# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Anjana Devi' 'Davide Barreca' 'Hans-Werner Becker' 'Roland A Fischer' 'Alberto Gasparotto' 'Andrian P Milanov' 'Ramasamy Pothiraja' 'Manuela Winter' _publ_contact_author_name 'Anjana Devi' _publ_contact_author_email ANJANA.DEVI@RUB.DE _publ_section_title ; Hafnium carbamates and ureates: New class of monomeric and volatile precursors for low temperature growth of HfO2 thin films ; # Attachment 'Pothiraja-Chem.Comm.cif' data_cvd271 _database_code_depnum_ccdc_archive 'CCDC 711072' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H56 Hf N4 O8' _chemical_formula_weight 755.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.7586(2) _cell_length_b 18.7004(2) _cell_length_c 20.4731(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7181.83(13) _cell_formula_units_Z 8 _cell_measurement_temperature 111(2) _cell_measurement_reflns_used 3834 _cell_measurement_theta_min 2.618 _cell_measurement_theta_max 27.499 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 2.951 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.3775 _exptl_absorpt_correction_T_max 0.5257 _exptl_absorpt_process_details 'Gaussian face-indexed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 111(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '887 images at 1.0 deg. in \w and 15 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 89956 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6318 _reflns_number_gt 4552 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 171.32.24, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 171.32.24, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 171.32.24, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^ > 2sigma(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^)+(0.0132P)^2^+26.0034P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6318 _refine_ls_number_parameters 386 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 1.301 _refine_ls_restrained_S_all 1.301 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Hf1 Hf 0.155356(9) 0.398606(10) 0.171593(9) 0.01321(6) Uani 1 1 d . . . O11 O 0.07556(17) 0.32689(17) 0.12699(15) 0.0186(7) Uani 1 1 d . . . C12 C 0.1121(3) 0.3186(3) 0.0750(2) 0.0186(11) Uani 1 1 d . . . O12 O 0.08624(17) 0.28256(18) 0.02366(16) 0.0234(8) Uani 1 1 d . . . C121 C 0.0145(2) 0.2522(3) 0.0299(2) 0.0245(12) Uani 1 1 d . . . H121 H -0.0156 0.2846 0.0572 0.029 Uiso 1 1 calc R . . C122 C -0.0151(3) 0.2493(4) -0.0385(3) 0.0391(15) Uani 1 1 d . . . H12A H -0.0163 0.2976 -0.0569 0.059 Uiso 1 1 calc R . . H12B H -0.0635 0.2296 -0.0373 0.059 Uiso 1 1 calc R . . H12C H 0.0153 0.2187 -0.0656 0.059 Uiso 1 1 calc R . . C123 C 0.0194(3) 0.1801(3) 0.0620(3) 0.0366(14) Uani 1 1 d . . . H12D H 0.0520 0.1496 0.0370 0.055 Uiso 1 1 calc R . . H12E H -0.0279 0.1581 0.0632 0.055 Uiso 1 1 calc R . . H12F H 0.0375 0.1857 0.1066 0.055 Uiso 1 1 calc R . . N13 N 0.1751(2) 0.3473(2) 0.07375(19) 0.0175(9) Uani 1 1 d . . . C13 C 0.2185(3) 0.3468(3) 0.0145(2) 0.0220(11) Uani 1 1 d . . . H13 H 0.2150 0.2984 -0.0059 0.026 Uiso 1 1 calc R . . C131 C 0.2958(3) 0.3605(3) 0.0321(3) 0.0295(13) Uani 1 1 d . . . H13A H 0.3001 0.4074 0.0530 0.044 Uiso 1 1 calc R . . H13B H 0.3249 0.3593 -0.0075 0.044 Uiso 1 1 calc R . . H13C H 0.3122 0.3234 0.0624 0.044 Uiso 1 1 calc R . . C132 C 0.1923(3) 0.4020(3) -0.0345(2) 0.0301(12) Uani 1 1 d . . . H13D H 0.1419 0.3933 -0.0442 0.045 Uiso 1 1 calc R . . H13E H 0.2203 0.3982 -0.0748 0.045 Uiso 1 1 calc R . . H13F H 0.1980 0.4500 -0.0161 0.045 Uiso 1 1 calc R . . O21 O 0.26870(16) 0.37474(17) 0.19234(16) 0.0192(8) Uani 1 1 d . . . C22 C 0.2525(2) 0.3210(3) 0.2278(2) 0.0178(10) Uani 1 1 d . . . O22 O 0.30071(16) 0.28652(18) 0.26375(17) 0.0232(8) Uani 1 1 d . . . C221 C 0.3755(2) 0.3081(3) 0.2591(2) 0.0208(11) Uani 1 1 d . . . H221 H 0.3782 0.3611 0.2531 0.025 Uiso 1 1 calc R . . C222 C 0.4080(3) 0.2716(3) 0.2010(3) 0.0286(13) Uani 1 1 d . . . H22A H 0.4030 0.2197 0.2057 0.043 Uiso 1 1 calc R . . H22B H 0.4587 0.2840 0.1981 0.043 Uiso 1 1 calc R . . H22C H 0.3835 0.2872 0.1612 0.043 Uiso 1 1 calc R . . C223 C 0.4082(3) 0.2884(3) 0.3237(3) 0.0281(12) Uani 1 1 d . . . H22D H 0.3809 0.3107 0.3591 0.042 Uiso 1 1 calc R . . H22E H 0.4575 0.3054 0.3251 0.042 Uiso 1 1 calc R . . H22F H 0.4073 0.2364 0.3289 0.042 Uiso 1 1 calc R . . N23 N 0.1856(2) 0.3019(2) 0.22915(19) 0.0175(9) Uani 1 1 d . . . C23 C 0.1616(3) 0.2431(3) 0.2716(2) 0.0214(11) Uani 1 1 d . . . H23 H 0.2014 0.2079 0.2757 0.026 Uiso 1 1 calc R . . C231 C 0.0990(3) 0.2056(3) 0.2408(3) 0.0302(13) Uani 1 1 d . . . H23A H 0.0603 0.2400 0.2337 0.045 Uiso 1 1 calc R . . H23B H 0.0823 0.1674 0.2699 0.045 Uiso 1 1 calc R . . H23C H 0.1135 0.1850 0.1989 0.045 Uiso 1 1 calc R . . C232 C 0.1443(3) 0.2712(3) 0.3396(2) 0.0366(14) Uani 1 1 d . . . H23D H 0.1855 0.2974 0.3567 0.055 Uiso 1 1 calc R . . H23E H 0.1333 0.2309 0.3685 0.055 Uiso 1 1 calc R . . H23F H 0.1031 0.3032 0.3372 0.055 Uiso 1 1 calc R . . O31 O 0.06237(16) 0.40203(18) 0.24002(15) 0.0179(7) Uani 1 1 d . . . C32 C 0.0935(3) 0.4477(3) 0.2770(2) 0.0194(11) Uani 1 1 d . . . O32 O 0.06193(17) 0.47488(17) 0.32995(17) 0.0229(7) Uani 1 1 d . . . C321 C -0.0085(3) 0.4486(3) 0.3489(3) 0.0251(12) Uani 1 1 d . . . H321 H -0.0127 0.3968 0.3376 0.030 Uiso 1 1 calc R . . C322 C -0.0652(3) 0.4898(3) 0.3144(3) 0.0397(15) Uani 1 1 d . . . H32A H -0.0601 0.5408 0.3245 0.060 Uiso 1 1 calc R . . H32B H -0.1122 0.4731 0.3289 0.060 Uiso 1 1 calc R . . H32C H -0.0607 0.4826 0.2672 0.060 Uiso 1 1 calc R . . C323 C -0.0113(3) 0.4575(4) 0.4218(3) 0.0406(16) Uani 1 1 d . . . H32D H 0.0278 0.4305 0.4419 0.061 Uiso 1 1 calc R . . H32E H -0.0570 0.4396 0.4383 0.061 Uiso 1 1 calc R . . H32F H -0.0065 0.5083 0.4329 0.061 Uiso 1 1 calc R . . N33 N 0.1584(2) 0.4662(2) 0.26151(18) 0.0168(8) Uani 1 1 d . . . C33 C 0.1972(3) 0.5203(3) 0.3003(3) 0.0234(11) Uani 1 1 d . . . H33 H 0.1885 0.5109 0.3477 0.028 Uiso 1 1 calc R . . C331 C 0.1702(3) 0.5947(3) 0.2838(3) 0.0345(13) Uani 1 1 d . . . H33A H 0.1807 0.6054 0.2380 0.052 Uiso 1 1 calc R . . H33B H 0.1939 0.6298 0.3119 0.052 Uiso 1 1 calc R . . H33C H 0.1186 0.5968 0.2910 0.052 Uiso 1 1 calc R . . C332 C 0.2766(3) 0.5133(3) 0.2868(3) 0.0359(15) Uani 1 1 d . . . H33D H 0.2931 0.4660 0.3008 0.054 Uiso 1 1 calc R . . H33E H 0.3025 0.5504 0.3109 0.054 Uiso 1 1 calc R . . H33F H 0.2853 0.5191 0.2399 0.054 Uiso 1 1 calc R . . O41 O 0.21495(17) 0.48805(17) 0.12584(16) 0.0197(7) Uani 1 1 d . . . C42 C 0.1581(3) 0.5176(2) 0.1048(2) 0.0191(10) Uani 1 1 d . . . O42 O 0.16027(19) 0.57705(18) 0.06815(17) 0.0259(8) Uani 1 1 d . . . C421 C 0.2299(3) 0.6048(3) 0.0496(3) 0.0309(12) Uani 1 1 d . . . H421 H 0.2644 0.5642 0.0453 0.037 Uiso 1 1 calc R . . C422 C 0.2557(4) 0.6557(4) 0.1011(3) 0.0471(16) Uani 1 1 d . . . H42A H 0.2205 0.6939 0.1071 0.071 Uiso 1 1 calc R . . H42B H 0.3013 0.6766 0.0875 0.071 Uiso 1 1 calc R . . H42C H 0.2622 0.6299 0.1424 0.071 Uiso 1 1 calc R . . C423 C 0.2191(4) 0.6395(4) -0.0166(3) 0.0500(18) Uani 1 1 d . . . H42D H 0.2009 0.6039 -0.0475 0.075 Uiso 1 1 calc R . . H42E H 0.2647 0.6583 -0.0325 0.075 Uiso 1 1 calc R . . H42F H 0.1847 0.6787 -0.0125 0.075 Uiso 1 1 calc R . . C43 C 0.0290(3) 0.5182(3) 0.0994(2) 0.0227(11) Uani 1 1 d . . . H43 H 0.0347 0.5396 0.0550 0.027 Uiso 1 1 calc R . . N43 N 0.0976(2) 0.4866(2) 0.11961(19) 0.0170(9) Uani 1 1 d . . . C431 C 0.0082(3) 0.5771(3) 0.1471(3) 0.0310(13) Uani 1 1 d . . . H43A H 0.0039 0.5570 0.1911 0.047 Uiso 1 1 calc R . . H43B H -0.0376 0.5978 0.1339 0.047 Uiso 1 1 calc R . . H43C H 0.0449 0.6144 0.1470 0.047 Uiso 1 1 calc R . . C432 C -0.0274(3) 0.4607(3) 0.0964(3) 0.0312(13) Uani 1 1 d . . . H43D H -0.0133 0.4243 0.0645 0.047 Uiso 1 1 calc R . . H43E H -0.0729 