . C63 . H633 . 109.4(14) no C61 . C64 . H641 . 109.3(15) no C61 . C64 . H642 . 109.3(13) no H641 . C64 . H642 . 109.9(16) no C61 . C64 . H643 . 109.1(14) no H641 . C64 . H643 . 109.4(15) no H642 . C64 . H643 . 109.7(16) no N7 . C71 . C72 . 116.1(14) yes N7 . C71 . C76 . 125.9(13) yes C72 . C71 . C76 . 117.7(13) yes C71 . C72 . C73 . 121.3(16) yes C71 . C72 . H721 . 119.2(14) no C73 . C72 . H721 . 119.5(15) no C72 . C73 . C74 . 121.8(16) yes C72 . C73 . H731 . 118.6(18) no C74 . C73 . H731 . 119.6(16) no C73 . C74 . C75 . 117.9(14) yes C73 . C74 . H741 . 121.4(16) no C75 . C74 . H741 . 120.7(18) no C74 . C75 . C76 . 121.7(16) yes C74 . C75 . H751 . 119.5(16) no C76 . C75 . H751 . 118.8(18) no C71 . C76 . C75 . 119.5(14) yes C71 . C76 . H761 . 120.2(12) no C75 . C76 . H761 . 120.2(15) no #=END data_Compound_7 _database_code_CSD 155034 _audit_creation_date 00-10-08 _audit_creation_method CRYSTALS_ver_12-03-99 #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Enraf-nonius DIP2000 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; DIP2000 software 'Xpress' (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct _atom_sites_solution_hydrogens mixed # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** _cell_length_a 11.623(1) _cell_angle_alpha 90 _cell_length_b 12.225(1) _cell_angle_beta 93.925(2) _cell_length_c 30.868(1) _cell_angle_gamma 90 _cell_volume 4375.8 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International_Tables_Vol_IV_Table_2.2B' 'Zr ' -2.9650 0.5600 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572 87.6627 2.0693 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C34 H65 Cl1 N6 Si4 Zr1 ' _chemical_formula_moiety ' C34 H65 Cl1 N6 Si4 Zr1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 796.95 _cell_measurement_reflns_used 15217 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' paleyellow ' _exptl_crystal_size_min 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.21 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1685.78 _exptl_absorpt_coefficient_mu 0.45 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.83 _diffrn_ambient_temperature 150 _diffrn_reflns_number 15217 _reflns_number_total 7155 _diffrn_reflns_av_R_equivalents 0.03 _diffrn_measured_fraction_theta_max 0.783 _reflns_number_gt 6779 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _refine_diff_density_min -0.65 _refine_diff_density_max 0.48 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 6779 _refine_ls_number_parameters 419 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.0378 _refine_ls_goodness_of_fit_ref 1.0439 _refine_ls_shift/su_max 