# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_mjs111_0m_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 911093' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C42 H42 Hf N2 P2 S' _chemical_formula_weight 847.27 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.2238(4) _cell_length_b 11.1436(5) _cell_length_c 11.2447(6) _cell_angle_alpha 108.516(2) _cell_angle_beta 111.217(2) _cell_angle_gamma 105.005(3) _cell_volume 925.82(8) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9971 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 27.49 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 426 _exptl_absorpt_coefficient_mu 2.992 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5860 _exptl_absorpt_correction_T_max 0.7958 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17662 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7772 _reflns_number_gt 7763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(3) _refine_ls_number_reflns 7772 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0198 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0373 _refine_ls_wR_factor_gt 0.0373 _refine_ls_goodness_of_fit_ref 0.793 _refine_ls_restrained_S_all 0.793 _refine_ls_shift/su_max 0.003 _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 0.4661 0.2740 0.4764 0.01808(3) Uani 1 1 d . . . S1 S 0.23651(10) 0.30290(9) 0.59235(9) 0.02509(16) Uani 1 1 d . . . P1 P 0.63576(10) 0.59398(8) 0.60521(8) 0.02279(16) Uani 1 1 d . . . P2 P 0.27538(9) 0.09667(8) 0.19447(8) 0.01972(15) Uani 1 1 d . . . N1 N 0.4424(3) 0.4561(3) 0.4937(3) 0.0238(5) Uani 1 1 d . . . N2 N 0.2174(3) 0.1316(2) 0.3207(2) 0.0203(5) Uani 1 1 d . . . C1 C 0.6376(4) 0.7040(3) 0.5145(3) 0.0219(6) Uani 1 1 d . . . C2 C 0.6162(4) 0.6940(3) 0.7591(3) 0.0230(6) Uani 1 1 d . . . C3 C 0.1761(4) 0.1574(3) 0.0676(3) 0.0206(6) Uani 1 1 d . . . C4 C 0.1832(4) -0.0918(3) 0.0873(3) 0.0234(6) Uani 1 1 d . . . C5 C 0.2785(4) 0.4679(3) 0.4545(3) 0.0268(6) Uani 1 1 d . . . H5A H 0.1957 0.3997 0.3530 0.032 Uiso 1 1 calc R . . H5B H 0.2962 0.5627 0.4639 0.032 Uiso 1 1 calc R . . C6 C 0.2041(4) 0.4408(3) 0.5502(4) 0.0279(7) Uani 1 1 d . . . H6A H 0.0795 0.4157 0.5012 0.033 Uiso 1 1 calc R . . H6B H 0.2583 0.5279 0.6407 0.033 Uiso 1 1 calc R . . C7 C 0.0455(4) 0.1055(3) 0.3027(3) 0.0264(6) Uani 1 1 d . . . H7A H -0.0325 0.0056 0.2376 0.032 Uiso 1 1 calc R . . H7B H 0.0002 0.1615 0.2594 0.032 Uiso 1 1 calc R . . C8 C 0.0524(4) 0.1448(3) 0.4477(3) 0.0287(7) Uani 1 1 d . . . H8A H 0.0530 0.0669 0.4720 0.034 Uiso 1 1 calc R . . H8B H -0.0531 0.1562 0.4400 0.034 Uiso 1 1 calc R . . C9 C 0.5301(4) 0.6511(3) 0.3690(3) 0.0266(6) Uani 1 1 d . . . H9A H 0.4475 0.5565 0.3157 0.032 Uiso 1 1 calc R . . C10 C 0.5408(4) 0.7338(3) 0.2991(3) 0.0301(7) Uani 1 1 d . . . H10A H 0.4656 0.6961 0.1993 0.036 Uiso 1 1 calc R . . C11 C 0.6618(4) 