0.4819 0.0833 0.047 Uiso 1 1 calc R . . H43F H -0.0325 0.4386 0.1396 0.047 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 Hf1 0.01205(9) 0.01366(9) 0.01391(9) 0.00019(9) -0.00020(8) -0.00003(8) O11 0.0182(17) 0.0206(18) 0.0171(18) -0.0018(14) 0.0005(14) -0.0027(14) C12 0.020(3) 0.020(3) 0.016(3) 0.003(2) 0.000(2) 0.005(2) O12 0.0200(18) 0.032(2) 0.0185(18) -0.0080(16) 0.0008(15) -0.0063(15) C121 0.017(2) 0.032(3) 0.025(3) -0.004(2) 0.000(2) -0.007(2) C122 0.034(3) 0.056(4) 0.028(3) 0.002(3) -0.006(3) -0.018(3) C123 0.041(4) 0.033(3) 0.036(3) -0.005(3) -0.005(3) -0.010(3) N13 0.016(2) 0.021(2) 0.016(2) -0.0001(17) -0.0002(16) -0.0017(17) C13 0.021(3) 0.026(3) 0.019(3) -0.002(2) 0.003(2) -0.001(2) C131 0.020(3) 0.041(3) 0.028(3) 0.003(3) 0.008(2) 0.003(2) C132 0.030(3) 0.038(3) 0.022(3) 0.006(3) 0.006(2) -0.001(3) O21 0.0156(17) 0.0201(18) 0.0218(18) 0.0011(14) -0.0011(14) -0.0006(14) C22 0.016(2) 0.020(3) 0.017(2) -0.003(2) 0.003(2) 0.003(2) O22 0.0143(17) 0.027(2) 0.028(2) 0.0074(16) -0.0048(15) 0.0014(15) C221 0.013(2) 0.024(3) 0.026(3) 0.001(2) -0.001(2) -0.004(2) C222 0.023(3) 0.035(3) 0.028(3) -0.003(3) 0.001(2) 0.001(2) C223 0.019(3) 0.036(3) 0.029(3) 0.000(3) -0.008(2) -0.001(2) N23 0.0151(19) 0.019(2) 0.019(2) 0.0026(18) 0.0009(17) -0.0015(17) C23 0.018(2) 0.024(3) 0.022(3) 0.008(2) 0.000(2) -0.001(2) C231 0.027(3) 0.031(3) 0.033(3) 0.011(3) -0.003(2) -0.008(3) C232 0.045(4) 0.041(3) 0.024(3) 0.007(3) 0.004(3) -0.008(3) O31 0.0164(16) 0.0193(17) 0.0180(16) -0.0036(15) 0.0013(13) -0.0021(15) C32 0.020(3) 0.021(3) 0.017(2) 0.000(2) -0.002(2) 0.002(2) O32 0.0229(17) 0.0252(18) 0.0206(17) -0.0073(16) 0.0056(16) -0.0048(14) C321 0.021(3) 0.021(3) 0.033(3) -0.008(2) 0.009(2) -0.001(2) C322 0.027(3) 0.053(4) 0.039(4) 0.003(3) 0.002(3) 0.000(3) C323 0.039(4) 0.053(4) 0.030(3) 0.009(3) 0.007(3) -0.007(3) N33 0.016(2) 0.018(2) 0.017(2) -0.0014(16) -0.0001(18) -0.0015(18) C33 0.020(3) 0.028(3) 0.022(3) -0.007(2) 0.001(2) -0.005(2) C331 0.034(3) 0.024(3) 0.045(3) -0.005(3) 0.002(3) -0.005(3) C332 0.023(3) 0.046(4) 0.039(3) -0.018(3) -0.005(3) -0.010(3) O41 0.0169(17) 0.0187(18) 0.0235(19) 0.0025(15) -0.0006(15) -0.0012(14) C42 0.026(3) 0.016(2) 0.015(2) -0.0008(19) 0.002(2) 0.000(2) O42 0.0261(19) 0.0226(18) 0.0289(19) 0.0106(15) -0.0006(17) -0.0018(16) C421 0.031(3) 0.028(3) 0.034(3) 0.008(3) 0.005(2) -0.005(3) C422 0.047(4) 0.049(4) 0.045(4) 0.007(3) 0.000(3) -0.022(3) C423 0.064(4) 0.049(4) 0.037(4) 0.020(3) -0.001(3) -0.021(4) C43 0.023(3) 0.023(3) 0.023(3) 0.002(2) -0.004(2) 0.004(2) N43 0.017(2) 0.017(2) 0.017(2) 0.0016(17) -0.0034(17) 0.0034(17) C431 0.031(3) 0.028(3) 0.034(3) -0.003(2) -0.003(3) 0.009(2) C432 0.024(3) 0.028(3) 0.042(3) 0.004(3) -0.012(3) 0.002(2) _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 Hf1 O11 2.208(3) . ? Hf1 O21 2.214(3) . ? Hf1 O41 2.219(3) . ? Hf1 N23 2.231(4) . ? Hf1 N33 2.234(4) . ? Hf1 O31 2.238(3) . ? Hf1 N43 2.240(4) . ? Hf1 N13 2.252(4) . ? Hf1 C22 2.599(5) . ? Hf1 C12 2.609(5) . ? Hf1 C42 2.612(5) . ? Hf1 C32 2.617(5) . ? O11 C12 1.277(5) . ? C12 N13 1.298(6) . ? C12 O12 1.339(6) . ? O12 C121 1.466(5) . ? C121 C123 1.502(8) . ? C121 C122 1.506(7) . ? C121 H121 1.0000 . ? C122 H12A 0.9800 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C123 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? N13 C13 1.460(6) . ? C13 C131 1.514(7) . ? C13 C132 1.520(7) . ? C13 H13 1.0000 . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C132 H13D 0.9800 . ? C132 H13E 0.9800 . ? C132 H13F 0.9800 . ? O21 C22 1.277(6) . ? C22 N23 1.306(6) . ? C22 O22 1.332(6) . ? O22 C221 1.462(5) . ? C221 C223 1.502(7) . ? C221 C222 1.503(7) . ? C221 H221 1.0000 . ? C222 H22A 0.9800 . ? C222 H22B 0.9800 . ? C222 H22C 0.9800 . ? C223 H22D 0.9800 . ? C223 H22E 0.9800 . ? C223 H22F 0.9800 . ? N23 C23 1.473(6) . ? C23 C231 1.506(7) . ? C23 C232 1.521(7) . ? C23 H23 1.0000 . ? C231 H23A 0.9800 . ? C231 H23B 0.9800 . ? C231 H23C 0.9800 . ? C232 H23D 0.9800 . ? C232 H23E 0.9800 . ? C232 H23F 0.9800 . ? O31 C32 1.282(6) . ? C32 N33 1.305(6) . ? C32 O32 1.336(6) . ? O32 C321 1.462(6) . ? C321 C322 1.491(7) . ? C321 C323 1.503(7) . ? C321 H321 1.0000 . ? C322 H32A 0.9800 . ? C322 H32B 0.9800 . ? C322 H32C 0.9800 . ? C323 H32D 0.9800 . ? C323 H32E 0.9800 . ? C323 H32F 0.9800 . ? N33 C33 1.478(6) . ? C33 C331 1.518(7) . ? C33 C332 1.520(7) . ? C33 H33 1.0000 . ? C331 H33A 0.9800 . ? C331 H33B 0.9800 . ? C331 H33C 0.9800 . ? C332 H33D 0.9800 . ? C332 H33E 0.9800 . ? C332 H33F 0.9800 . ? O41 C42 1.276(6) . ? C42 N43 1.309(6) . ? C42 O42 1.342(5) . ? O42 C421 1.456(6) . ? C421 C422 1.502(8) . ? C421 C423 1.515(8) . ? C421 H421 1.0000 . ? C422 H42A 0.9800 . ? C422 H42B 0.9800 . ? C422 H42C 0.9800 . ? C423 H42D 0.9800 . ? C423 H42E 0.9800 . ? C423 H42F 0.9800 . ? C43 N43 1.475(6) . ? C43 C432 1.509(7) . ? C43 C431 1.522(7) . ? C43 H43 1.0000 . ? C431 H43A 0.9800 . ? C431 H43B 0.9800 . ? C431 H43C 0.9800 . ? C432 H43D 0.9800 . ? C432 H43E 0.9800 . ? C432 H43F 0.9800 . ? 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 O11 Hf1 O21 127.46(12) . . ? O11 Hf1 O41 128.67(12) . . ? O21 Hf1 O41 75.47(12) . . ? O11 Hf1 N23 84.17(13) . . ? O21 Hf1 N23 59.43(13) . . ? O41 Hf1 N23 134.89(13) . . ? O11 Hf1 N33 134.59(13) . . ? O21 Hf1 N33 86.06(13) . . ? O41 Hf1 N33 84.74(13) . . ? N23 Hf1 N33 90.96(14) . . ? O11 Hf1 O31 75.40(11) . . ? O21 Hf1 O31 129.36(11) . . ? O41 Hf1 O31 129.43(12) . . ? N23 Hf1 O31 83.72(13) . . ? N33 Hf1 O31 59.20(13) . . ? O11 Hf1 N43 85.52(13) . . ? O21 Hf1 N43 134.75(13) . . ? O41 Hf1 N43 59.28(12) . . ? N23 Hf1 N43 165.78(14) . . ? N33 Hf1 N43 89.32(14) . . ? O31 Hf1 N43 84.22(13) . . ? O11 Hf1 N13 59.00(13) . . ? O21 Hf1 N13 85.78(13) . . ? O41 Hf1 N13 82.10(13) . . ? N23 Hf1 N13 94.75(14) . . ? N33 Hf1 N13 165.91(14) . . ? O31 Hf1 N13 134.23(12) . . ? N43 Hf1 N13 88.29(14) . . ? O11 Hf1 C22 108.64(13) . . ? O21 Hf1 C22 29.40(13) . . ? O41 Hf1 C22 104.76(13) . . ? N23 Hf1 C22 30.16(14) . . ? N33 Hf1 C22 86.15(14) . . ? O31 Hf1 C22 106.57(13) . . ? N43 Hf1 C22 163.79(15) . . ? N13 Hf1 C22 92.34(14) . . ? O11 Hf1 C12 29.24(13) . . ? O21 Hf1 C12 109.16(13) . . ? O41 Hf1 C12 105.58(13) . . ? N23 Hf1 C12 90.84(14) . . ? N33 Hf1 C12 163.17(14) . . ? O31 Hf1 C12 104.41(13) . . ? N43 Hf1 C12 84.89(14) . . ? N13 Hf1 C12 29.84(14) . . ? C22 Hf1 C12 103.51(14) . . ? O11 Hf1 C42 108.30(14) . . ? O21 Hf1 C42 104.68(14) . . ? O41 Hf1 C42 29.21(13) . . ? N23 Hf1 C42 164.09(15) . . ? N33 Hf1 C42 87.09(14) . . ? O31 Hf1 C42 108.59(14) . . ? N43 Hf1 C42 30.08(14) . . ? N13 Hf1 C42 83.89(14) . . ? C22 Hf1 C42 133.94(16) . . ? C12 Hf1 C42 95.58(14) . . ? O11 Hf1 C32 104.68(13) . . ? O21 Hf1 C32 109.81(13) . . ? O41 Hf1 C32 107.87(14) . . ? N23 Hf1 C32 87.81(14) . . ? N33 Hf1 C32 29.92(14) . . ? O31 Hf1 C32 29.31(13) . . ? N43 Hf1 C32 85.36(14) . . ? N13 Hf1 C32 162.98(14) . . ? C22 Hf1 C32 98.16(14) . . ? C12 Hf1 C32 133.52(15) . . ? C42 Hf1 C32 98.14(15) . . ? C12 O11 Hf1 93.1(3) . . ? O11 C12 N13 117.1(4) . . ? O11 C12 O12 121.4(4) . . ? N13 C12 O12 121.6(4) . . ? O11 C12 Hf1 57.6(2) . . ? N13 C12 Hf1 59.6(3) . . ? O12 C12 Hf1 174.8(3) . . ? C12 O12 C121 117.4(4) . . ? O12 C121 C123 109.2(4) . . ? O12 C121 C122 105.8(4) . . ? C123 C121 C122 113.3(5) . . ? O12 C121 H121 109.5 . . ? C123 C121 H121 109.5 . . ? C122 C121 H121 109.5 . . ? C121 C122 H12A 109.5 . . ? C121 C122 H12B 109.5 . . ? H12A C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C123 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12D C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C12 N13 C13 121.4(4) . . ? C12 N13 Hf1 90.5(3) . . ? C13 N13 Hf1 146.4(3) . . ? N13 C13 C131 109.5(4) . . ? N13 C13 C132 111.3(4) . . ? C131 C13 C132 110.6(4) . . ? N13 C13 H13 