0.001884 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979, 3.16 1.46 2.82 0.534 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Zr1 0.232170(16) 0.232001(15) 0.853433(6) 0.0154 1.0000 Uani Cl1 0.11725(5) 0.31365(4) 0.792841(16) 0.0281 1.0000 Uani Si1 0.51907(6) 0.21212(5) 0.84477(2) 0.0308 1.0000 Uani Si2 0.40323(6) 0.42371(5) 0.81862(2) 0.0326 1.0000 Uani Si3 0.21983(6) 0.38965(5) 0.945436(19) 0.0265 1.0000 Uani Si4 0.00193(5) 0.30857(5) 0.89933(2) 0.0237 1.0000 Uani N1 0.24306(14) 0.07665(13) 0.89167(5) 0.0165 1.0000 Uani N2 0.19361(15) 0.06602(14) 0.82120(5) 0.0182 1.0000 Uani N3 0.18929(17) -0.18102(14) 0.88451(6) 0.0252 1.0000 Uani N4 0.02495(15) -0.09226(14) 0.85777(6) 0.0194 1.0000 Uani N5 0.39147(16) 0.29108(15) 0.84128(6) 0.0238 1.0000 Uani N6 0.15358(16) 0.31359(14) 0.90247(5) 0.0202 1.0000 Uani C1 0.19625(16) 0.01447(15) 0.85875(6) 0.0160 1.0000 Uani C2 0.14045(17) -0.09666(16) 0.86765(6) 0.0177 1.0000 Uani C3 0.24396(18) 0.04846(16) 0.93611(6) 0.0186 1.0000 Uani C4 0.1487(2) 0.00710(18) 0.95571(7) 0.0239 1.0000 Uani C5 0.1566(2) -0.0194(2) 0.99952(8) 0.0313 1.0000 Uani C6 0.2585(2) -0.0028(2) 1.02479(7) 0.0338 1.0000 Uani C7 0.3523(2) 0.0403(2) 1.00583(8) 0.0347 1.0000 Uani C8 0.3451(2) 0.06641(19) 0.96157(7) 0.0267 1.0000 Uani C9 0.3087(2) -0.19351(18) 0.89465(9) 0.0307 1.0000 Uani C10 0.3455(3) -0.2215(2) 0.93698(11) 0.0485 1.0000 Uani C11 0.4627(4) -0.2462(3) 0.94679(14) 0.0662 1.0000 Uani C12 0.5411(3) -0.2433(3) 0.91511(15) 0.0604 1.0000 Uani C13 0.5043(3) -0.2170(3) 0.87385(14) 0.0559 1.0000 Uani C14 0.3891(2) -0.1923(2) 0.86335(11) 0.0418 1.0000 Uani C15 0.16535(19) 0.02220(17) 0.77636(6) 0.0229 1.0000 Uani C16 0.1910(2) -0.1000(2) 0.77184(7) 0.0329 1.0000 Uani C17 0.2437(2) 0.0837(2) 0.74674(7) 0.0291 1.0000 Uani C18 0.0394(2) 0.04394(19) 0.76164(7) 0.0256 1.0000 Uani C19 -0.0586(2) -0.18247(19) 0.86195(7) 0.0270 1.0000 Uani C20 -0.1748(2) -0.1353(3) 0.84538(11) 0.0455 1.0000 Uani C21 -0.0625(2) -0.2173(2) 0.90914(8) 0.0371 1.0000 Uani C22 -0.0277(2) -0.2788(2) 0.83350(8) 0.0360 1.0000 Uani C23 0.6029(3) 0.2258(3) 0.79546(12) 0.0535 1.0000 Uani C24 0.4907(2) 0.0631(2) 0.8488(1) 0.0362 1.0000 Uani C25 0.6150(2) 0.2487(3) 0.89422(11) 0.0481 1.0000 Uani C26 0.5427(3) 0.4926(2) 0.83715(11) 0.0496 1.0000 Uani C27 0.2882(3) 0.5196(2) 0.8346(1) 0.0415 1.0000 Uani C28 0.3956(3) 0.4147(3) 0.7580(1) 0.0515 1.0000 Uani C29 0.2031(3) 0.3250(2) 0.99975(8) 0.0411 1.0000 Uani C30 0.1580(3) 0.5305(2) 0.94719(9) 0.0404 1.0000 Uani C31 0.3787(3) 0.4001(3) 0.94208(9) 0.0442 1.0000 Uani C32 -0.0623(2) 0.3000(2) 0.95299(9) 0.0389 1.0000 Uani C33 -0.0487(2) 