0.8713(3) 0.3761(4) 0.0321(7) Uani 1 1 d . . . H11A H 0.6692 0.9285 0.3295 0.039 Uiso 1 1 calc R . . C12 C 0.7721(4) 0.9256(3) 0.5213(3) 0.0322(7) Uani 1 1 d . . . H12A H 0.8561 1.0196 0.5740 0.039 Uiso 1 1 calc R . . C13 C 0.7598(4) 0.8425(3) 0.5892(3) 0.0266(6) Uani 1 1 d . . . H13A H 0.8361 0.8805 0.6888 0.032 Uiso 1 1 calc R . . C14 C 0.5513(4) 0.7943(3) 0.7680(3) 0.0252(6) Uani 1 1 d . . . H14A H 0.5255 0.8235 0.6952 0.030 Uiso 1 1 calc R . . C15 C 0.5239(4) 0.8518(3) 0.8825(4) 0.0305(7) Uani 1 1 d . . . H15A H 0.4788 0.9198 0.8875 0.037 Uiso 1 1 calc R . . C16 C 0.5617(5) 0.8107(4) 0.9887(4) 0.0367(8) Uani 1 1 d . . . H16A H 0.5397 0.8486 1.0654 0.044 Uiso 1 1 calc R . . C17 C 0.6315(5) 0.7147(4) 0.9851(4) 0.0416(9) Uani 1 1 d . . . H17A H 0.6601 0.6884 1.0601 0.050 Uiso 1 1 calc R . . C18 C 0.6596(5) 0.6567(4) 0.8706(3) 0.0321(7) Uani 1 1 d . . . H18A H 0.7086 0.5913 0.8683 0.039 Uiso 1 1 calc R . . C19 C 0.2808(4) 0.2675(3) 0.0623(3) 0.0269(6) Uani 1 1 d . . . H19A H 0.4015 0.3078 0.1226 0.032 Uiso 1 1 calc R . . C20 C 0.2106(5) 0.3196(3) -0.0304(4) 0.0372(8) Uani 1 1 d . . . H20A H 0.2832 0.3939 -0.0350 0.045 Uiso 1 1 calc R . . C21 C 0.0354(5) 0.2628(4) -0.1156(4) 0.0371(8) Uani 1 1 d . . . H21A H -0.0126 0.2980 -0.1794 0.045 Uiso 1 1 calc R . . C22 C -0.0722(4) 0.1542(3) -0.1091(3) 0.0316(7) Uani 1 1 d . . . H22A H -0.1932 0.1173 -0.1660 0.038 Uiso 1 1 calc R . . C23 C -0.0014(4) 0.1006(3) -0.0190(3) 0.0259(6) Uani 1 1 d . . . H23A H -0.0739 0.0248 -0.0162 0.031 Uiso 1 1 calc R . . C24 C 0.1616(4) -0.1494(4) -0.0513(4) 0.0348(8) Uani 1 1 d . . . H24A H 0.1870 -0.0901 -0.0928 0.042 Uiso 1 1 calc R . . C25 C 0.1034(5) -0.2921(4) -0.1286(4) 0.0485(10) Uani 1 1 d . . . H25A H 0.0884 -0.3305 -0.2230 0.058 Uiso 1 1 calc R . . C26 C 0.0674(6) -0.3782(4) -0.0693(5) 0.0570(12) Uani 1 1 d . . . H26A H 0.0280 -0.4760 -0.1224 0.068 Uiso 1 1 calc R . . C27 C 0.0883(5) -0.3228(4) 0.0681(5) 0.0548(11) Uani 1 1 d . . . H27A H 0.0628 -0.3828 0.1088 0.066 Uiso 1 1 calc R . . C28 C 0.1463(4) -0.1801(4) 0.1459(4) 0.0369(8) Uani 1 1 d . . . H28A H 0.1608 -0.1425 0.2401 0.044 Uiso 1 1 calc R . . C29 C 0.5773(4) 0.2263(4) 0.6648(4) 0.0338(8) Uani 1 1 d . . . H29A H 0.6764 0.2058 0.6676 0.041 Uiso 1 1 calc R . . H29B H 0.6185 0.3090 0.7559 0.041 Uiso 1 1 calc R . . C30 C 0.4458(4) 0.1055(4) 0.6500(3) 0.0283(7) Uani 1 1 d . . . C31 C 0.3638(4) 0.1208(4) 0.7340(3) 0.0295(7) Uani 1 1 d . . . H31A H 0.4036 0.2100 0.8106 0.035 Uiso 1 1 calc R . . C32 C 0.2274(5) 0.0102(4) 0.7086(4) 0.0395(8) Uani 1 1 d . . . H32A H 0.1734 0.0246 0.7663 0.047 Uiso 1 1 calc R . . C33 C 0.1687(5) -0.1208(4) 0.6006(4) 0.0437(9) Uani 1 1 d . . . H33A H 0.0735 -0.1965 0.5825 0.052 Uiso 1 1 calc R . . C34 C 0.2487(5) -0.1416(4) 0.5188(4) 0.0432(9) Uani 1 1 d . . . H34A H 0.2104 -0.2324 0.4455 0.052 Uiso 1 1 calc R . . C35 C 