108.4 . . ? C131 C13 H13 108.4 . . ? C132 C13 H13 108.4 . . ? C13 C131 H13A 109.5 . . ? C13 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C13 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C13 C132 H13D 109.5 . . ? C13 C132 H13E 109.5 . . ? H13D C132 H13E 109.5 . . ? C13 C132 H13F 109.5 . . ? H13D C132 H13F 109.5 . . ? H13E C132 H13F 109.5 . . ? C22 O21 Hf1 92.3(3) . . ? O21 C22 N23 117.1(4) . . ? O21 C22 O22 122.3(4) . . ? N23 C22 O22 120.6(4) . . ? O21 C22 Hf1 58.3(2) . . ? N23 C22 Hf1 59.1(3) . . ? O22 C22 Hf1 172.3(3) . . ? C22 O22 C221 118.8(4) . . ? O22 C221 C223 105.5(4) . . ? O22 C221 C222 108.3(4) . . ? C223 C221 C222 114.8(4) . . ? O22 C221 H221 109.4 . . ? C223 C221 H221 109.4 . . ? C222 C221 H221 109.4 . . ? C221 C222 H22A 109.5 . . ? C221 C222 H22B 109.5 . . ? H22A C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22A C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C221 C223 H22D 109.5 . . ? C221 C223 H22E 109.5 . . ? H22D C223 H22E 109.5 . . ? C221 C223 H22F 109.5 . . ? H22D C223 H22F 109.5 . . ? H22E C223 H22F 109.5 . . ? C22 N23 C23 120.7(4) . . ? C22 N23 Hf1 90.7(3) . . ? C23 N23 Hf1 147.1(3) . . ? N23 C23 C231 109.8(4) . . ? N23 C23 C232 110.3(4) . . ? C231 C23 C232 112.2(4) . . ? N23 C23 H23 108.1 . . ? C231 C23 H23 108.1 . . ? C232 C23 H23 108.1 . . ? C23 C231 H23A 109.5 . . ? C23 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? C23 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? C23 C232 H23D 109.5 . . ? C23 C232 H23E 109.5 . . ? H23D C232 H23E 109.5 . . ? C23 C232 H23F 109.5 . . ? H23D C232 H23F 109.5 . . ? H23E C232 H23F 109.5 . . ? C32 O31 Hf1 91.9(3) . . ? O31 C32 N33 117.3(4) . . ? O31 C32 O32 122.1(4) . . ? N33 C32 O32 120.6(4) . . ? O31 C32 Hf1 58.7(2) . . ? N33 C32 Hf1 58.6(2) . . ? O32 C32 Hf1 178.2(3) . . ? C32 O32 C321 119.2(4) . . ? O32 C321 C322 110.2(4) . . ? O32 C321 C323 104.9(4) . . ? C322 C321 C323 112.9(5) . . ? O32 C321 H321 109.6 . . ? C322 C321 H321 109.6 . . ? C323 C321 H321 109.6 . . ? C321 C322 H32A 109.5 . . ? C321 C322 H32B 109.5 . . ? H32A C322 H32B 109.5 . . ? C321 C322 H32C 109.5 . . ? H32A C322 H32C 109.5 . . ? H32B C322 H32C 109.5 . . ? C321 C323 H32D 109.5 . . ? C321 C323 H32E 109.5 . . ? H32D C323 H32E 109.5 . . ? C321 C323 H32F 109.5 . . ? H32D C323 H32F 109.5 . . ? H32E C323 H32F 109.5 . . ? C32 N33 C33 120.7(4) . . ? C32 N33 Hf1 91.5(3) . . ? C33 N33 Hf1 147.4(3) . . ? N33 C33 C331 110.1(4) . . ? N33 C33 C332 109.0(4) . . ? C331 C33 C332 111.4(5) . . ? N33 C33 H33 108.8 . . ? C331 C33 H33 108.8 . . ? C332 C33 H33 108.8 . . ? C33 C331 H33A 109.5 . . ? C33 C331 H33B 109.5 . . ? H33A C331 H33B 109.5 . . ? C33 C331 H33C 109.5 . . ? H33A C331 H33C 109.5 . . ? H33B C331 H33C 109.5 . . ? C33 C332 H33D 109.5 . . ? C33 C332 H33E 109.5 . . ? H33D C332 H33E 109.5 . . ? C33 C332 H33F 109.5 . . ? H33D C332 H33F 109.5 . . ? H33E C332 H33F 109.5 . . ? C42 O41 Hf1 92.7(3) . . ? O41 C42 N43 117.0(4) . . ? O41 C42 O42 121.5(4) . . ? N43 C42 O42 121.5(4) . . ? O41 C42 Hf1 58.1(2) . . ? N43 C42 Hf1 59.0(2) . . ? O42 C42 Hf1 177.5(3) . . ? C42 O42 C421 117.9(4) . . ? O42 C421 C422 109.3(4) . . ? O42 C421 C423 105.4(4) . . ? C422 C421 C423 113.5(5) . . ? O42 C421 H421 109.5 . . ? C422 C421 H421 109.5 . . ? C423 C421 H421 109.5 . . ? C421 C422 H42A 109.5 . . ? C421 C422 H42B 109.5 . . ? H42A C422 H42B 109.5 . . ? C421 C422 H42C 109.5 . . ? H42A C422 H42C 109.5 . . ? H42B C422 H42C 109.5 . . ? C421 C423 H42D 109.5 . . ? C421 C423 H42E 109.5 . . ? H42D C423 H42E 109.5 . . ? C421 C423 H42F 109.5 . . ? H42D C423 H42F 109.5 . . ? H42E C423 H42F 109.5 . . ? N43 C43 C432 109.7(4) . . ? N43 C43 C431 109.5(4) . . ? C432 C43 C431 111.2(4) . . ? N43 C43 H43 108.8 . . ? C432 C43 H43 108.8 . . ? C431 C43 H43 108.8 . . ? C42 N43 C43 120.9(4) . . ? C42 N43 Hf1 90.9(3) . . ? C43 N43 Hf1 148.2(3) . . ? C43 C431 H43A 109.5 . . ? C43 C431 H43B 109.5 . . ? H43A C431 H43B 109.5 . . ? C43 C431 H43C 109.5 . . ? H43A C431 H43C 109.5 . . ? H43B C431 H43C 109.5 . . ? C43 C432 H43D 109.5 . . ? C43 C432 H43E 109.5 . . ? H43D C432 H43E 109.5 . . ? C43 C432 H43F 109.5 . . ? H43D C432 H43F 109.5 . . ? H43E C432 H43F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O21 Hf1 O11 C12 -58.5(3) . . . . ? O41 Hf1 O11 C12 43.5(3) . . . . ? N23 Hf1 O11 C12 -102.3(3) . . . . ? N33 Hf1 O11 C12 172.1(3) . . . . ? O31 Hf1 O11 C12 172.7(3) . . . . ? N43 Hf1 O11 C12 87.5(3) . . . . ? N13 Hf1 O11 C12 -3.2(3) . . . . ? C22 Hf1 O11 C12 -84.4(3) . . . . ? C42 Hf1 O11 C12 67.6(3) . . . . ? C32 Hf1 O11 C12 171.5(3) . . . . ? Hf1 O11 C12 N13 5.3(4) . . . . ? Hf1 O11 C12 O12 -174.0(4) . . . . ? O21 Hf1 C12 O11 134.2(2) . . . . ? O41 Hf1 C12 O11 -146.1(2) . . . . ? N23 Hf1 C12 O11 76.4(3) . . . . ? N33 Hf1 C12 O11 -19.7(6) . . . . ? O31 Hf1 C12 O11 -7.3(3) . . . . ? N43 Hf1 C12 O11 -90.0(3) . . . . ? N13 Hf1 C12 O11 174.5(4) . . . . ? C22 Hf1 C12 O11 104.1(3) . . . . ? C42 Hf1 C12 O11 -118.1(3) . . . . ? C32 Hf1 C12 O11 -11.3(4) . . . . ? O11 Hf1 C12 N13 -174.5(4) . . . . ? O21 Hf1 C12 N13 -40.3(3) . . . . ? O41 Hf1 C12 N13 39.4(3) . . . . ? N23 Hf1 C12 N13 -98.1(3) . . . . ? N33 Hf1 C12 N13 165.8(4) . . . . ? O31 Hf1 C12 N13 178.2(3) . . . . ? N43 Hf1 C12 N13 95.5(3) . . . . ? C22 Hf1 C12 N13 -70.4(3) . . . . ? C42 Hf1 C12 N13 67.3(3) . . . . ? C32 Hf1 C12 N13 174.1(3) . . . . ? O11 Hf1 C12 O12 81(4) . . . . ? O21 Hf1 C12 O12 -145(4) . . . . ? O41 Hf1 C12 O12 -66(4) . . . . ? N23 Hf1 C12 O12 157(4) . . . . ? N33 Hf1 C12 O12 61(4) . . . . ? O31 Hf1 C12 O12 73(4) . . . . ? N43 Hf1 C12 O12 -9(4) . . . . ? N13 Hf1 C12 O12 -105(4) . . . . ? C22 Hf1 C12 O12 -175(4) . . . . ? C42 Hf1 C12 O12 -38(4) . . . . ? C32 Hf1 C12 O12 69(4) . . . . ? O11 C12 O12 C121 -0.7(6) . . . . ? N13 C12 O12 C121 -179.9(4) . . . . ? Hf1 C12 O12 C121 -78(4) . . . . ? C12 O12 C121 C123 -85.6(5) . . . . ? C12 O12 C121 C122 152.2(4) . . . . ? O11 C12 N13 C13 -174.1(4) . . . . ? O12 C12 N13 C13 5.1(7) . . . . ? Hf1 C12 N13 C13 -168.9(5) . . . . ? O11 C12 N13 Hf1 -5.2(4) . . . . ? O12 C12 N13 Hf1 174.1(4) . . . . ? O11 Hf1 N13 C12 3.1(3) . . . . ? O21 Hf1 N13 C12 142.2(3) . . . . ? O41 Hf1 N13 C12 -141.9(3) . . . . ? N23 Hf1 N13 C12 83.4(3) . . . . ? N33 Hf1 N13 C12 -163.0(5) . . . . ? O31 Hf1 N13 C12 -2.5(4) . . . . ? N43 Hf1 N13 C12 -82.7(3) . . . . ? C22 Hf1 N13 C12 113.5(3) . . . . ? C42 Hf1 N13 C12 -112.5(3) . . . . ? C32 Hf1 N13 C12 -14.7(6) . . . . ? O11 Hf1 N13 C13 165.9(6) . . . . ? O21 Hf1 N13 C13 -55.1(6) . . . . ? O41 Hf1 N13 C13 20.8(6) . . . . ? N23 Hf1 N13 C13 -113.9(6) . . . . ? N33 Hf1 N13 C13 -0.3(10) . . . . ? O31 Hf1 N13 C13 160.3(5) . . . . ? N43 Hf1 N13 C13 80.1(6) . . . . ? C22 Hf1 N13 C13 -83.7(6) . . . . ? C12 Hf1 N13 C13 162.8(7) . . . . ? C42 Hf1 N13 C13 50.2(6) . . . . ? C32 Hf1 N13 C13 148.1(6) . . . . ? C12 N13 C13 C131 -161.2(4) . . . . ? Hf1 N13 C13 C131 39.1(7) . . . . ? C12 N13 C13 C132 76.2(6) . . . . ? Hf1 N13 C13 C132 -83.5(6) . . . . ? O11 Hf1 O21 C22 -57.4(3) . . . . ? O41 Hf1 O21 C22 174.7(3) . . . . ? N23 Hf1 O21 C22 -4.3(3) . . . . ? N33 Hf1 O21 C22 89.1(3) . . . . ? O31 Hf1 O21 C22 45.2(3) . . . . ? N43 Hf1 O21 C22 174.3(3) . . . . ? N13 Hf1 O21 C22 -102.4(3) . . . . ? C12 Hf1 O21 C22 -83.5(3) . . . . ? C42 Hf1 O21 C22 175.1(3) . . . . ? C32 Hf1 O21 C22 70.6(3) . . . . ? Hf1 O21 C22 N23 7.1(4) . . . . ? Hf1 O21 C22 O22 -171.0(4) . . . . ? O11 Hf1 C22 O21 135.1(2) . . . . ? O41 Hf1 C22 O21 -5.3(3) . . . . ? N23 Hf1 C22 O21 172.6(4) . . . . ? N33 Hf1 C22 O21 -88.8(3) . . . . ? O31 Hf1 C22 O21 -145.1(2) . . . . ? N43 Hf1 C22 O21 -14.7(7) . . . . ? N13 Hf1 C22 O21 77.2(3) . . . . ? C12 Hf1 C22 O21 105.1(3) . . . . ? C42 Hf1 C22 O21 -6.6(3) . . . . ? C32 Hf1 C22 O21 -116.3(3) . . . . ? O11 Hf1 C22 N23 -37.5(3) . . . . ? O21 Hf1 