0.18094(19) 0.87016(8) 0.0310 1.0000 Uani C34 -0.0646(2) 0.4299(2) 0.87042(9) 0.0384 1.0000 Uani H4 0.001(2) -0.030(2) 0.8468(8) 0.014(6) 1.0000 Uiso H41 0.0741 -0.0036 0.9381 0.0287 1.0000 Uiso H51 0.0881 -0.0508 1.0130 0.0378 1.0000 Uiso H61 0.2637 -0.0220 1.0564 0.0403 1.0000 Uiso H71 0.4259 0.0530 1.0238 0.0410 1.0000 Uiso H81 0.4136 0.0983 0.9482 0.0318 1.0000 Uiso H101 0.2896 -0.2240 0.9602 0.0567 1.0000 Uiso H111 0.4897 -0.2662 0.9772 0.0766 1.0000 Uiso H121 0.6242 -0.2604 0.9226 0.0709 1.0000 Uiso H131 0.5605 -0.2153 0.8507 0.0663 1.0000 Uiso H141 0.3635 -0.1733 0.8327 0.0497 1.0000 Uiso H161 0.1703 -0.1238 0.7413 0.0397 1.0000 Uiso H162 0.1445 -0.1425 0.7921 0.0397 1.0000 Uiso H163 0.2750 -0.1135 0.7792 0.0397 1.0000 Uiso H171 0.2285 0.0576 0.7162 0.0353 1.0000 Uiso H172 0.3262 0.0697 0.7565 0.0353 1.0000 Uiso H173 0.2275 0.1639 0.7482 0.0353 1.0000 Uiso H181 0.0226 0.0140 0.7317 0.0306 1.0000 Uiso H182 -0.0117 0.0075 0.7821 0.0306 1.0000 Uiso H183 0.0246 0.1245 0.7615 0.0306 1.0000 Uiso H201 -0.2359 -0.1924 0.8473 0.0543 1.0000 Uiso H202 -0.1936 -0.0708 0.8635 0.0543 1.0000 Uiso H203 -0.1710 -0.1119 0.8145 0.0543 1.0000 Uiso H211 -0.1193 -0.2782 0.9112 0.0449 1.0000 Uiso H212 -0.0863 -0.1537 0.9268 0.0449 1.0000 Uiso H213 0.0157 -0.2429 0.9204 0.0449 1.0000 Uiso H221 -0.0846 -0.3392 0.8365 0.0429 1.0000 Uiso H222 0.0514 -0.3054 0.8428 0.0429 1.0000 Uiso H223 -0.0299 -0.2548 0.8025 0.0429 1.0000 Uiso H231 0.6740 0.1798 0.7990 0.0660 1.0000 Uiso H232 0.6251 0.3041 0.7917 0.0660 1.0000 Uiso H233 0.5543 0.2009 0.7693 0.0660 1.0000 Uiso H241 0.5656 0.0225 0.8507 0.0438 1.0000 Uiso H242 0.4487 0.0482 0.8754 0.0438 1.0000 Uiso H243 0.4426 0.0384 0.8225 0.0438 1.0000 Uiso H251 0.6862 0.2026 0.8952 0.0574 1.0000 Uiso H252 0.5729 0.2352 0.9209 0.0574 1.0000 Uiso H253 0.6368 0.3277 0.8929 0.0574 1.0000 Uiso H261 0.5457 0.5668 0.8237 0.0604 1.0000 Uiso H262 0.5477 0.4999 0.8695 0.0604 1.0000 Uiso H263 0.6089 0.4477 0.8282 0.0604 1.0000 Uiso H271 0.2993 0.5926 0.8210 0.0501 1.0000 Uiso H272 0.2931 0.5276 0.8670 0.0501 1.0000 Uiso H273 0.2109 0.4898 0.8246 0.0501 1.0000 Uiso H281 0.4023 0.4897 0.7455 0.0626 1.0000 Uiso H282 0.4602 0.3680 0.7488 0.0626 1.0000 Uiso H283 0.3202 0.3816 0.7474 0.0626 1.0000 Uiso H291 0.2422 0.3714 1.0230 0.0494 1.0000 Uiso H292 0.1193 0.3186 1.0048 0.0494 1.0000 Uiso H293 0.2389 0.2506 1.0004 0.0494 1.0000 Uiso H301 0.1972 0.5720 0.9719 0.0489 1.0000 Uiso H302 0.0735 0.5257 0.9513 0.0489 1.0000 Uiso H303 0.1701 0.5691 0.9193 0.0489 1.0000 Uiso H311 0.4125 0.4440 0.9671 0.0529 1.0000 Uiso H312 0.4132 0.3252 0.9430 0.0529 1.0000 Uiso H313 0.3956 