0.3859(5) -0.0300(4) 0.5430(4) 0.0365(8) Uani 1 1 d . . . H35A H 0.4400 -0.0461 0.4857 0.044 Uiso 1 1 calc R . . C36 C 0.7079(4) 0.2887(3) 0.4541(4) 0.0244(6) Uani 1 1 d . . . H36A H 0.8082 0.3599 0.5479 0.029 Uiso 1 1 calc R . . H36B H 0.7145 0.1981 0.4382 0.029 Uiso 1 1 calc R . . C37 C 0.7306(4) 0.3229(3) 0.3414(3) 0.0244(6) Uani 1 1 d . . . C38 C 0.6861(4) 0.2186(4) 0.2087(4) 0.0312(7) Uani 1 1 d . . . H38A H 0.6422 0.1236 0.1897 0.037 Uiso 1 1 calc R . . C39 C 0.7044(5) 0.2507(4) 0.1043(4) 0.0396(8) Uani 1 1 d . . . H39A H 0.6742 0.1778 0.0155 0.047 Uiso 1 1 calc R . . C40 C 0.7660(5) 0.3873(4) 0.1278(4) 0.0440(9) Uani 1 1 d . . . H40A H 0.7771 0.4087 0.0554 0.053 Uiso 1 1 calc R . . C41 C 0.8114(5) 0.4926(4) 0.2579(4) 0.0379(8) Uani 1 1 d . . . H41A H 0.8545 0.5872 0.2755 0.045 Uiso 1 1 calc R . . C42 C 0.7943(4) 0.4602(3) 0.3633(4) 0.0286(7) Uani 1 1 d . . . H42A H 0.8269 0.5338 0.4526 0.034 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 0.01267(5) 0.02173(5) 0.01897(5) 0.01093(4) 0.00554(4) 0.00710(4) S1 0.0217(4) 0.0326(5) 0.0254(4) 0.0165(4) 0.0127(3) 0.0117(4) P1 0.0236(4) 0.0245(4) 0.0212(4) 0.0102(3) 0.0117(3) 0.0105(3) P2 0.0155(4) 0.0208(4) 0.0198(4) 0.0106(3) 0.0055(3) 0.0061(3) N1 0.0237(14) 0.0205(13) 0.0259(13) 0.0112(11) 0.0122(11) 0.0062(11) N2 0.0137(12) 0.0233(13) 0.0206(12) 0.0119(11) 0.0054(10) 0.0051(10) C1 0.0222(16) 0.0232(16) 0.0216(15) 0.0085(13) 0.0141(13) 0.0083(13) C2 0.0209(15) 0.0281(16) 0.0201(14) 0.0112(13) 0.0097(12) 0.0102(13) C3 0.0236(16) 0.0177(14) 0.0188(14) 0.0083(12) 0.0089(12) 0.0085(12) C4 0.0176(16) 0.0223(16) 0.0275(16) 0.0108(13) 0.0068(13) 0.0109(13) C5 0.0263(17) 0.0242(16) 0.0295(16) 0.0141(14) 0.0109(14) 0.0118(14) C6 0.0241(17) 0.0276(17) 0.0365(18) 0.0162(15) 0.0161(15) 0.0136(14) C7 0.0137(15) 0.0291(17) 0.0291(16) 0.0132(14) 0.0070(13) 0.0041(13) C8 0.0197(16) 0.0326(18) 0.0382(18) 0.0216(15) 0.0158(14) 0.0076(14) C9 0.0276(18) 0.0200(16) 0.0247(16) 0.0068(13) 0.0126(14) 0.0040(14) C10 0.0346(19) 0.0317(18) 0.0207(15) 0.0115(14) 0.0139(14) 0.0090(15) C11 0.041(2) 0.0308(18) 0.0317(17) 0.0188(15) 0.0238(16) 0.0100(16) C12 0.0311(19) 0.0238(17) 0.0299(17) 0.0075(14) 0.0179(15) -0.0032(14) C13 0.0202(16) 0.0306(17) 0.0220(15) 0.0085(13) 0.0119(13) 0.0027(13) C14 0.0232(16) 0.0229(16) 0.0256(16) 0.0110(13) 0.0103(13) 0.0064(13) C15 0.0322(19) 0.0315(18) 0.0337(18) 0.0150(15) 0.0195(15) 0.0166(15) C16 0.042(2) 0.043(2) 0.0253(17) 0.0115(16) 0.0195(16) 0.0196(18) C17 0.050(2) 0.058(2) 0.0279(18) 0.0247(18) 0.0201(17) 0.030(2) C18 0.037(2) 0.038(2) 0.0273(17) 0.0168(16) 0.0154(16) 0.0222(17) C19 0.0254(17) 0.0239(16) 0.0232(15) 0.0088(13) 0.0076(13) 0.0075(14) C20 0.048(2) 0.0224(17) 0.0378(19) 0.0193(16) 0.0157(17) 0.0102(16) C21 0.043(2) 0.0307(19) 0.0326(18) 0.0186(16) 0.0080(16) 0.0180(17) C22 0.0255(17) 0.0298(18) 0.0245(16) 0.0077(14) 