C22 N23 -172.6(4) . . . . ? O41 Hf1 C22 N23 -177.9(3) . . . . ? N33 Hf1 C22 N23 98.6(3) . . . . ? O31 Hf1 C22 N23 42.3(3) . . . . ? N43 Hf1 C22 N23 172.7(4) . . . . ? N13 Hf1 C22 N23 -95.4(3) . . . . ? C12 Hf1 C22 N23 -67.5(3) . . . . ? C42 Hf1 C22 N23 -179.2(3) . . . . ? C32 Hf1 C22 N23 71.1(3) . . . . ? O11 Hf1 C22 O22 -128(3) . . . . ? O21 Hf1 C22 O22 97(3) . . . . ? O41 Hf1 C22 O22 92(3) . . . . ? N23 Hf1 C22 O22 -91(3) . . . . ? N33 Hf1 C22 O22 8(3) . . . . ? O31 Hf1 C22 O22 -48(3) . . . . ? N43 Hf1 C22 O22 82(3) . . . . ? N13 Hf1 C22 O22 174(3) . . . . ? C12 Hf1 C22 O22 -158(3) . . . . ? C42 Hf1 C22 O22 90(3) . . . . ? C32 Hf1 C22 O22 -19(3) . . . . ? O21 C22 O22 C221 -3.9(6) . . . . ? N23 C22 O22 C221 178.0(4) . . . . ? Hf1 C22 O22 C221 -96(3) . . . . ? C22 O22 C221 C223 153.0(4) . . . . ? C22 O22 C221 C222 -83.6(5) . . . . ? O21 C22 N23 C23 -176.6(4) . . . . ? O22 C22 N23 C23 1.6(7) . . . . ? Hf1 C22 N23 C23 -169.5(5) . . . . ? O21 C22 N23 Hf1 -7.1(4) . . . . ? O22 C22 N23 Hf1 171.1(4) . . . . ? O11 Hf1 N23 C22 144.6(3) . . . . ? O21 Hf1 N23 C22 4.2(3) . . . . ? O41 Hf1 N23 C22 2.9(4) . . . . ? N33 Hf1 N23 C22 -80.6(3) . . . . ? O31 Hf1 N23 C22 -139.5(3) . . . . ? N43 Hf1 N23 C22 -171.7(5) . . . . ? N13 Hf1 N23 C22 86.5(3) . . . . ? C12 Hf1 N23 C22 116.1(3) . . . . ? C42 Hf1 N23 C22 2.1(7) . . . . ? C32 Hf1 N23 C22 -110.4(3) . . . . ? O11 Hf1 N23 C23 -52.2(6) . . . . ? O21 Hf1 N23 C23 167.4(6) . . . . ? O41 Hf1 N23 C23 166.1(5) . . . . ? N33 Hf1 N23 C23 82.6(6) . . . . ? O31 Hf1 N23 C23 23.7(6) . . . . ? N43 Hf1 N23 C23 -8.5(10) . . . . ? N13 Hf1 N23 C23 -110.3(6) . . . . ? C22 Hf1 N23 C23 163.2(7) . . . . ? C12 Hf1 N23 C23 -80.7(6) . . . . ? C42 Hf1 N23 C23 165.3(5) . . . . ? C32 Hf1 N23 C23 52.8(6) . . . . ? C22 N23 C23 C231 -149.3(5) . . . . ? Hf1 N23 C23 C231 50.4(7) . . . . ? C22 N23 C23 C232 86.6(5) . . . . ? Hf1 N23 C23 C232 -73.8(7) . . . . ? O11 Hf1 O31 C32 -177.7(3) . . . . ? O21 Hf1 O31 C32 55.5(3) . . . . ? O41 Hf1 O31 C32 -49.2(3) . . . . ? N23 Hf1 O31 C32 96.7(3) . . . . ? N33 Hf1 O31 C32 1.9(3) . . . . ? N43 Hf1 O31 C32 -90.8(3) . . . . ? N13 Hf1 O31 C32 -172.7(3) . . . . ? C22 Hf1 O31 C32 76.8(3) . . . . ? C12 Hf1 O31 C32 -174.0(3) . . . . ? C42 Hf1 O31 C32 -72.9(3) . . . . ? Hf1 O31 C32 N33 -3.1(4) . . . . ? Hf1 O31 C32 O32 178.1(4) . . . . ? O11 Hf1 C32 O31 2.3(3) . . . . ? O21 Hf1 C32 O31 -137.4(2) . . . . ? O41 Hf1 C32 O31 142.1(2) . . . . ? N23 Hf1 C32 O31 -81.1(3) . . . . ? N33 Hf1 C32 O31 -176.8(4) . . . . ? N43 Hf1 C32 O31 86.5(3) . . . . ? N13 Hf1 C32 O31 18.0(6) . . . . ? C22 Hf1 C32 O31 -109.5(3) . . . . ? C12 Hf1 C32 O31 8.0(4) . . . . ? C42 Hf1 C32 O31 113.8(3) . . . . ? O11 Hf1 C32 N33 179.1(3) . . . . ? O21 Hf1 C32 N33 39.4(3) . . . . ? O41 Hf1 C32 N33 -41.1(3) . . . . ? N23 Hf1 C32 N33 95.7(3) . . . . ? O31 Hf1 C32 N33 176.8(4) . . . . ? N43 Hf1 C32 N33 -96.7(3) . . . . ? N13 Hf1 C32 N33 -165.2(4) . . . . ? C22 Hf1 C32 N33 67.3(3) . . . . ? C12 Hf1 C32 N33 -175.2(3) . . . . ? C42 Hf1 C32 N33 -69.4(3) . . . . ? O11 Hf1 C32 O32 -116(11) . . . . ? O21 Hf1 C32 O32 104(11) . . . . ? O41 Hf1 C32 O32 24(11) . . . . ? N23 Hf1 C32 O32 161(11) . . . . ? N33 Hf1 C32 O32 65(11) . . . . ? O31 Hf1 C32 O32 -118(11) . . . . ? N43 Hf1 C32 O32 -32(11) . . . . ? N13 Hf1 C32 O32 -100(11) . . . . ? C22 Hf1 C32 O32 132(11) . . . . ? C12 Hf1 C32 O32 -110(11) . . . . ? C42 Hf1 C32 O32 -4(11) . . . . ? O31 C32 O32 C321 3.8(7) . . . . ? N33 C32 O32 C321 -174.9(4) . . . . ? Hf1 C32 O32 C321 121(11) . . . . ? C32 O32 C321 C322 -87.1(5) . . . . ? C32 O32 C321 C323 151.1(4) . . . . ? O31 C32 N33 C33 178.0(4) . . . . ? O32 C32 N33 C33 -3.2(7) . . . . ? Hf1 C32 N33 C33 174.9(5) . . . . ? O31 C32 N33 Hf1 3.1(4) . . . . ? O32 C32 N33 Hf1 -178.1(4) . . . . ? O11 Hf1 N33 C32 -1.2(4) . . . . ? O21 Hf1 N33 C32 -143.2(3) . . . . ? O41 Hf1 N33 C32 141.1(3) . . . . ? N23 Hf1 N33 C32 -83.9(3) . . . . ? O31 Hf1 N33 C32 -1.8(3) . . . . ? N43 Hf1 N33 C32 81.9(3) . . . . ? N13 Hf1 N33 C32 162.1(5) . . . . ? C22 Hf1 N33 C32 -113.7(3) . . . . ? C12 Hf1 N33 C32 12.2(6) . . . . ? C42 Hf1 N33 C32 111.9(3) . . . . ? O11 Hf1 N33 C33 -173.1(5) . . . . ? O21 Hf1 N33 C33 44.9(6) . . . . ? O41 Hf1 N33 C33 -30.9(6) . . . . ? N23 Hf1 N33 C33 104.2(6) . . . . ? O31 Hf1 N33 C33 -173.7(6) . . . . ? N43 Hf1 N33 C33 -90.1(6) . . . . ? N13 Hf1 N33 C33 -9.9(10) . . . . ? C22 Hf1 N33 C33 74.4(6) . . . . ? C12 Hf1 N33 C33 -159.7(5) . . . . ? C42 Hf1 N33 C33 -60.0(6) . . . . ? C32 Hf1 N33 C33 -171.9(7) . . . . ? C32 N33 C33 C331 -76.3(6) . . . . ? Hf1 N33 C33 C331 94.2(6) . . . . ? C32 N33 C33 C332 161.2(5) . . . . ? Hf1 N33 C33 C332 -28.2(8) . . . . ? O11 Hf1 O41 C42 52.6(3) . . . . ? O21 Hf1 O41 C42 179.3(3) . . . . ? N23 Hf1 O41 C42 -179.6(3) . . . . ? N33 Hf1 O41 C42 -93.4(3) . . . . ? O31 Hf1 O41 C42 -51.3(3) . . . . ? N43 Hf1 O41 C42 -1.1(3) . . . . ? N13 Hf1 O41 C42 91.6(3) . . . . ? C22 Hf1 O41 C42 -178.1(3) . . . . ? C12 Hf1 O41 C42 73.0(3) . . . . ? C32 Hf1 O41 C42 -74.2(3) . . . . ? Hf1 O41 C42 N43 1.8(4) . . . . ? Hf1 O41 C42 O42 -177.2(4) . . . . ? O11 Hf1 C42 O41 -139.2(2) . . . . ? O21 Hf1 C42 O41 -0.7(3) . . . . ? N23 Hf1 C42 O41 1.1(7) . . . . ? N33 Hf1 C42 O41 84.4(3) . . . . ? O31 Hf1 C42 O41 140.5(2) . . . . ? N43 Hf1 C42 O41 178.1(4) . . . . ? N13 Hf1 C42 O41 -84.7(3) . . . . ? C22 Hf1 C42 O41 2.6(4) . . . . ? C12 Hf1 C42 O41 -112.2(3) . . . . ? C32 Hf1 C42 O41 112.3(3) . . . . ? O11 Hf1 C42 N43 42.7(3) . . . . ? O21 Hf1 C42 N43 -178.8(3) . . . . ? O41 Hf1 C42 N43 -178.1(4) . . . . ? N23 Hf1 C42 N43 -176.9(5) . . . . ? N33 Hf1 C42 N43 -93.7(3) . . . . ? O31 Hf1 C42 N43 -37.6(3) . . . . ? N13 Hf1 C42 N43 97.2(3) . . . . ? C22 Hf1 C42 N43 -175.5(3) . . . . ? C12 Hf1 C42 N43 69.7(3) . . . . ? C32 Hf1 C42 N43 -65.8(3) . . . . ? O11 Hf1 C42 O42 -60(9) . . . . ? O21 Hf1 C42 O42 79(9) . . . . ? O41 Hf1 C42 O42 79(9) . . . . ? N23 Hf1 C42 O42 81(9) . . . . ? N33 Hf1 C42 O42 164(9) . . . . ? O31 Hf1 C42 O42 -140(9) . . . . ? N43 Hf1 C42 O42 -102(9) . . . . ? N13 Hf1 C42 O42 -5(9) . . . . ? C22 Hf1 C42 O42 82(9) . . . . ? C12 Hf1 C42 O42 -33(9) . . . . ? C32 Hf1 C42 O42 -168(9) . . . . ? O41 C42 O42 C421 3.8(6) . . . . ? N43 C42 O42 C421 -175.2(4) . . . . ? Hf1 C42 O42 C421 -74(9) . . . . ? C42 O42 C421 C422 -89.2(6) . . . . ? C42 O42 C421 C423 148.4(5) . . . . ? O41 C42 N43 C43 177.8(4) . . . . ? O42 C42 N43 C43 -3.2(7) . . . . ? Hf1 C42 N43 C43 179.6(5) . . . . ? O41 C42 N43 Hf1 -1.8(4) . . . . ? O42 C42 N43 Hf1 177.2(4) . . . . ? C432 C43 N43 C42 156.2(4) . . . . ? C431 C43 N43 C42 -81.4(5) . . . . ? C432 C43 N43 Hf1 -24.5(8) . . . . ? C431 C43 N43 Hf1 97.8(6) . . . . ? O11 Hf1 N43 C42 -139.8(3) . . . . ? O21 Hf1 N43 C42 1.6(4) . . . . ? O41 Hf1 N43 C42 1.1(2) . . . . ? N23 Hf1 N43 C42 176.6(5) . . . . ? N33 Hf1 N43 C42 85.4(3) . . . . ? O31 Hf1 N43 C42 144.5(3) . . . . ? N13 Hf1 N43 C42 -80.7(3) . . . . ? C22 Hf1 N43 C42 11.7(7) . . . . ? C12 Hf1 N43 C42 -110.4(3) . . . . ? C32 Hf1 N43 C42 115.1(3) . . . . ? O11 Hf1 N43 C43 40.9(6) . . . . ? O21 Hf1 N43 C43 -177.7(5) . . . . ? O41 Hf1 N43 C43 -178.3(6) . . . . ? N23 Hf1 N43 C43 -2.8(10) . . . . ? N33 Hf1 N43 C43 -94.0(6) . . . . ? O31 Hf1 N43 C43 -34.9(6) . . . . ? N13 Hf1 N43 C43 99.9(6) . . . . ? C22 Hf1 N43 C43 -167.6(5) . . . . ? C12 Hf1 N43 C43 70.2(6) . . . . ? C42 Hf1 N43 C43 -179.3(8) . . . . ? C32 Hf1 N43 C43 -64.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.273 _refine_diff_density_min -1.581 _refine_diff_density_rms 0.125 #=================================END data_cvd263 _database_code_depnum_ccdc_archive 'CCDC 711073' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H60 Hf N8 O4' _chemical_formula_weight 751.