0.4368 0.9143 0.0529 1.0000 Uiso H321 -0.1482 0.2975 0.9484 0.0476 1.0000 Uiso H322 -0.0389 0.3656 0.9708 0.0476 1.0000 Uiso H323 -0.0341 0.2323 0.9685 0.0476 1.0000 Uiso H331 -0.1349 0.1783 0.8684 0.0375 1.0000 Uiso H332 -0.0171 0.1155 0.8863 0.0375 1.0000 Uiso H333 -0.0212 0.1811 0.8402 0.0375 1.0000 Uiso H341 -0.1505 0.4236 0.8694 0.0461 1.0000 Uiso H342 -0.0398 0.4982 0.8862 0.0461 1.0000 Uiso H343 -0.0391 0.4326 0.8402 0.0461 1.0000 Uiso 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 Zr1 0.0186(1) 0.0142(1) 0.01385(9) 0.00053(7) 0.00430(6) -0.00212(7) Cl1 0.0387(3) 0.0240(3) 0.0210(2) 0.0039(2) -0.0030(2) 0.0034(2) Si1 0.0222(3) 0.0333(4) 0.0382(3) -0.0045(3) 0.0118(2) -0.0061(2) Si2 0.0439(4) 0.0254(3) 0.0300(3) 0.0037(2) 0.0136(3) -0.0130(3) Si3 0.0353(3) 0.0276(3) 0.0169(3) -0.0039(2) 0.0051(2) 0.0003(2) Si4 0.0260(3) 0.0198(3) 0.0261(3) -0.0009(2) 0.0085(2) 0.0034(2) N1 0.0185(9) 0.0161(8) 0.0151(7) -0.0006(6) 0.0027(6) -0.0006(6) N2 0.0195(9) 0.0186(9) 0.0167(8) -0.0000(6) 0.0024(6) 0.0004(6) N3 0.029(1) 0.0161(9) 0.0296(9) 0.0017(7) -0.0068(7) 0.0000(7) N4 0.0199(9) 0.0169(9) 0.0216(8) 0.0022(7) 0.0017(6) -0.0017(7) N5 0.025(1) 0.025(1) 0.0220(8) 0.0003(7) 0.0083(7) -0.0082(7) N6 0.0243(9) 0.0178(8) 0.0192(8) 0.0011(6) 0.0066(6) 0.0015(6) C1 0.0138(9) 0.015(1) 0.0201(9) -0.0010(7) 0.0037(7) 0.0014(7) C2 0.022(1) 0.016(1) 0.0147(8) -0.0023(7) -0.0018(7) -0.0017(7) C3 0.024(1) 0.015(1) 0.0170(9) -0.0012(7) 0.0020(7) 0.0006(7) C4 0.0281(11) 0.0246(11) 0.0189(9) 0.0003(8) 0.0023(8) -0.0018(8) C5 0.0392(14) 0.0321(13) 0.0231(11) 0.0061(9) 0.0058(9) -0.0021(9) C6 0.0492(15) 0.0362(13) 0.0152(9) 0.0028(8) -0.0031(9) 0.0071(11) C7 0.0342(13) 0.0414(14) 0.0269(11) -0.004(1) -0.0101(9) 0.003(1) C8 0.0254(11) 0.0305(12) 0.024(1) -0.0017(8) -0.0018(8) -0.0018(9) C9 0.0317(13) 0.014(1) 0.0441(13) -0.0023(9) -0.013(1) 0.0008(8) C10 0.0541(18) 0.0389(15) 0.0487(16) -0.0051(12) -0.0238(13) 0.0121(13) C11 0.071(3) 0.051(2) 0.069(2) -0.0062(15) -0.047(2) 0.0144(16) C12 0.0363(17) 0.0485(19) 0.093(3) -0.0153(17) -0.0246(17) 0.0128(13) C13 0.0285(15) 0.0430(17) 0.094(3) -0.0029(17) -0.0081(15) 0.0045(12) C14 0.0285(14) 0.0350(14) 0.0606(18) 0.0051(12) -0.0069(12) 0.002(1) C15 0.0296(12) 0.0250(11) 0.0146(9) -0.0029(7) 0.0057(8) -0.0012(8) C16 0.0517(15) 0.0274(12) 0.020(1) -0.0056(8) 0.008(1) 0.005(1) C17 0.0328(13) 0.0372(13) 0.0183(9) -0.0015(8) 0.0094(8) -0.0014(9) C18 0.0292(12) 0.0294(11) 0.0178(9) -0.0007(8) -0.0003(8) -0.0021(9) C19 0.0241(12) 0.0279(12) 0.0286(11) 0.0018(9) -0.0004(8) -0.0101(8) C20 0.0253(14) 0.0520(17) 0.0585(17) 0.0086(13) -0.0031(11) -0.0113(11) C21 