0.0017(14) 0.0120(15) C23 0.0235(16) 0.0262(16) 0.0231(15) 0.0098(13) 0.0077(13) 0.0107(14) C24 0.034(2) 0.0301(18) 0.0367(19) 0.0108(16) 0.0158(16) 0.0168(16) C25 0.045(2) 0.039(2) 0.043(2) 0.0023(18) 0.0137(19) 0.0234(19) C26 0.048(3) 0.027(2) 0.067(3) 0.008(2) 0.009(2) 0.0192(19) C27 0.045(2) 0.031(2) 0.073(3) 0.032(2) 0.009(2) 0.0122(19) C28 0.033(2) 0.0296(19) 0.0371(19) 0.0164(16) 0.0072(16) 0.0107(16) C29 0.0251(18) 0.056(2) 0.0352(18) 0.0326(18) 0.0161(15) 0.0214(17) C30 0.0256(17) 0.046(2) 0.0261(16) 0.0265(16) 0.0109(14) 0.0222(16) C31 0.0327(19) 0.0375(19) 0.0259(16) 0.0212(15) 0.0136(14) 0.0179(16) C32 0.041(2) 0.052(2) 0.041(2) 0.034(2) 0.0216(18) 0.0221(19) C33 0.041(2) 0.045(2) 0.055(2) 0.036(2) 0.0217(19) 0.0186(19) C34 0.051(3) 0.032(2) 0.040(2) 0.0200(18) 0.0095(19) 0.0225(19) C35 0.047(2) 0.051(2) 0.0344(19) 0.0284(19) 0.0227(17) 0.037(2) C36 0.0192(16) 0.0288(17) 0.0225(16) 0.0107(14) 0.0078(13) 0.0112(14) C37 0.0141(15) 0.0337(18) 0.0284(16) 0.0128(15) 0.0118(13) 0.0137(14) C38 0.0248(17) 0.0313(18) 0.0341(18) 0.0110(15) 0.0139(15) 0.0127(15) C39 0.035(2) 0.049(2) 0.0268(18) 0.0082(17) 0.0180(16) 0.0137(18) C40 0.039(2) 0.063(3) 0.035(2) 0.025(2) 0.0240(18) 0.016(2) C41 0.031(2) 0.040(2) 0.045(2) 0.0219(18) 0.0212(17) 0.0112(17) C42 0.0202(16) 0.0305(17) 0.0308(17) 0.0100(14) 0.0129(14) 0.0087(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 N1 2.052(2) . ? Hf1 N2 2.071(2) . ? Hf1 C29 2.290(3) . ? Hf1 C36 2.303(3) . ? Hf1 P2 2.6897(8) . ? Hf1 S1 2.8939(8) . ? Hf1 P1 3.0743(8) . ? S1 C8 1.807(3) . ? S1 C6 1.809(3) . ? P1 N1 1.689(3) . ? P1 C1 1.828(3) . ? P1 C2 1.837(3) . ? P2 N2 1.661(2) . ? P2 C4 1.820(3) . ? P2 C3 1.823(3) . ? N1 C5 1.468(4) . ? N2 C7 1.460(4) . ? C1 C9 1.385(4) . ? C1 C13 1.396(4) . ? C2 C14 1.391(4) . ? C2 C18 1.400(4) . ? C3 C19 1.383(4) . ? C3 C23 1.395(4) . ? C4 C28 1.384(4) . ? C4 C24 1.398(5) . ? C5 C6 1.535(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.520(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.396(4) . ? C9 H9A 0.9500 . ? C10 C11 1.384(5) . ? C10 H10A 0.9500 . ? C11 C12 1.385(5) . ? C11 H11A 0.9500 . ? C12 C13 1.382(4) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.389(4) . ? C14 H14A 0.9500 . ? C15 C16 1.374(4) . ? C15 H15A 0.9500 . ? C16 C17 1.382(5) . ? C16 H16A 0.9500 . ? C17 C18 1.393(5) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.391(4) . ? C19 H19A 0.9500 . ? C20 C21 1.377(5) . ? C20 H20A 0.9500 . ? C21 C22 1.394(5) . ? C21 H21A 0.9500 . ? C22 C23 1.385(4) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C25 1.384(5) . ? C24 H24A 0.9500 . ? C25 C26 1.370(6) . ? C25 H25A 0.9500 . ? C26 C27 1.386(7) . ? C26 H26A 0.9500 . ? C27 C28 1.385(5) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.476(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C35 1.402(5) . ? C30 C31 1.406(4) . ? C31 