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 11.1068(4) _cell_length_b 19.5845(7) _cell_length_c 16.2298(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.163(3) _cell_angle_gamma 90.00 _cell_volume 3474.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 109(2) _cell_measurement_reflns_used 10112 _cell_measurement_theta_min 2.738 _cell_measurement_theta_max 27.499 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 3.044 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.4242 _exptl_absorpt_correction_T_max 0.5811 _exptl_absorpt_process_details 'Gaussian face-indexed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 109(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '390 images at 1.0 deg. in \w and 25 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19139 _diffrn_reflns_av_R_equivalents 0.0748 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6085 _reflns_number_gt 4622 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^ > 2sigma(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^)+(0.0188P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6085 _refine_ls_number_parameters 386 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0537 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 Hf1 Hf 0.507025(17) 0.195747(7) 0.747098(11) 0.01445(6) Uani 1 1 d . . . N11 N 0.3488(3) 0.26494(16) 0.7620(2) 0.0178(8) Uani 1 1 d . . . C11 C 0.3025(4) 0.3108(2) 0.8205(2) 0.0248(10) Uani 1 1 d . . . H11 H 0.2199 0.3269 0.7926 0.030 Uiso 1 1 calc R . . C111 C 0.2866(6) 0.2731(3) 0.8978(3) 0.0678(19) Uani 1 1 d . . . H11A H 0.2383 0.2318 0.8823 0.102 Uiso 1 1 calc R . . H11B H 0.2440 0.3024 0.9324 0.102 Uiso 1 1 calc R . . H11C H 0.3669 0.2606 0.9295 0.102 Uiso 1 1 calc R . . C112 C 0.3832(4) 0.3726(3) 0.8377(3) 0.0471(14) Uani 1 1 d . . . H11D H 0.4650 0.3586 0.8656 0.071 Uiso 1 1 calc R . . H11E H 0.3482 0.4042 0.8740 0.071 Uiso 1 1 calc R . . H11F H 0.3890 0.3954 0.7848 0.071 Uiso 1 1 calc R . . N12 N 0.1815(3) 0.2748(2) 0.6455(2) 0.0362(10) Uani 1 1 d . . . C12 C 0.2982(4) 0.2558(2) 0.6840(3) 0.0201(9) Uani 1 1 d . . . C121 C 0.1538(4) 0.2653(3) 0.5548(3) 0.0373(12) Uani 1 1 d . . . H12A H 0.2213 0.2832 0.5296 0.056 Uiso 1 1 calc R . . H12B H 0.0783 0.2898 0.5320 0.056 Uiso 1 1 calc R . . H12C H 0.1430 0.2165 0.5420 0.056 Uiso 1 1 calc R . . C122 C 0.0773(4) 0.2490(3) 0.6896(3) 0.0409(13) Uani 1 1 d . . . H12D H 0.0475 0.2044 0.6653 0.049 Uiso 1 1 calc R . . H12E H 0.1101 0.2418 0.7498 0.049 Uiso 1 1 calc R . . C123 C -0.0247(5) 0.2967(3) 0.6812(4) 0.0582(16) Uani 1 1 d . . . H12F H 0.0059 0.3423 0.6986 0.087 Uiso 1 1 calc R . . H12G H -0.0826 0.2817 0.7166 0.087 Uiso 1 1 calc R . . H12H H -0.0661 0.2981 0.6226 0.087 Uiso 1 1 calc R . . O13 O 0.3648(2) 0.22239(14) 0.63967(15) 0.0167(6) Uani 1 1 d . . . N21 N 0.6073(3) 0.28578(16) 0.70378(19) 0.0175(7) Uani 1 1 d . . . C21 C 0.6140(4) 0.3249(2) 0.6275(2) 0.0224(10) Uani 1 1 d . . . H21 H 0.6929 0.3507 0.6360 0.027 Uiso 1 1 calc R . . C211 C 0.6121(4) 0.2756(2) 0.5553(3) 0.0335(11) Uani 1 1 d . . . H21A H 0.6821 0.2446 0.5677 0.050 Uiso 1 1 calc R . . H21B H 0.6169 0.3013 0.5041 0.050 Uiso 1 1 calc R . . H21C H 0.5360 0.2492 0.5473 0.050 Uiso 1 1 calc R . . C212 C 0.5081(4) 0.3759(2) 0.6084(3) 0.0337(11) Uani 1 1 d . . . H21D H 0.4305 0.3510 0.5961 0.051 Uiso 1 1 calc R . . H21E H 0.5181 0.4036 0.5598 0.051 Uiso 1 1 calc R . . H21F H 0.5081 0.4056 0.6569 0.051 Uiso 1 1 calc R . . N22 N 0.7149(3) 0.36049(17) 0.8120(2) 0.0214(8) Uani 1 1 d . . . C22 C 0.6503(3) 0.3039(2) 0.7813(2) 0.0183(9) Uani 1 1 d . . . C221 C 0.7563(4) 0.4150(2) 0.7635(3) 0.0265(10) Uani 1 1 d . . . H22A H 0.8251 0.3988 0.7384 0.040 Uiso 1 1 calc R . . H22B H 0.7826 0.4540 0.8001 0.040 Uiso 1 1 calc R . . H22C H 0.6892 0.4290 0.7191 0.040 Uiso 1 1 calc R . . C222 C 0.7654(4) 0.3639(2) 0.9023(2) 0.0276(10) Uani 1 1 d . . . H22D H 0.7238 0.3294 0.9319 0.033 Uiso 1 1 calc R . . H22E H 0.7476 0.4094 0.9237 0.033 Uiso 1 1 calc R . . C223 C 0.9011(4) 0.3516(2) 0.9220(3) 0.0387(12) Uani 1 1 d . . . H22F H 0.9198 0.3071 0.8997 0.058 Uiso 1 1 calc R . . H22G H 0.9284 0.3521 0.9829 0.058 Uiso 1 1 calc R . . H22H H 0.9435 0.3876 0.8964 0.058 Uiso 1 1 calc R . . O23 O 0.6221(2) 0.26094(13) 0.83607(15) 0.0170(6) Uani 1 1 d . . . O33 O 0.5518(2) 0.13891(14) 0.63978(16) 0.0158(6) Uani 1 1 d . . . N31 N 0.6790(3) 0.12921(16) 0.75890(19) 0.0163(7) Uani 1 1 d . . . C31 C 0.7798(4) 0.1001(2) 0.8186(2) 0.0218(9) Uani 1 1 d . . . H31 H 0.8283 0.0692 0.7878 0.026 Uiso 1 1 calc R . . C311 C 0.8635(4) 0.1566(2) 0.8603(3) 0.0314(11) Uani 1 1 d . . . H31A H 0.9005 0.1805 0.8180 0.047 Uiso 1 1 calc R . . H31B H 0.9281 0.1366 0.9024 0.047 Uiso 1 1 calc R . . H31C H 0.8158 0.1889 0.8875 0.047 Uiso 1 1 calc R . . C312 C 0.7288(4) 0.0584(2) 0.8837(3) 0.0281(11) Uani 1 1 d . . . H31D H 0.6909 0.0891 0.9194 0.042 Uiso 1 1 calc R . . H31E H 0.7954 0.0331 0.9183 0.042 Uiso 1 1 calc R . . H31F H 0.6675 0.0263 0.8555 0.042 Uiso 1 1 calc R . . C32 C 0.6565(3) 0.11610(19) 0.6784(2) 0.0143(9) Uani 1 1 d . . . N32 N 0.7291(3) 0.08001(16) 0.63288(19) 0.0154(7) Uani 1 1 d . . . C321 C 0.6724(4) 0.0634(2) 0.5472(2) 0.0240(10) Uani 1 1 d . . . H32A H 0.5917 0.0431 0.5471 0.036 Uiso 1 1 calc R . . H32B H 0.7241 0.0309 0.5235 0.036 Uiso 1 1 calc R . . H32C H 0.6631 0.1052 0.5134 0.036 Uiso 1 1 calc R . . C322 C 0.8574(3) 0.0994(2) 0.6397(3) 0.0245(10) Uani 1 1 d . . . H32D H 0.8818 0.1268 0.6912 0.029 Uiso 1 1 calc R . . H32E H 0.8663 0.1287 0.5914 0.029 Uiso 1 1 calc R . . C323 C 0.9432(4) 0.0390(2) 0.6422(3) 0.0388(12) Uani 1 1 d . . . H32F H 0.9395 0.0115 0.6921 0.058 Uiso 1 1 calc R . . H32G H 1.0270 0.0555 0.6442 0.058 Uiso 1 1 calc R . . H32H H 0.9188 0.0111 0.5920 0.058 Uiso 1 1 calc R . . N41 N 0.3864(3) 0.10338(16) 0.75957(19) 0.0163(7) Uani 1 1 d . . . C41 C 0.3260(4) 0.0466(2) 0.7089(2) 0.0192(9) Uani 1 1 d . . . H41 H 0.2547 0.0309 0.7338 0.023 Uiso 1 1 calc R . . C411 C 0.4150(4) -0.0126(2) 0.7095(3) 0.0296(11) Uani 1 1 d . . . H41A H 0.4881 0.0031 0.6890 0.044 Uiso 1 1 calc R . . H41B H 0.3758 -0.0492 0.6732 0.044 Uiso 1 1 calc R . . H41C H 0.4385 -0.0299 0.7668 0.044 Uiso 1 1 calc R . . C412 C 0.2797(4) 0.0714(2) 0.6203(3) 0.0264(11) Uani 1 1 d . . . H41D H 0.2205 0.1083 0.6215 0.040 Uiso 1 1 calc R . . H41E H 0.2401 0.0335 0.5864 0.040 Uiso 1 1 calc R . . H41F H 0.3486 0.0883 0.5958 0.040 Uiso 1 1 calc R . . N42 N 0.3852(3) 0.06130(17) 0.9009(2) 0.0234(8) Uani 1 1 d . . . C42 C 0.4157(4) 0.1054(2) 0.8421(2) 0.0178(9) Uani 1 1 d . . . C421 C 0.4234(4) 0.0822(2) 0.9887(2) 0.0337(11) Uani 1 1 d . . . H42A H 0.5074 0.0997 0.9968 0.051 Uiso 1 1 calc R . . H42B H 0.4197 0.0428 1.0254 0.051 Uiso 1 1 calc R . . H42C H 0.3686 0.1181 1.0022 0.051 Uiso 1 1 calc R . . C422 C 0.2776(4) 0.0168(2) 0.8870(3) 0.0283(11) Uani 1 1 d . . . H42D H 0.2804 -0.0140 0.9357 0.034 Uiso 1 1 calc R . . H42E H 0.2795 -0.0119 0.8370 0.034 Uiso 1 1 calc R . . C423 C 0.1590(4) 0.0571(3) 0.8744(3) 0.0418(13) Uani 1 1 d . . . H42F H 0.1562 0.0850 0.9241 0.063 Uiso 1 1 calc R . . H42G H 0.0895 0.0255 0.8657 0.063 Uiso 1 1 calc R . . H42H H 0.1548 0.0867 0.8254 0.063 Uiso 1 1 calc R . . O43 O 0.4864(2) 0.15575(14) 0.86932(16) 0.0180(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hf1 0.01585(9) 0.01311(8) 0.01400(8) -0.00080(9) 0.00154(5) 0.00030(10) N11 0.0188(18) 0.0179(19) 0.0174(18) -0.0012(15) 0.0051(14) 0.0004(16) C11 0.028(2) 0.021(2) 0.028(2) -0.002(2) 0.0101(19) 0.005(2) C111 0.125(6) 0.048(4) 0.041(3) -0.002(3) 0.046(4) 0.025(4) C112 0.041(3) 0.036(3) 0.066(4) -0.030(3) 0.016(3) -0.003(3) N12 0.027(2) 0.058(3) 0.0221(19) -0.0024(19) -0.0009(16) 0.023(2) C12 0.023(2) 0.013(2) 0.026(2) 0.0062(18) 0.0083(19) 0.004(2) C121 0.039(3) 0.050(3) 0.020(2) -0.002(2) -0.002(2) 0.024(3) C122 0.034(3) 0.043(3) 0.042(3) 0.001(2) -0.005(2) -0.004(3) C123 