0.0418(15) 0.0420(15) 0.0284(11) 0.002(1) 0.008(1) -0.0164(11) C22 0.0477(15) 0.0289(13) 0.0308(11) -0.004(1) -0.001(1) -0.0154(11) C23 0.0519(18) 0.0524(18) 0.0607(18) -0.0069(14) 0.0363(15) -0.0084(14) C24 0.0257(13) 0.0303(13) 0.0534(15) -0.0010(11) 0.008(1) 0.0027(9) C25 0.0275(14) 0.058(2) 0.0577(18) -0.0111(14) -0.0032(12) -0.0031(11) C26 0.0532(18) 0.0396(16) 0.0584(18) -0.0039(13) 0.0215(15) -0.0249(13) C27 0.0526(17) 0.0218(13) 0.0508(16) 0.0035(11) 0.0100(13) -0.005(1) C28 0.075(2) 0.0473(17) 0.0338(14) 0.0072(12) 0.0183(14) -0.0127(15) C29 0.0525(17) 0.0536(17) 0.017(1) 0.001(1) 0.004(1) 0.0065(13) C30 0.0600(18) 0.0293(13) 0.0329(13) -0.012(1) 0.0108(12) -0.0017(11) C31 0.0417(16) 0.0609(19) 0.0295(13) -0.0160(11) -0.0006(11) -0.0081(12) C32 0.0424(15) 0.0407(15) 0.0358(13) -0.005(1) 0.0189(11) -0.0061(11) C33 0.0266(12) 0.0252(12) 0.0420(13) -0.0022(9) 0.008(1) 0.0000(9) C34 0.0384(15) 0.0302(13) 0.0467(14) 0.0006(11) 0.0045(11) 0.015(1) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zr1 . Cl1 . 2.4366(5) yes Zr1 . N1 . 2.2351(16) yes Zr1 . N2 . 2.2907(17) yes Zr1 . N5 . 2.0459(18) yes Zr1 . N6 . 2.0760(17) yes Si1 . N5 . 1.767(2) yes Si1 . C23 . 1.870(3) yes Si1 . C24 . 1.857(3) yes Si1 . C25 . 1.881(3) yes Si2 . N5 . 1.7746(19) yes Si2 . C26 . 1.881(3) yes Si2 . C27 . 1.870(3) yes Si2 . C28 . 1.869(3) yes Si3 . N6 . 1.7540(19) yes Si3 . C29 . 1.876(3) yes Si3 . C30 . 1.868(3) yes Si3 . C31 . 1.861(3) yes Si4 . N6 . 1.7597(19) yes Si4 . C32 . 1.866(3) yes Si4 . C33 . 1.876(2) yes Si4 . C34 . 1.870(3) yes N1 . C1 . 1.353(3) yes N1 . C3 . 1.414(2) yes N2 . C1 . 1.318(3) yes N2 . C15 . 1.499(2) yes N3 . C2 . 1.271(3) yes N3 . C9 . 1.410(3) yes N4 . C2 . 1.357(3) yes N4 . C19 . 1.481(3) yes N4 . H4 . 0.87(3) no C1 . C2 . 1.538(3) yes C3 . C4 . 1.392(3) yes C3 . C8 . 1.386(3) yes C4 . C5 . 1.388(3) yes C4 . H41 . 1.000(2) no C5 . C6 . 1.387(4) yes C5 . H51 . 1.000(2) no C6 . C7 . 1.377(4) yes C6 . H61 . 1.000(2) no C7 . C8 . 1.400(3) yes C7 . H71 . 1.000(2) no C8 . H81 . 1.000(2) no C9 . C10 . 1.390(4) yes C9 . C14 . 1.389(4) yes C10 . C11 . 1.407(5) yes C10 . H101 . 1.000(4) no C11 . C12 . 1.382(6) yes C11 . H111 . 1.000(4) no C12 . C13 . 1.354(6) yes C12 . H121 . 1.000(3) no C13 . C14 . 1.389(4) yes C13 . H131 . 1.000(4) no C14 . H141 . 1.000(3) no C15 . C16 . 1.532(3) yes C15 . C17 . 1.530(3) yes C15 . C18 . 1.527(3) yes C16 . H161 . 1.000(2) no C16 . H162 . 1.000(2) no C16 . H163 . 1.000(3) no C17 . H171 . 1.000(2) no C17 . H172 . 1.000(2) no C17 . H173 . 1.000(2) no C18 . H181 . 1.000(2) no C18 . H182 . 1.000(2) no C18 . H183 . 1.000(2) no C19 . C20 . 