C32 1.377(5) . ? C31 H31A 0.9500 . ? C32 C33 1.375(5) . ? C32 H32A 0.9500 . ? C33 C34 1.374(5) . ? C33 H33A 0.9500 . ? C34 C35 1.394(5) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C37 1.502(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C42 1.392(5) . ? C37 C38 1.398(4) . ? C38 C39 1.383(5) . ? C38 H38A 0.9500 . ? C39 C40 1.377(5) . ? C39 H39A 0.9500 . ? C40 C41 1.379(5) . ? C40 H40A 0.9500 . ? C41 C42 1.393(4) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? 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 N1 Hf1 N2 99.38(9) . . ? N1 Hf1 C29 124.98(12) . . ? N2 Hf1 C29 114.05(11) . . ? N1 Hf1 C36 107.12(10) . . ? N2 Hf1 C36 125.29(10) . . ? C29 Hf1 C36 88.22(11) . . ? N1 Hf1 P2 104.61(7) . . ? N2 Hf1 P2 38.13(6) . . ? C29 Hf1 P2 128.89(10) . . ? C36 Hf1 P2 88.44(8) . . ? N1 Hf1 S1 71.40(7) . . ? N2 Hf1 S1 70.87(6) . . ? C29 Hf1 S1 79.71(8) . . ? C36 Hf1 S1 163.18(8) . . ? P2 Hf1 S1 108.25(2) . . ? N1 Hf1 P1 31.05(7) . . ? N2 Hf1 P1 130.26(6) . . ? C29 Hf1 P1 105.19(10) . . ? C36 Hf1 P1 83.78(8) . . ? P2 Hf1 P1 125.06(2) . . ? S1 Hf1 P1 88.10(2) . . ? C8 S1 C6 104.68(15) . . ? C8 S1 Hf1 95.86(10) . . ? C6 S1 Hf1 96.24(10) . . ? N1 P1 C1 103.57(13) . . ? N1 P1 C2 104.84(13) . . ? C1 P1 C2 102.71(13) . . ? N1 P1 Hf1 38.81(8) . . ? C1 P1 Hf1 129.44(10) . . ? C2 P1 Hf1 116.92(10) . . ? N2 P2 C4 108.90(13) . . ? N2 P2 C3 109.68(12) . . ? C4 P2 C3 104.04(13) . . ? N2 P2 Hf1 50.33(8) . . ? C4 P2 Hf1 134.98(10) . . ? C3 P2 Hf1 120.17(9) . . ? C5 N1 P1 123.6(2) . . ? C5 N1 Hf1 123.48(19) . . ? P1 N1 Hf1 110.14(12) . . ? C7 N2 P2 128.2(2) . . ? C7 N2 Hf1 136.51(19) . . ? P2 N2 Hf1 91.53(10) . . ? C9 C1 C13 118.0(3) . . ? C9 C1 P1 121.8(2) . . ? C13 C1 P1 119.9(2) . . ? C14 C2 C18 118.7(3) . . ? C14 C2 P1 125.5(2) . . ? C18 C2 P1 115.7(2) . . ? C19 C3 C23 119.5(3) . . ? C19 C3 P2 118.4(2) . . ? C23 C3 P2 122.1(2) . . ? C28 C4 C24 118.8(3) . . ? C28 C4 P2 120.5(2) . . ? C24 C4 P2 120.5(2) . . ? N1 C5 C6 111.3(2) . . ? N1 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? N1 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 S1 113.1(2) . . ? C5 C6 H6A 109.0 . . ? S1 C6 H6A 109.0 . . ? C5 C6 H6B 109.0 . . ? S1 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N2 C7 C8 109.6(2) . . ? N2 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? N2 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C7 C8 S1 114.3(2) . . ? C7 C8 H8A 108.7 . . ? S1 C8 H8A 108.7 . . ? C7 C8 H8B 108.7 . . ? S1 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C1 C9 C10 121.3(3) . . ? C1 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C11 C10 C9 119.5(3) . . ? C11 C10 H10A 120.3 . . ? C9 C10 H10A 120.3 . . ? C10 C11 C12 120.1(3) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C13 C12 C11 119.8(3) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 C1 121.3(3) . . ? C12 C13 H13A 119.3 . . ? C1 C13 H13A 119.3 . . ? C15 C14 C2 120.5(3) . . ? C15 C14 H14A 119.8 . . ? C2 C14 H14A 119.8 . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C15 C16 C17 120.6(3) . . ? C15 C16 H16A 119.7 . . ? C17 C16 H16A 119.7 . . ? C16 C17 C18 119.5(3) . . ? C16 C17 H17A 120.2 . . ? C18 C17 H17A 120.2 . . ? C17 C18 C2 120.5(3) . . ? C17 C18 H18A 119.7 . . ? C2 C18 H18A 119.7 . . ? C3 C19 C20 120.5(3) . . ? C3 C19 H19A 119.7 . . ? C20 C19 H19A 119.7 . . ? C21 C20 C19 119.7(3) . . ? C21 C20 H20A 120.2 . . ? C19 C20 H20A 120.2 . . ? C20 C21 C22 120.5(3) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C23 C22 C21 119.5(3) . . ? C23 C22 H22A 120.2 . . ? C21 C22 H22A 120.2 . . ? C22 C23 C3 120.3(3) . . ? C22 C23 H23A 119.9 . . ? C3 C23 H23A 119.9 . . ? C25 C24 C4 120.4(3) . . ? C25 C24 H24A 119.8 . . ? C4 C24 H24A 119.8 . . ? C26 C25 C24 120.1(4) . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C25 C26 C27 120.2(4) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C28 C27 C26 120.0(4) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C4 C28 C27 120.5(4) . . ? C4 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C30 C29 Hf1 110.4(2) . . ? C30 C29 H29A 109.6 . . ? Hf1 C29 H29A 109.6 . . ? C30 C29 H29B 109.6 . . ? Hf1 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C35 C30 C31 116.2(3) . . ? C35 C30 C29 121.5(3) . . ? C31 C30 C29 122.2(3) . . ? C32 C31 C30 121.9(3) . . ? C32 C31 H31A 119.0 . . ? C30 C31 H31A 119.0 . . ? C33 C32 C31 120.5(3) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? C34 C33 C32 119.6(4) . . ? C34 C33 H33A 120.2 . . ? C32 C33 H33A 120.2 . . ? C33 C34 C35 120.3(4) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? C34 C35 C30 121.5(3) . . ? C34 C35 H35A 119.3 . . ? C30 C35 H35A 119.3 . . ? C37 C36 Hf1 120.55(19) . . ? C37 C36 H36A 107.2 . . ? Hf1 C36 H36A 107.2 . . ? C37 C36 H36B 107.2 . . ? Hf1 C36 H36B 107.2 . . ? H36A C36 H36B 106.8 . . ? C42 C37 C38 116.9(3) . . ? C42 C37 C36 121.4(3) . . ? C38 C37 C36 121.7(3) . . ? C39 C38 C37 121.4(3) . . ? C39 C38 H38A 119.3 . . ? C37 C38 H38A 119.3 . . ? C40 C39 C38 120.8(3) . . ? C40 C39 H39A 119.6 . . ? C38 C39 H39A 119.6 . . ? C39 C40 C41 119.2(3) . . ? C39 C40 H40A 120.4 . . ? C41 C40 H40A 120.4 . . ? C40 C41 C42 120.0(3) . . ? C40 C41 H41A 120.0 . . ? C42 C41 H41A 120.0 . . ? C37 C42 C41 121.8(3) . . ? C37 C42 H42A 119.1 . . ? C41 C42 H42A 119.1 . . ? 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 N1 Hf1 S1 C8 119.12(13) . . . . ? N2 Hf1 S1 C8 11.73(12) . . . . ? C29 Hf1 S1 C8 -108.36(14) . . . . ? C36 Hf1 S1 C8 -153.2(3) . . . . ? P2 Hf1 S1 C8 19.38(10) . . . . ? P1 Hf1 S1 C8 145.83(10) . . . . ? N1 Hf1 S1 C6 13.61(13) . . . . ? N2 Hf1 S1 C6 -93.78(13) . . . . ? C29 Hf1 S1 C6 146.13(15) . . . . ? C36 Hf1 S1 C6 101.3(3) . . . . ? P2 Hf1 S1 C6 -86.14(12) . . . . ? P1 Hf1 S1 C6 40.32(12) . . . . ? N2 