0.037(3) 0.071(4) 0.072(4) 0.001(3) 0.024(3) 0.002(3) O13 0.0129(13) 0.0195(15) 0.0173(14) -0.0016(12) 0.0019(11) 0.0031(13) N21 0.0194(17) 0.0159(18) 0.0163(17) -0.0013(14) 0.0011(14) 0.0000(16) C21 0.029(2) 0.018(2) 0.021(2) 0.0019(18) 0.0089(18) -0.008(2) C211 0.055(3) 0.027(3) 0.020(2) 0.003(2) 0.012(2) -0.012(3) C212 0.040(3) 0.031(3) 0.027(2) 0.011(2) -0.002(2) 0.000(2) N22 0.0254(19) 0.0194(19) 0.0185(18) -0.0012(15) 0.0014(15) -0.0106(17) C22 0.013(2) 0.019(2) 0.022(2) 0.001(2) 0.0031(16) 0.005(2) C221 0.028(2) 0.019(2) 0.031(2) 0.0015(19) -0.0001(19) -0.006(2) C222 0.033(2) 0.031(3) 0.019(2) -0.0054(19) 0.0042(19) -0.015(2) C223 0.044(3) 0.034(3) 0.032(3) -0.001(2) -0.010(2) 0.003(3) O23 0.0191(14) 0.0158(15) 0.0160(14) -0.0011(12) 0.0029(11) -0.0027(13) O33 0.0165(14) 0.0158(16) 0.0152(14) -0.0011(12) 0.0035(12) 0.0030(13) N31 0.0146(17) 0.0159(18) 0.0182(17) 0.0002(14) 0.0023(14) 0.0014(16) C31 0.021(2) 0.026(2) 0.017(2) -0.0015(18) -0.0015(17) 0.003(2) C311 0.026(2) 0.035(3) 0.030(2) -0.005(2) -0.004(2) 0.004(2) C312 0.027(2) 0.034(3) 0.024(2) 0.011(2) 0.007(2) 0.010(2) C32 0.015(2) 0.0070(19) 0.020(2) 0.0019(16) 0.0021(17) -0.0050(18) N32 0.0127(16) 0.0161(18) 0.0184(17) -0.0023(14) 0.0056(14) 0.0028(16) C321 0.027(2) 0.025(2) 0.020(2) -0.0037(18) 0.0035(19) 0.003(2) C322 0.024(2) 0.027(3) 0.024(2) -0.0011(19) 0.0099(18) -0.004(2) C323 0.020(2) 0.044(3) 0.053(3) -0.005(3) 0.009(2) 0.003(2) N41 0.0166(17) 0.0149(18) 0.0175(17) -0.0023(14) 0.0032(14) 0.0005(16) C41 0.021(2) 0.016(2) 0.022(2) -0.0046(17) 0.0059(18) -0.006(2) C411 0.031(3) 0.017(2) 0.040(3) -0.007(2) 0.007(2) -0.001(2) C412 0.031(2) 0.025(3) 0.022(2) -0.0054(19) 0.002(2) -0.011(2) N42 0.028(2) 0.024(2) 0.0189(18) 0.0004(15) 0.0072(16) -0.0091(18) C42 0.015(2) 0.016(2) 0.025(2) 0.0037(18) 0.0099(18) 0.001(2) C421 0.046(3) 0.037(3) 0.018(2) 0.004(2) 0.006(2) -0.012(3) C422 0.033(3) 0.025(3) 0.028(2) 0.003(2) 0.009(2) -0.011(2) C423 0.039(3) 0.043(3) 0.046(3) -0.013(3) 0.013(2) -0.009(3) O43 0.0205(14) 0.0167(15) 0.0170(14) -0.0013(12) 0.0036(12) -0.0035(14) _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 Hf1 O23 2.167(2) . ? Hf1 O43 2.182(3) . ? Hf1 O33 2.197(3) . ? Hf1 O13 2.199(2) . ? Hf1 N21 2.263(3) . ? Hf1 N11 2.266(3) . ? Hf1 N41 2.281(3) . ? Hf1 N31 2.293(3) . ? Hf1 C12 2.641(4) . ? Hf1 C22 2.649(4) . ? Hf1 C32 2.662(4) . ? Hf1 C42 2.663(4) . ? N11 C12 1.304(5) . ? N11 C11 1.464(5) . ? C11 C111 1.493(6) . ? C11 C112 1.503(6) . ? C11 H11 1.0000 . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C112 H11D 0.9800 . ? C112 H11E 0.9800 . ? C112 H11F 0.9800 . ? N12 C12 1.386(5) . ? N12 C121 1.461(5) . ? N12 C122 1.549(6) . ? C12 O13 1.297(5) . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C122 C123 1.456(7) . ? C122 H12D 0.9900 . ? C122 H12E 0.9900 . ? C123 H12F 0.9800 . ? C123 H12G 0.9800 . ? C123 H12H 0.9800 . ? N21 C22 1.314(5) . ? N21 C21 1.469(5) . ? C21 C211 1.515(6) . ? C21 C212 1.533(6) . ? C21 H21 1.0000 . ? C211 H21A 0.9800 . ? C211 H21B 0.9800 . ? C211 H21C 0.9800 . ? C212 H21D 0.9800 . ? C212 H21E 0.9800 . ? C212 H21F 0.9800 . ? N22 C22 1.365(5) . ? N22 C221 1.449(5) . ? N22 C222 1.475(5) . ? C22 O23 1.302(4) . ? C221 H22A 0.9800 . ? C221 H22B 0.9800 . ? C221 H22C 0.9800 . ? C222 C223 1.504(6) . ? C222 H22D 0.9900 . ? C222 H22E 0.9900 . ? C223 H22F 0.9800 . ? C223 H22G 0.9800 . ? C223 H22H 0.9800 . ? O33 C32 1.299(4) . ? N31 C32 1.311(5) . ? N31 C31 1.461(5) . ? C31 C312 1.522(6) . ? C31 C311 1.524(6) . ? C31 H31 1.0000 . ? C311 H31A 0.9800 . ? C311 H31B 0.9800 . ? C311 H31C 0.9800 . ? C312 H31D 0.9800 . ? C312 H31E 0.9800 . ? C312 H31F 0.9800 . ? C32 N32 1.381(5) . ? N32 C321 1.459(5) . ? N32 C322 1.460(5) . ? C321 H32A 0.9800 . ? C321 H32B 0.9800 . ? C321 H32C 0.9800 . ? C322 C323 1.515(6) . ? C322 H32D 0.9900 . ? C322 H32E 0.9900 . ? C323 H32F 0.9800 . ? C323 H32G 0.9800 . ? C323 H32H 0.9800 . ? N41 C42 1.322(5) . ? N41 C41 1.472(5) . ? C41 C412 1.519(5) . ? C41 C411 1.523(6) . ? C41 H41 1.0000 . ? C411 H41A 0.9800 . ? C411 H41B 0.9800 . ? C411 H41C 0.9800 . ? C412 H41D 0.9800 . ? C412 H41E 0.9800 . ? C412 H41F 0.9800 . ? N42 C42 1.373(5) . ? N42 C422 1.465(5) . ? N42 C421 1.470(5) . ? C42 O43 1.289(4) . ? C421 H42A 0.9800 . ? C421 H42B 0.9800 . ? C421 H42C 0.9800 . ? C422 C423 1.518(6) . ? C422 H42D 0.9900 . ? C422 H42E 0.9900 . ? C423 H42F 0.9800 . ? C423 H42G 0.9800 . ? C423 H42H 0.9800 . ? 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 O23 Hf1 O43 75.51(10) . . ? O23 Hf1 O33 129.60(9) . . ? O43 Hf1 O33 127.86(10) . . ? O23 Hf1 O13 130.17(10) . . ? O43 Hf1 O13 129.05(9) . . ? O33 Hf1 O13 73.93(9) . . ? O23 Hf1 N21 58.89(10) . . ? O43 Hf1 N21 134.31(11) . . ? O33 Hf1 N21 87.46(10) . . ? O13 Hf1 N21 83.86(10) . . ? O23 Hf1 N11 87.34(10) . . ? O43 Hf1 N11 84.82(11) . . ? O33 Hf1 N11 132.55(10) . . ? O13 Hf1 N11 58.71(10) . . ? N21 Hf1 N11 90.05(12) . . ? O23 Hf1 N41 133.98(10) . . ? O43 Hf1 N41 58.48(10) . . ? O33 Hf1 N41 83.54(10) . . ? O13 Hf1 N41 84.70(10) . . ? N21 Hf1 N41 167.03(11) . . ? N11 Hf1 N41 89.20(12) . . ? O23 Hf1 N31 83.95(10) . . ? O43 Hf1 N31 86.54(10) . . ? O33 Hf1 N31 58.41(10) . . ? O13 Hf1 N31 132.26(10) . . ? N21 Hf1 N31 91.15(11) . . ? N11 Hf1 N31 169.02(11) . . ? N41 Hf1 N31 92.05(12) . . ? O23 Hf1 C12 111.74(11) . . ? O43 Hf1 C12 106.64(11) . . ? O33 Hf1 C12 102.97(11) . . ? O13 Hf1 C12 29.30(11) . . ? N21 Hf1 C12 88.83(11) . . ? N11 Hf1 C12 29.58(12) . . ? N41 Hf1 C12 84.14(11) . . ? N31 Hf1 C12 161.36(12) . . ? O23 Hf1 C22 29.23(10) . . ? O43 Hf1 C22 104.59(11) . . ? O33 Hf1 C22 111.09(11) . . ? O13 Hf1 C22 107.30(11) . . ? N21 Hf1 C22 29.72(11) . . ? N11 Hf1 C22 87.00(11) . . ? N41 Hf1 C22 162.94(11) . . ? N31 Hf1 C22 88.64(11) . . ? C12 Hf1 C22 100.33(12) . . ? O23 Hf1 C32 106.63(10) . . ? O43 Hf1 C32 110.09(10) . . ? O33 Hf1 C32 29.05(10) . . ? O13 Hf1 C32 102.77(10) . . ? N21 Hf1 C32 87.07(11) . . ? N11 Hf1 C32 161.47(11) . . ? N41 Hf1 C32 89.54(11) . . ? N31 Hf1 C32 29.50(11) . . ? C12 Hf1 C32 131.97(12) . . ? C22 Hf1 C32 99.24(11) . . ? O23 Hf1 C42 104.22(11) . . ? O43 Hf1 C42 28.73(10) . . ? O33 Hf1 C42 106.58(12) . . ? O13 Hf1 C42 108.85(11) . . ? N21 Hf1 C42 163.02(12) . . ? N11 Hf1 C42 87.33(12) . . ? N41 Hf1 C42 29.77(11) . . ? N31 Hf1 C42 88.34(11) . . ? C12 Hf1 C42 97.01(12) . . ? C22 Hf1 C42 133.31(12) . . ? C32 Hf1 C42 100.53(11) . . ? C12 N11 C11 125.0(3) . . ? C12 N11 Hf1 91.4(2) . . ? C11 N11 Hf1 143.5(3) . . ? N11 C11 C111 110.4(4) . . ? N11 C11 C112 110.4(3) . . ? C111 C11 C112 113.4(4) . . ? N11 C11 H11 107.4 . . ? C111 C11 H11 107.4 . . ? C112 C11 H11 107.4 . . ? C11 C111 H11A 109.5 . . ? C11 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C11 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C11 C112 H11D 109.5 . . ? C11 C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? C11 C112 H11F 109.5 . . ? H11D C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? C12 N12 C121 115.8(3) . . ? C12 N12 C122 114.8(3) . . ? C121 N12 C122 112.5(4) . . ? O13 C12 N11 114.7(3) . . ? O13 C12 N12 117.7(4) . . ? N11 C12 N12 127.6(4) . . ? O13 C12 Hf1 56.09(18) . . ? N11 C12 Hf1 59.1(2) . . ? N12 C12 Hf1 168.9(3) . . ? N12 C121 H12A 109.5 . . ? N12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? N12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C123 C122 N12 112.3(4) . . ? C123 C122 H12D 109.1 . . ? N12 C122 H12D 109.1 . . ? C123 C122 H12E 109.1 . . ? N12 C122 H12E 109.1 . . ? H12D C122 H12E 107.9 . . ? C122 C123 H12F 109.5 . . ? C122 C123 H12G 109.5 . . ? H12F C123 H12G 109.5 . . ? C122 C123 H12H 109.5 . . ? H12F C123 H12H 109.5 . . ? H12G C123 H12H 109.5 . . ? C12 O13 Hf1 94.6(2) . . ? C22 N21 C21 127.1(3) . . ? C22 N21 Hf1 91.6(3) . . ? C21 N21 Hf1 140.2(2) . . ? N21 C21 C211 108.9(3) . . ? N21 C21 C212 111.1(3) . . ? C211 C21 C212 110.6(4) . . ? N21 C21 H21 108.7 . . ? C211 C21 H21 108.7 . . ? C212 C21 H21 108.7 . . ? C21 C211 H21A 109.5 . . ? C21 C211 H21B 109.5 . . ? H21A C211 H21B 109.5 . . ? C21 C211 H21C 109.5 . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? C21 C212 H21D 109.5 . . ? C21 C212 H21E 109.5 . . ? H21D C212 H21E 109.5 . . ? C21 C212 H21F 109.5 . . ? H21D C212 H21F 109.5 . . ? H21E C212 H21F 109.5 . . ? C22 N22 C221 126.6(3) . . ? C22 N22 C222 118.8(3) . . ? C221 N22 C222 113.9(3) . . ? O23 C22 N21 112.9(4) . . ? O23 C22 N22 116.8(3) . . ? N21 C22 N22 130.3(4) . . ? O23 C22 Hf1 54.40(18) . . ? N21 C22 Hf1 58.7(2) . . ? N22 C22 Hf1 169.5(3) . . ? N22 C221 H22A 109.5 . . ? N22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? N22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? N22 C222 C223 113.3(4) . . ? N22 C222 H22D 108.9 . . ? C223 C222 H22D 108.9 . . ? N22 C222 H22E 108.9 . . ? C223 C222 H22E 108.9 . . ? H22D C222 H22E 107.7 . . ? C222 C223 H22F 109.5 . . ? C222 C223 H22G 109.5 . . ? H22F C223 H22G 109.5 . . ? C222 C223 H22H 109.5 . . ? H22F C223 H22H 109.5 . . ? H22G C223 H22H 109.5 . . ? C22 O23 Hf1 96.4(2) . . ? C32 O33 Hf1 95.7(2) . . ? C32 N31 C31 125.0(3) . . ? C32 N31 Hf1 91.1(2) . . ? C31 N31 Hf1 143.8(2) . . ? N31 C31 C312 109.5(3) . . ? N31 C31 C311 110.3(3) . . ? C312 C31 C311 110.7(3) . . ? N31 C31 H31 108.8 . . ? C312 C31 H31 108.8 . . ? C311 C31 H31 108.8 . . ? C31 C311 H31A 109.5 . . ? C31 C311 H31B 109.5 . . ? H31A C311 H31B 109.5 . . ? C31 C311 H31C 109.5 . . ? H31A C311 H31C 109.5 . . ? H31B C311 H31C 109.5 . . ? C31 C312 H31D 109.5 . . ? C31 C312 H31E 109.5 . . ? H31D C312 H31E 109.5 . . ? C31 C312 H31F 109.5 . . ? H31D C312 H31F 109.5 . . ? H31E C312 H31F 109.5 . . ? O33 C32 N31 114.3(3) . . ? O33 C32 N32 118.3(3) . . ? N31 C32 N32 127.4(3) . . ? O33 C32 Hf1 55.20(18) . . ? N31 C32 Hf1 59.4(2) . . ? N32 C32 Hf1 172.1(3) . . ? C32 N32 C321 115.4(3) . . ? C32 N32 C322 118.7(3) . . ? C321 N32 C322 112.5(3) . . ? N32 C321 H32A 109.5 . . ? N32 C321 H32B 109.5 . . ? H32A C321 H32B 109.5 . . ? N32 C321 H32C 109.5 . . ? H32A C321 H32C 109.5 . . ? H32B C321 H32C 109.5 . . ? N32 C322 C323 113.6(3) . . ? N32 C322 H32D 108.9 . . ? C323 C322 H32D 108.9 . . ? N32 C322 H32E 108.9 . . ? C323 C322 H32E 108.9 . . ? H32D C322 H32E 107.7 . . ? C322 C323 H32F 109.5 . . ? C322 C323 H32G 109.5 . . ? H32F C323 H32G 109.5 . . ? C322 C323 H32H 109.5 . . ? H32F C323 H32H 109.5 . . ? H32G C323 H32H 109.5 . . ? C42 N41 C41 126.6(3) . . ? C42 N41 Hf1 91.3(2) . . ? C41 N41 Hf1 140.0(2) . . ? N41 C41 C412 109.5(3) . . ? N41 C41 C411 109.9(3) . . ? C412 C41 C411 111.2(3) . . ? N41 C41 H41 108.8 . . ? C412 C41 H41 108.8 . . ? C411 C41 H41 108.8 . . ? C41 C411 H41A 109.5 . . ? C41 C411 H41B 109.5 . . ? H41A C411 H41B 109.5 . . ? C41 C411 H41C 109.5 . . ? H41A C411 H41C 109.5 . . ? H41B C411 H41C 109.5 . . ? C41 C412 H41D 109.5 . . ? C41 C412 H41E 109.5 . . ? H41D C412 H41E 109.5 . . ? C41 C412 H41F 109.5 . . ? H41D C412 H41F 109.5 . . ? H41E C412 H41F 109.5 . . ? C42 N42 C422 124.1(3) . . ? C42 N42 C421 115.7(3) . . ? C422 N42 C421 113.8(3) . . ? O43 C42 N41 113.3(3) . . ? O43 C42 N42 116.9(4) . . ? N41 C42 N42 129.7(4) . . ? O43 C42 Hf1 54.46(18) . . ? N41 C42 Hf1 58.9(2) . . ? N42 C42 Hf1 170.5(3) . . ? N42 C421 H42A 109.5 . . ? N42 C421 H42B 109.5 . . ? H42A C421 H42B 109.5 . . ? N42 C421 H42C 109.5 . . ? H42A C421 H42C 109.5 . . ? H42B C421 H42C 109.5 . . ? N42 C422 C423 112.1(4) . . ? N42 C422 H42D 109.2 . . ? C423 C422 H42D 109.2 . . ? N42 C422 H42E 109.2 . . ? C423 C422 H42E 109.2 . . ? H42D C422 H42E 107.9 . . ? C422 C423 H42F 109.5 . . ? C422 C423 H42G 109.5 . . ? H42F C423 H42G 109.5 . . ? C422 C423 H42H 109.5 . . ? H42F C423 H42H 109.5 . . ? H42G C423 H42H 109.5 . . ? C42 O43 Hf1 96.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O23 Hf1 N11 C12 146.4(2) . . . . ? O43 Hf1 N11 C12 -137.9(2) . . . . ? O33 Hf1 N11 C12 1.0(3) . . . . ? O13 Hf1 N11 C12 4.8(2) . . . . ? N21 Hf1 N11 C12 87.5(2) . . . . ? N41 Hf1 N11 C12 -79.5(2) . . . . ? N31 Hf1 N11 C12 -176.2(5) . . . . ? C22 Hf1 N11 C12 117.1(2) . . . . ? C32 Hf1 N11 C12 6.7(5) . . . . ? C42 Hf1 N11 C12 -109.2(3) . . . . ? O23 Hf1 N11 C11 -28.4(4) . . . . ? O43 Hf1 N11 C11 47.3(4) . . . . ? O33 Hf1 N11 C11 -173.8(4) . . . . ? O13 Hf1 N11 C11 -170.0(5) . . . . ? N21 Hf1 N11 C11 -87.2(4) . . . . ? N41 Hf1 N11 C11 105.7(4) . . . . ? N31 Hf1 N11 C11 9.1(9) . . . . ? C12 Hf1 N11 C11 -174.8(6) . . . . ? C22 Hf1 N11 C11 -57.6(4) . . . . ? C32 Hf1 N11 C11 -168.1(4) . . . . ? C42 Hf1 N11 C11 76.0(4) . . . . ? C12 N11 C11 C111 126.2(5) . . . . ? Hf1 N11 C11 C111 -60.2(6) . . . . ? C12 N11 C11 C112 -107.6(5) . . . . ? Hf1 N11 C11 C112 66.0(5) . . . . ? C11 N11 C12 O13 168.6(3) . . . . ? Hf1 N11 C12 O13 -7.6(3) . . . . ? C11 N11 C12 N12 -14.6(7) . . . . ? Hf1 N11 C12 N12 169.2(4) . . . . ? C11 N11 C12 Hf1 176.2(4) . . . . ? C121 N12 C12 O13 -10.1(6) . . . . ? C122 N12 C12 O13 123.5(4) . . . . ? C121 N12 C12 N11 173.1(4) . . . . ? C122 N12 C12 N11 -53.3(6) . . . . ? C121 N12 C12 Hf1 -63.3(16) . . . . ? C122 N12 C12 Hf1 70.3(16) . . . . ? O23 Hf1 C12 O13 135.1(2) . . . . ? O43 Hf1 C12 O13 -144.2(2) . . . . ? O33 Hf1 C12 O13 -7.6(2) . . . . ? N21 Hf1 C12 O13 79.5(2) . . . . ? N11 Hf1 C12 O13 171.7(4) . . . . ? N41 Hf1 C12 O13 -89.6(2) . . . . ? N31 Hf1 C12 O13 -10.6(5) . . . . ? C22 Hf1 C12 O13 107.0(2) . . . . ? C32 Hf1 C12 O13 -5.5(3) . . . . ? C42 Hf1 C12 O13 -116.5(2) . . . . ? O23 Hf1 C12 N11 -36.5(3) . . . . ? O43 Hf1 C12 N11 44.2(3) . . . . ? O33 Hf1 C12 N11 -179.3(2) . . . . ? O13 Hf1 C12 N11 -171.7(4) . . . . ? N21 Hf1 C12 N11 -92.2(2) . . . . ? N41 Hf1 C12 N11 98.8(2) . . . . ? N31 Hf1 C12 N11 177.7(3) . . . . ? C22 Hf1 C12 N11 -64.6(2) . . . . ? C32 Hf1 C12 N11 -177.2(2) . . . . ? C42 Hf1 C12 N11 71.8(3) . . . . ? O23 Hf1 C12 N12 -166.2(15) . . . . ? O43 Hf1 C12 N12 -85.5(15) . . . . ? O33 Hf1 C12 N12 51.1(15) . . . . ? O13 Hf1 C12 N12 58.7(15) . . . . ? N21 Hf1 C12 N12 138.2(15) . . . . ? N11 Hf1 C12 N12 -129.7(16) . . . . ? N41 Hf1 C12 N12 -30.9(15) . . . . ? N31 Hf1 C12 N12 48.1(17) . . . . ? C22 Hf1 C12 N12 165.7(15) . . . . ? C32 Hf1 C12 N12 53.2(16) . . . . ? C42 Hf1 C12 N12 -57.8(15) . . . . ? C12 N12 C122 C123 147.1(4) . . . . ? C121 N12 C122 C123 -77.8(5) . . . . ? N11 C12 O13 Hf1 7.9(4) . . . . ? N12 C12 O13 Hf1 -169.3(3) . . . . ? O23 Hf1 O13 C12 -59.1(3) . . . . ? O43 Hf1 O13 C12 46.2(3) . . . . ? O33 Hf1 O13 C12 172.3(2) . . . . ? N21 Hf1 O13 C12 -98.6(2) . . . . ? N11 Hf1 O13 C12 -4.8(2) . . . . ? N41 Hf1 O13 C12 87.5(2) . . . . ? N31 Hf1 O13 C12 175.4(2) . . . . ? C22 Hf1 O13 C12 -80.1(2) . . . . ? C32 Hf1 O13 C12 175.8(2) . . . . ? C42 Hf1 O13 C12 69.8(2) . . . . ? O23 Hf1 N21 C22 -3.0(2) . . . . ? O43 Hf1 N21 C22 1.1(3) . . . . ? O33 Hf1 N21 C22 -143.5(2) . . . . ? O13 Hf1 N21 C22 142.4(2) . . . . ? N11 Hf1 N21 C22 83.9(2) . . . . ? N41 Hf1 N21 C22 170.5(4) . . . . ? N31 Hf1 N21 C22 -85.2(2) . . . . ? C12 Hf1 N21 C22 113.4(2) . . . . ? C32 Hf1 N21 C22 -114.5(2) . . . . ? C42 Hf1 N21 C22 2.9(5) . . . . ? O23 Hf1 N21 C21 -170.9(4) . . . . ? O43 Hf1 N21 C21 -166.8(3) . . . . ? O33 Hf1 N21 C21 48.6(4) . . . . ? O13 Hf1 N21 C21 -25.5(4) . . . . ? N11 Hf1 N21 C21 -84.0(4) . . . . ? N41 Hf1 N21 C21 2.6(8) . . . . ? N31 Hf1 N21 C21 106.9(4) . . . . ? C12 Hf1 N21 C21 -54.4(4) . . . . ? C22 Hf1 N21 C21 -167.9(5) . . . . ? C32 Hf1 N21 C21 77.7(4) . . . . ? C42 Hf1 N21 C21 -165.0(4) . . . . ? C22 N21 C21 C211 152.8(4) . . . . ? Hf1 N21 C21 C211 -42.5(5) . . . . ? C22 N21 C21 C212 -85.1(5) . . . . ? Hf1 N21 C21 C212 79.6(5) . . . . ? C21 N21 C22 O23 174.9(3) . . . . ? Hf1 N21 C22 O23 4.7(3) . . . . ? C21 N21 C22 N22 -2.9(7) . . . . ? Hf1 