1.524(4) yes C19 . C21 . 1.521(3) yes C19 . C22 . 1.526(4) yes C20 . H201 . 1.000(3) no C20 . H202 . 1.000(3) no C20 . H203 . 1.000(3) no C21 . H211 . 1.000(2) no C21 . H212 . 1.000(3) no C21 . H213 . 1.000(3) no C22 . H221 . 1.000(2) no C22 . H222 . 1.000(3) no C22 . H223 . 1.000(3) no C23 . H231 . 1.000(4) no C23 . H232 . 1.000(3) no C23 . H233 . 1.000(4) no C24 . H241 . 1.000(2) no C24 . H242 . 1.000(3) no C24 . H243 . 1.000(3) no C25 . H251 . 1.000(3) no C25 . H252 . 1.000(3) no C25 . H253 . 1.000(3) no C26 . H261 . 1.000(3) no C26 . H262 . 1.000(3) no C26 . H263 . 1.000(3) no C27 . H271 . 1.000(3) no C27 . H272 . 1.000(3) no C27 . H273 . 1.000(3) no C28 . H281 . 1.000(3) no C28 . H282 . 1.000(4) no C28 . H283 . 1.000(4) no C29 . H291 . 1.000(3) no C29 . H292 . 1.000(3) no C29 . H293 . 1.000(3) no C30 . H301 . 1.000(3) no C30 . H302 . 1.000(3) no C30 . H303 . 1.000(3) no C31 . H311 . 1.000(3) no C31 . H312 . 1.000(3) no C31 . H313 . 1.000(3) no C32 . H321 . 1.000(3) no C32 . H322 . 1.000(3) no C32 . H323 . 1.000(3) no C33 . H331 . 1.000(2) no C33 . H332 . 1.000(2) no C33 . H333 . 1.000(3) no C34 . H341 . 1.000(3) no C34 . H342 . 1.000(3) no C34 . H343 . 1.000(3) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Zr1 . N1 . 139.62(5) yes Cl1 . Zr1 . N2 . 87.06(4) yes N1 . Zr1 . N2 . 58.60(6) yes Cl1 . Zr1 . N5 . 99.79(5) yes N1 . Zr1 . N5 . 112.19(7) yes N2 . Zr1 . N5 . 112.69(7) yes Cl1 . Zr1 . N6 . 96.74(5) yes N1 . Zr1 . N6 . 92.00(6) yes N2 . Zr1 . N6 . 131.26(6) yes N5 . Zr1 . N6 . 114.39(7) yes N5 . Si1 . C23 . 112.53(14) yes N5 . Si1 . C24 . 112.8(1) yes C23 . Si1 . C24 . 104.33(14) yes N5 . Si1 . C25 . 111.60(11) yes C23 . Si1 . C25 . 109.05(16) yes C24 . Si1 . C25 . 106.04(14) yes N5 . Si2 . C26 . 112.16(13) yes N5 . Si2 . C27 . 113.13(11) yes C26 . Si2 . C27 . 104.82(14) yes N5 . Si2 . C28 . 109.92(11) yes C26 . Si2 . C28 . 108.16(14) yes C27 . Si2 . C28 . 108.40(15) yes N6 . Si3 . C29 . 112.67(11) yes N6 . Si3 . C30 . 111.13(11) yes C29 . Si3 . C30 . 107.39(12) yes N6 . Si3 . C31 . 112.4(1) yes C29 . Si3 . C31 . 104.05(13) yes C30 . Si3 . C31 . 108.88(14) yes N6 . Si4 . C32 . 114.39(11) yes N6 . Si4 . C33 . 109.6(1) yes C32 . Si4 . C33 . 104.35(11) yes N6 . Si4 . C34 . 112.24(11) yes C32 . Si4 . C34 . 106.91(13) yes C33 . Si4 . C34 . 108.92(12) yes Zr1 . N1 . C1 . 94.32(12) yes Zr1 . N1 . C3 . 135.72(13) yes C1 . N1 . C3 . 124.59(17) yes Zr1 . N2 . C1 . 92.83(12) yes Zr1 . N2 . C15 . 137.85(13) yes C1 . N2 . C15 . 129.17(17) yes C2 . N3 . C9 . 125.72(19) yes C2 . N4 . C19 . 126.55(18) yes C2 . N4 . H4 . 113.9(16) no C19 . N4 . H4 . 119.4(16) no Zr1 . N5 . Si1 . 