Hf1 P1 N1 7.05(15) . . . . ? C29 Hf1 P1 N1 -134.50(15) . . . . ? C36 Hf1 P1 N1 139.06(15) . . . . ? P2 Hf1 P1 N1 55.37(13) . . . . ? S1 Hf1 P1 N1 -55.70(13) . . . . ? N1 Hf1 P1 C1 -57.46(17) . . . . ? N2 Hf1 P1 C1 -50.40(15) . . . . ? C29 Hf1 P1 C1 168.04(14) . . . . ? C36 Hf1 P1 C1 81.60(14) . . . . ? P2 Hf1 P1 C1 -2.08(12) . . . . ? S1 Hf1 P1 C1 -113.15(12) . . . . ? N1 Hf1 P1 C2 80.03(16) . . . . ? N2 Hf1 P1 C2 87.09(13) . . . . ? C29 Hf1 P1 C2 -54.46(13) . . . . ? C36 Hf1 P1 C2 -140.91(13) . . . . ? P2 Hf1 P1 C2 135.41(10) . . . . ? S1 Hf1 P1 C2 24.34(11) . . . . ? N1 Hf1 P2 N2 -86.61(12) . . . . ? C29 Hf1 P2 N2 79.65(14) . . . . ? C36 Hf1 P2 N2 166.10(12) . . . . ? S1 Hf1 P2 N2 -11.75(10) . . . . ? P1 Hf1 P2 N2 -112.63(10) . . . . ? N1 Hf1 P2 C4 -163.08(16) . . . . ? N2 Hf1 P2 C4 -76.47(17) . . . . ? C29 Hf1 P2 C4 3.18(18) . . . . ? C36 Hf1 P2 C4 89.62(16) . . . . ? S1 Hf1 P2 C4 -88.22(14) . . . . ? P1 Hf1 P2 C4 170.90(14) . . . . ? N1 Hf1 P2 C3 4.77(13) . . . . ? N2 Hf1 P2 C3 91.38(15) . . . . ? C29 Hf1 P2 C3 171.03(14) . . . . ? C36 Hf1 P2 C3 -102.53(13) . . . . ? S1 Hf1 P2 C3 79.63(11) . . . . ? P1 Hf1 P2 C3 -21.25(11) . . . . ? C1 P1 N1 C5 -60.4(2) . . . . ? C2 P1 N1 C5 47.0(2) . . . . ? Hf1 P1 N1 C5 161.7(3) . . . . ? C1 P1 N1 Hf1 137.95(12) . . . . ? C2 P1 N1 Hf1 -114.70(13) . . . . ? N2 Hf1 N1 C5 23.8(2) . . . . ? C29 Hf1 N1 C5 -104.5(2) . . . . ? C36 Hf1 N1 C5 155.3(2) . . . . ? P2 Hf1 N1 C5 62.4(2) . . . . ? S1 Hf1 N1 C5 -42.28(19) . . . . ? P1 Hf1 N1 C5 -161.7(3) . . . . ? N2 Hf1 N1 P1 -174.55(11) . . . . ? C29 Hf1 N1 P1 57.15(17) . . . . ? C36 Hf1 N1 P1 -42.97(15) . . . . ? P2 Hf1 N1 P1 -135.89(10) . . . . ? S1 Hf1 N1 P1 119.41(12) . . . . ? C4 P2 N2 C7 -65.8(3) . . . . ? C3 P2 N2 C7 47.4(3) . . . . ? Hf1 P2 N2 C7 160.8(3) . . . . ? C4 P2 N2 Hf1 133.38(11) . . . . ? C3 P2 N2 Hf1 -113.38(12) . . . . ? N1 Hf1 N2 C7 -56.2(3) . . . . ? C29 Hf1 N2 C7 79.0(3) . . . . ? C36 Hf1 N2 C7 -175.0(2) . . . . ? P2 Hf1 N2 C7 -157.9(3) . . . . ? S1 Hf1 N2 C7 10.3(2) . . . . ? P1 Hf1 N2 C7 -59.9(3) . . . . ? N1 Hf1 N2 P2 101.74(10) . . . . ? C29 Hf1 N2 P2 -123.02(12) . . . . ? C36 Hf1 N2 P2 -17.11(15) . . . . ? S1 Hf1 N2 P2 168.19(10) . . . . ? P1 Hf1 N2 P2 98.06(9) . . . . ? N1 P1 C1 C9 -20.5(3) . . . . ? C2 P1 C1 C9 -129.4(3) . . . . ? Hf1 P1 C1 C9 12.4(3) . . . . ? N1 P1 C1 C13 165.2(2) . . . . ? C2 P1 C1 C13 56.3(3) . . . . ? Hf1 P1 C1 C13 -161.87(18) . . . . ? N1 P1 C2 C14 -85.7(3) . . . . ? C1 P1 C2 C14 22.3(3) . . . . ? Hf1 P1 C2 C14 -125.4(2) . . . . ? N1 P1 C2 C18 89.4(3) . . . . ? C1 P1 C2 C18 -162.6(3) . . . . ? Hf1 P1 C2 C18 49.7(3) . . . . ? N2 P2 C3 C19 112.7(2) . . . . ? C4 P2 C3 C19 -130.9(2) . . . . ? Hf1 P2 C3 C19 57.9(2) . . . . ? N2 P2 C3 C23 -64.5(3) . . . . ? C4 P2 C3 C23 51.9(3) . . . . ? Hf1 P2 C3 C23 -119.3(2) . . . . ? N2 P2 C4 C28 -26.8(3) . . . . ? C3 P2 