N21 C22 N22 -173.2(4) . . . . ? C21 N21 C22 Hf1 170.3(4) . . . . ? C221 N22 C22 O23 180.0(3) . . . . ? C222 N22 C22 O23 9.9(5) . . . . ? C221 N22 C22 N21 -2.3(7) . . . . ? C222 N22 C22 N21 -172.3(4) . . . . ? C221 N22 C22 Hf1 -148.6(13) . . . . ? C222 N22 C22 Hf1 41.4(16) . . . . ? O43 Hf1 C22 O23 6.1(2) . . . . ? O33 Hf1 C22 O23 -135.2(2) . . . . ? O13 Hf1 C22 O23 145.8(2) . . . . ? N21 Hf1 C22 O23 -174.7(4) . . . . ? N11 Hf1 C22 O23 89.9(2) . . . . ? N41 Hf1 C22 O23 12.5(5) . . . . ? N31 Hf1 C22 O23 -80.0(2) . . . . ? C12 Hf1 C22 O23 116.4(2) . . . . ? C32 Hf1 C22 O23 -107.6(2) . . . . ? C42 Hf1 C22 O23 6.4(3) . . . . ? O23 Hf1 C22 N21 174.7(4) . . . . ? O43 Hf1 C22 N21 -179.2(2) . . . . ? O33 Hf1 C22 N21 39.5(2) . . . . ? O13 Hf1 C22 N21 -39.5(2) . . . . ? N11 Hf1 C22 N21 -95.4(2) . . . . ? N41 Hf1 C22 N21 -172.7(3) . . . . ? N31 Hf1 C22 N21 94.7(2) . . . . ? C12 Hf1 C22 N21 -68.8(2) . . . . ? C32 Hf1 C22 N21 67.1(2) . . . . ? C42 Hf1 C22 N21 -178.9(2) . . . . ? O23 Hf1 C22 N22 -35.0(14) . . . . ? O43 Hf1 C22 N22 -28.9(15) . . . . ? O33 Hf1 C22 N22 -170.2(14) . . . . ? O13 Hf1 C22 N22 110.8(15) . . . . ? N21 Hf1 C22 N22 150.3(16) . . . . ? N11 Hf1 C22 N22 54.9(15) . . . . ? N41 Hf1 C22 N22 -22.4(17) . . . . ? N31 Hf1 C22 N22 -115.0(15) . . . . ? C12 Hf1 C22 N22 81.5(15) . . . . ? C32 Hf1 C22 N22 -142.6(15) . . . . ? C42 Hf1 C22 N22 -28.6(15) . . . . ? C22 N22 C222 C223 104.4(4) . . . . ? C221 N22 C222 C223 -66.9(5) . . . . ? N21 C22 O23 Hf1 -4.9(3) . . . . ? N22 C22 O23 Hf1 173.3(3) . . . . ? O43 Hf1 O23 C22 -173.9(2) . . . . ? O33 Hf1 O23 C22 58.5(2) . . . . ? O13 Hf1 O23 C22 -44.6(2) . . . . ? N21 Hf1 O23 C22 3.1(2) . . . . ? N11 Hf1 O23 C22 -88.6(2) . . . . ? N41 Hf1 O23 C22 -174.9(2) . . . . ? N31 Hf1 O23 C22 98.1(2) . . . . ? C12 Hf1 O23 C22 -71.5(2) . . . . ? C32 Hf1 O23 C22 79.0(2) . . . . ? C42 Hf1 O23 C22 -175.2(2) . . . . ? O23 Hf1 O33 C32 43.6(2) . . . . ? O43 Hf1 O33 C32 -59.8(2) . . . . ? O13 Hf1 O33 C32 172.9(2) . . . . ? N21 Hf1 O33 C32 88.5(2) . . . . ? N11 Hf1 O33 C32 176.3(2) . . . . ? N41 Hf1 O33 C32 -100.8(2) . . . . ? N31 Hf1 O33 C32 -4.4(2) . . . . ? C12 Hf1 O33 C32 176.8(2) . . . . ? C22 Hf1 O33 C32 70.1(2) . . . . ? C42 Hf1 O33 C32 -81.8(2) . . . . ? O23 Hf1 N31 C32 -140.5(2) . . . . ? O43 Hf1 N31 C32 143.7(2) . . . . ? O33 Hf1 N31 C32 4.3(2) . . . . ? O13 Hf1 N31 C32 0.7(3) . . . . ? N21 Hf1 N31 C32 -82.0(2) . . . . ? N11 Hf1 N31 C32 -178.2(5) . . . . ? N41 Hf1 N31 C32 85.4(2) . . . . ? C12 Hf1 N31 C32 7.8(5) . . . . ? C22 Hf1 N31 C32 -111.6(2) . . . . ? C42 Hf1 N31 C32 115.0(2) . . . . ? O23 Hf1 N31 C31 44.4(4) . . . . ? O43 Hf1 N31 C31 -31.4(4) . . . . ? O33 Hf1 N31 C31 -170.8(5) . . . . ? O13 Hf1 N31 C31 -174.3(4) . . . . ? N21 Hf1 N31 C31 102.9(4) . . . . ? N11 Hf1 N31 C31 6.7(9) . . . . ? N41 Hf1 N31 C31 -89.6(4) . . . . ? C12 Hf1 N31 C31 -167.3(4) . . . . ? C22 Hf1 N31 C31 73.3(4) . . . . ? C32 Hf1 N31 C31 -175.1(6) . . . . ? C42 Hf1 N31 C31 -60.1(4) . . . . ? C32 N31 C31 C312 -118.3(4) . . . . ? Hf1 N31 C31 C312 55.6(5) . . . . ? C32 N31 C31 C311 119.6(4) . . . . ? Hf1 N31 C31 C311 -66.4(5) . . . . ? Hf1 O33 C32 N31 7.2(3) . . . . ? Hf1 O33 C32 N32 -174.6(3) . . . . ? C31 N31 C32 O33 169.6(3) . . . . ? Hf1 N31 C32 O33 -6.8(3) . . . . ? C31 N31 C32 N32 -8.4(6) . . . . ? Hf1 N31 C32 N32 175.1(4) . . . . ? C31 N31 C32 Hf1 176.4(4) . . . . ? O23 Hf1 C32 O33 -146.3(2) . . . . ? O43 Hf1 C32 O33 133.4(2) . . . . ? O13 Hf1 C32 O33 -7.0(2) . . . . ? N21 Hf1 C32 O33 -90.0(2) . . . . ? N11 Hf1 C32 O33 -8.7(5) . . . . ? N41 Hf1 C32 O33 77.4(2) . . . . ? N31 Hf1 C32 O33 172.4(4) . . . . ? C12 Hf1 C32 O33 -4.3(3) . . . . ? C22 Hf1 C32 O33 -117.3(2) . . . . ? C42 Hf1 C32 O33 105.3(2) . . . . ? O23 Hf1 C32 N31 41.3(2) . . . . ? O43 Hf1 C32 N31 -39.0(2) . . . . ? O33 Hf1 C32 N31 -172.4(4) . . . . ? O13 Hf1 C32 N31 -179.4(2) . . . . ? N21 Hf1 C32 N31 97.5(2) . . . . ? N11 Hf1 C32 N31 178.9(3) . . . . ? N41 Hf1 C32 N31 -95.0(2) . . . . ? C12 Hf1 C32 N31 -176.7(2) . . . . ? C22 Hf1 C32 N31 70.3(2) . . . . ? C42 Hf1 C32 N31 -67.2(2) . . . . ? O23 Hf1 C32 N32 -109.3(19) . . . . ? O43 Hf1 C32 N32 170.4(19) . . . . ? O33 Hf1 C32 N32 37.0(18) . . . . ? O13 Hf1 C32 N32 30.0(19) . . . . ? N21 Hf1 C32 N32 -53.1(19) . . . . ? N11 Hf1 C32 N32 28(2) . . . . ? N41 Hf1 C32 N32 114.4(19) . . . . ? N31 Hf1 C32 N32 -151(2) . . . . ? C12 Hf1 C32 N32 32.7(19) . . . . ? C22 Hf1 C32 N32 -80.3(19) . . . . ? C42 Hf1 C32 N32 142.2(19) . . . . ? O33 C32 N32 C321 -7.8(5) . . . . ? N31 C32 N32 C321 170.1(4) . . . . ? Hf1 C32 N32 C321 -42(2) . . . . ? O33 C32 N32 C322 130.1(4) . . . . ? N31 C32 N32 C322 -51.9(5) . . . . ? Hf1 C32 N32 C322 96.0(19) . . . . ? C32 N32 C322 C323 140.2(4) . . . . ? C321 N32 C322 C323 -80.7(4) . . . . ? O23 Hf1 N41 C42 -0.5(3) . . . . ? O43 Hf1 N41 C42 -1.6(2) . . . . ? O33 Hf1 N41 C42 140.9(2) . . . . ? O13 Hf1 N41 C42 -144.7(2) . . . . ? N21 Hf1 N41 C42 -172.8(4) . . . . ? N11 Hf1 N41 C42 -86.0(2) . . . . ? N31 Hf1 N41 C42 83.1(2) . . . . ? C12 Hf1 N41 C42 -115.2(2) . . . . ? C22 Hf1 N41 C42 -9.0(5) . . . . ? C32 Hf1 N41 C42 112.5(2) . . . . ? O23 Hf1 N41 C41 -162.9(3) . . . . ? O43 Hf1 N41 C41 -164.0(4) . . . . ? O33 Hf1 N41 C41 -21.4(4) . . . . ? O13 Hf1 N41 C41 53.0(4) . . . . ? N21 Hf1 N41 C41 24.9(7) . . . . ? N11 Hf1 N41 C41 111.6(4) . . . . ? N31 Hf1 N41 C41 -79.3(4) . . . . ? C12 Hf1 N41 C41 82.4(4) . . . . ? C22 Hf1 N41 C41 -171.3(4) . . . . ? C32 Hf1 N41 C41 -49.9(4) . . . . ? C42 Hf1 N41 C41 -162.4(5) . . . . ? C42 N41 C41 C412 165.4(4) . . . . ? Hf1 N41 C41 C412 -36.8(5) . . . . ? C42 N41 C41 C411 -72.2(5) . . . . ? Hf1 N41 C41 C411 85.6(4) . . . . ? C41 N41 C42 O43 168.5(3) . . . . ? Hf1 N41 C42 O43 2.5(3) . . . . ? C41 N41 C42 N42 -9.2(7) . . . . ? Hf1 N41 C42 N42 -175.1(4) . . . . ? C41 N41 C42 Hf1 166.0(4) . . . . ? C422 N42 C42 O43 158.3(3) . . . . ? C421 N42 C42 O43 8.1(5) . . . . ? C422 N42 C42 N41 -24.1(6) . . . . ? C421 N42 C42 N41 -174.3(4) . . . . ? C422 N42 C42 Hf1 -177.9(15) . . . . ? C421 N42 C42 Hf1 31.9(19) . . . . ? O23 Hf1 C42 O43 2.5(2) . . . . ? O33 Hf1 C42 O43 142.1(2) . . . . ? O13 Hf1 C42 O43 -139.7(2) . . . . ? N21 Hf1 C42 O43 -2.7(5) . . . . ? N11 Hf1 C42 O43 -84.1(2) . . . . ? N41 Hf1 C42 O43 -177.1(4) . . . . ? N31 Hf1 C42 O43 85.8(2) . . . . ? C12 Hf1 C42 O43 -112.1(2) . . . . ? C22 Hf1 C42 O43 -0.7(3) . . . . ? C32 Hf1 C42 O43 112.8(2) . . . . ? O23 Hf1 C42 N41 179.6(2) . . . . ? O43 Hf1 C42 N41 177.1(4) . . . . ? O33 Hf1 C42 N41 -40.8(2) . . . . ? O13 Hf1 C42 N41 37.5(2) . . . . ? N21 Hf1 C42 N41 174.4(3) . . . . ? N11 Hf1 C42 N41 93.0(2) . . . . ? N31 Hf1 C42 N41 -97.0(2) . . . . ? C12 Hf1 C42 N41 65.0(2) . . . . ? C22 Hf1 C42 N41 176.4(2) . . . . ? C32 Hf1 C42 N41 -70.0(2) . . . . ? O23 Hf1 C42 N42 -23.8(18) . . . . ? O43 Hf1 C42 N42 -26.3(16) . . . . ? O33 Hf1 C42 N42 115.8(17) . . . . ? O13 Hf1 C42 N42 -165.9(17) . . . . ? N21 Hf1 C42 N42 -29(2) . . . . ? N11 Hf1 C42 N42 -110.3(17) . . . . ? N41 Hf1 C42 N42 156.6(19) . . . . ? N31 Hf1 C42 N42 59.6(17) . . . . ? C12 Hf1 C42 N42 -138.3(17) . . . . ? C22 Hf1 C42 N42 -27.0(18) . . . . ? C32 Hf1 C42 N42 86.6(17) . . . . ? C42 N42 C422 C423 -65.5(5) . . . . ? C421 N42 C422 C423 85.2(4) . . . . ? N41 C42 O43 Hf1 -2.7(3) . . . . ? N42 C42 O43 Hf1 175.3(3) . . . . ? O23 Hf1 O43 C42 -177.5(2) . . . . ? O33 Hf1 O43 C42 -48.2(2) . . . . ? O13 Hf1 O43 C42 52.1(2) . . . . ? N21 Hf1 O43 C42 178.9(2) . . . . ? N11 Hf1 O43 C42 93.9(2) . . . . ? N41 Hf1 O43 C42 1.7(2) . . . . ? N31 Hf1 O43 C42 -92.9(2) . . . . ? C12 Hf1 O43 C42 73.7(2) . . . . ? C22 Hf1 O43 C42 179.4(2) . . . . ? C32 Hf1 O43 C42 -74.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.384 _refine_diff_density_min -2.040 _refine_diff_density_rms 0.117 #=================================END