124.2(1) yes Zr1 . N5 . Si2 . 119.3(1) yes Si1 . N5 . Si2 . 115.9(1) yes Zr1 . N6 . Si3 . 127.9(1) yes Zr1 . N6 . Si4 . 115.60(9) yes Si3 . N6 . Si4 . 116.5(1) yes N1 . C1 . N2 . 112.09(17) yes N1 . C1 . C2 . 120.98(17) yes N2 . C1 . C2 . 126.49(17) yes N3 . C2 . N4 . 122.09(19) yes N3 . C2 . C1 . 127.42(19) yes N4 . C2 . C1 . 110.33(16) yes N1 . C3 . C4 . 123.84(18) yes N1 . C3 . C8 . 117.47(18) yes C4 . C3 . C8 . 118.66(19) yes C3 . C4 . C5 . 120.5(2) yes C3 . C4 . H41 . 119.8(2) no C5 . C4 . H41 . 119.8(2) no C4 . C5 . C6 . 120.7(2) yes C4 . C5 . H51 . 119.7(2) no C6 . C5 . H51 . 119.7(2) no C5 . C6 . C7 . 119.2(2) yes C5 . C6 . H61 . 120.4(3) no C7 . C6 . H61 . 120.4(2) no C6 . C7 . C8 . 120.4(2) yes C6 . C7 . H71 . 119.8(2) no C8 . C7 . H71 . 119.8(3) no C3 . C8 . C7 . 120.6(2) yes C3 . C8 . H81 . 119.7(2) no C7 . C8 . H81 . 119.7(2) no N3 . C9 . C10 . 118.1(3) yes N3 . C9 . C14 . 122.9(2) yes C10 . C9 . C14 . 118.5(3) yes C9 . C10 . C11 . 119.1(4) yes C9 . C10 . H101 . 120.4(3) no C11 . C10 . H101 . 120.4(3) no C10 . C11 . C12 . 121.2(3) yes C10 . C11 . H111 . 119.4(5) no C12 . C11 . H111 . 119.4(4) no C11 . C12 . C13 . 119.4(3) yes C11 . C12 . H121 . 120.3(4) no C13 . C12 . H121 . 120.3(5) no C12 . C13 . C14 . 120.6(4) yes C12 . C13 . H131 . 119.7(3) no C14 . C13 . H131 . 119.7(4) no C9 . C14 . C13 . 121.3(3) yes C9 . C14 . H141 . 119.4(2) no C13 . C14 . H141 . 119.4(3) no N2 . C15 . C16 . 113.62(17) yes N2 . C15 . C17 . 105.93(17) yes C16 . C15 . C17 . 107.27(18) yes N2 . C15 . C18 . 110.96(17) yes C16 . C15 . C18 . 109.36(19) yes C17 . C15 . C18 . 109.53(18) yes C15 . C16 . H161 . 109.5(2) no C15 . C16 . H162 . 109.5(2) no H161 . C16 . H162 . 109.5(2) no C15 . C16 . H163 . 109.5(2) no H161 . C16 . H163 . 109.5(2) no H162 . C16 . H163 . 109.5(2) no C15 . C17 . H171 . 109.5(2) no C15 . C17 . H172 . 109.5(2) no H171 . C17 . H172 . 109.5(2) no C15 . C17 . H173 . 109.47(19) no H171 . C17 . H173 . 109.5(2) no H172 . C17 . H173 . 109.5(2) no C15 . C18 . H181 . 109.47(19) no C15 . C18 . H182 . 109.47(18) no H181 . C18 . H182 . 109.5(2) no C15 . C18 . H183 . 109.47(19) no H181 . C18 . H183 . 109.5(2) no H182 . C18 . H183 . 109.5(2) no N4 . C19 . C20 . 105.11(19) yes N4 . C19 . C21 . 110.75(18) yes C20 . C19 . C21 . 110.1(2) yes N4 . C19 . C22 . 110.03(19) yes C20 . C19 . C22 . 109.7(2) yes C21 . C19 . C22 . 111.0(2) yes C19 . C20 . H201 . 109.5(3) no C19 . C20 . H202 . 109.5(2) no H201 . C20 . H202 . 109.5(3) no C19 . C20 . H203 . 109.5(3) no H201 . C20 . H203 . 109.5(3) no H202 . C20 . H203 . 109.5(3) no C19 . C21 . H211 . 109.5(2) no C19 . C21 . H212 . 109.5(2) no H211 . C21 . H212 . 109.5(2) no C19 . C21 . H213 . 109.5(2) no H211 . C21 . H213 . 109.5(3) no H212 . C21 . H213 . 109.5(2) no C19 . C22 . H221 . 109.5(2) no C19 . C22 . H222 . 109.5(2) no H221 . C22 . H222 . 109.5(3) no C19 . C22 . H223 . 109.5(2) no H221 . C22 . H223 . 109.5(2) no H222 . C22 . H223 . 109.5(3) no Si1 . C23 . H231 . 109.5(3) no Si1 . C23 . H232 . 109.5(2) no H231 . C23 . H232 . 109.5(3) no Si1 . C23 . H233 . 109.5(2) no H231 . C23 . H233 . 109.5(3) no H232 . C23 . H233 . 109.5(4) no Si1 . C24 . H241 . 109.47(19) no Si1 . C24 . H242 . 109.47(19) no H241 . C24 . H242 . 109.5(3) no Si1 . C24 . H243 . 109.5(2) no H241 . C24 . H243 . 109.5(2) no H242 . C24 . H243 . 109.5(2) no Si1 . C25 . H251 . 109.5(2) no Si1 . C25 . H252 . 109.5(2) no H251 . C25 . H252 . 109.5(3) no Si1 . C25 . H253 . 109.5(2) no H251 . C25 . H253 . 109.5(3) no H252 . C25 . H253 . 109.5(3) no Si2 . C26 . H261 . 109.5(3) no Si2 . C26 . H262 . 109.5(2) no H261 . C26 . H262 . 109.5(3) no Si2 . C26 . H263 . 109.5(2) no H261 . C26 . H263 . 109.5(3) no H262 . C26 . H263 . 109.5(4) no Si2 . C27 . H271 . 109.5(2) no Si2 . C27 . H272 . 109.5(2) no H271 . C27 . H272 . 109.5(2) no Si2 . C27 . H273 . 109.5(2) no H271 . C27 . H273 . 109.5(3) no H272 . C27 . H273 . 109.5(3) no Si2 . C28 . H281 . 109.5(2) no Si2 . C28 . H282 . 109.5(3) no H281 . C28 . H282 . 109.5(3) no Si2 . C28 . H283 . 109.5(2) no H281 . C28 . H283 . 109.5(3) no H282 . C28 . H283 . 109.5(3) no Si3 . C29 . H291 . 109.5(2) no Si3 . C29 . H292 . 109.47(19) no H291 . C29 . H292 . 109.5(2) no Si3 . C29 . H293 . 109.47(18) no H291 . C29 . H293 . 109.5(3) no H292 . C29 . H293 . 109.5(3) no Si3 . C30 . H301 . 109.5(2) no Si3 . C30 . H302 . 109.5(2) no H301 . C30 . H302 . 109.5(2) no Si3 . C30 . H303 . 109.47(19) no H301 . C30 . H303 . 109.5(3) no H302 . C30 . H303 . 109.5(3) no Si3 . C31 . H311 . 109.5(2) no Si3 . C31 . H312 . 109.5(2) no H311 . C31 . H312 . 109.5(3) no Si3 . C31 . H313 . 109.5(2) no H311 . C31 . H313 . 109.5(3) no H312 . C31 . H313 . 109.5(3) no Si4 . C32 . H321 . 109.5(2) no Si4 . C32 . H322 . 109.47(19) no H321 . C32 . H322 . 109.5(3) no Si4 . C32 . H323 . 109.47(19) no H321 . C32 . H323 . 109.5(2) no H322 . C32 . H323 . 109.5(3) no Si4 . C33 . H331 . 109.47(17) no Si4 . C33 . H332 . 109.47(19) no H331 . C33 . H332 . 109.5(2) no Si4 . C33 . H333 . 109.47(17) no H331 . C33 . H333 . 109.5(2) no H332 . C33 . H333 . 109.5(2) no Si4 . C34 . H341 . 109.5(2) no Si4 . C34 . H342 . 109.5(2) no H341 . C34 . H342 . 109.5(2) no Si4 . C34 . H343 . 109.47(18) no H341 . C34 . H343 . 109.5(3) no H342 . C34 . H343 . 109.5(3) no