C4 C28 -143.7(3) . . . . ? Hf1 P2 C4 C28 25.4(3) . . . . ? N2 P2 C4 C24 158.4(2) . . . . ? C3 P2 C4 C24 41.5(3) . . . . ? Hf1 P2 C4 C24 -149.3(2) . . . . ? P1 N1 C5 C6 -95.5(3) . . . . ? Hf1 N1 C5 C6 63.7(3) . . . . ? N1 C5 C6 S1 -38.4(3) . . . . ? C8 S1 C6 C5 -88.4(2) . . . . ? Hf1 S1 C6 C5 9.4(2) . . . . ? P2 N2 C7 C8 175.8(2) . . . . ? Hf1 N2 C7 C8 -32.8(4) . . . . ? N2 C7 C8 S1 40.3(3) . . . . ? C6 S1 C8 C7 67.2(2) . . . . ? Hf1 S1 C8 C7 -30.9(2) . . . . ? C13 C1 C9 C10 -1.2(4) . . . . ? P1 C1 C9 C10 -175.6(2) . . . . ? C1 C9 C10 C11 0.4(5) . . . . ? C9 C10 C11 C12 0.6(5) . . . . ? C10 C11 C12 C13 -0.7(5) . . . . ? C11 C12 C13 C1 -0.1(5) . . . . ? C9 C1 C13 C12 1.0(4) . . . . ? P1 C1 C13 C12 175.5(2) . . . . ? C18 C2 C14 C15 -2.5(5) . . . . ? P1 C2 C14 C15 172.5(3) . . . . ? C2 C14 C15 C16 0.4(5) . . . . ? C14 C15 C16 C17 1.7(5) . . . . ? C15 C16 C17 C18 -1.6(6) . . . . ? C16 C17 C18 C2 -0.6(6) . . . . ? C14 C2 C18 C17 2.6(5) . . . . ? P1 C2 C18 C17 -172.8(3) . . . . ? C23 C3 C19 C20 -1.3(4) . . . . ? P2 C3 C19 C20 -178.6(2) . . . . ? C3 C19 C20 C21 1.3(5) . . . . ? C19 C20 C21 C22 0.4(5) . . . . ? C20 C21 C22 C23 -1.9(5) . . . . ? C21 C22 C23 C3 1.8(5) . . . . ? C19 C3 C23 C22 -0.2(4) . . . . ? P2 C3 C23 C22 176.9(2) . . . . ? C28 C4 C24 C25 0.3(5) . . . . ? P2 C4 C24 C25 175.2(3) . . . . ? C4 C24 C25 C26 -0.4(5) . . . . ? C24 C25 C26 C27 0.3(6) . . . . ? C25 C26 C27 C28 -0.2(6) . . . . ? C24 C4 C28 C27 -0.3(5) . . . . ? P2 C4 C28 C27 -175.1(3) . . . . ? C26 C27 C28 C4 0.2(6) . . . . ? N1 Hf1 C29 C30 117.4(2) . . . . ? N2 Hf1 C29 C30 -4.7(3) . . . . ? C36 Hf1 C29 C30 -132.9(2) . . . . ? P2 Hf1 C29 C30 -46.3(3) . . . . ? S1 Hf1 C29 C30 58.9(2) . . . . ? P1 Hf1 C29 C30 144.0(2) . . . . ? Hf1 C29 C30 C35 69.7(3) . . . . ? Hf1 C29 C30 C31 -105.0(3) . . . . ? C35 C30 C31 C32 -2.8(4) . . . . ? C29 C30 C31 C32 172.2(3) . . . . ? C30 C31 C32 C33 1.3(5) . . . . ? C31 C32 C33 C34 0.9(5) . . . . ? C32 C33 C34 C35 -1.5(5) . . . . ? C33 C34 C35 C30 -0.1(5) . . . . ? C31 C30 C35 C34 2.2(4) . . . . ? C29 C30 C35 C34 -172.8(3) . . . . ? N1 Hf1 C36 C37 -52.9(3) . . . . ? N2 Hf1 C36 C37 62.4(3) . . . . ? C29 Hf1 C36 C37 -179.1(3) . . . . ? P2 Hf1 C36 C37 51.9(2) . . . . ? S1 Hf1 C36 C37 -135.2(2) . . . . ? P1 Hf1 C36 C37 -73.6(2) . . . . ? Hf1 C36 C37 C42 82.8(3) . . . . ? Hf1 C36 C37 C38 -96.0(3) . . . . ? C42 C37 C38 C39 0.0(4) . . . . ? C36 C37 C38 C39 178.8(3) . . . . ? C37 C38 C39 C40 -0.6(5) . . . . ? C38 C39 C40 C41 0.7(5) . . . . ? C39 C40 C41 C42 -0.2(5) . . . . ? C38 C37 C42 C41 0.6(4) . . . . ? C36 C37 C42 C41 -178.3(3) . . . . ? C40 C41 C42 C37 -0.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.693 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.062 _vrf_PLAT161_mjs111_0m ; PROBLEM: Missing or Zero su (esd) on x-coordinate for ... HF1 RESPONSE: For the above error and the multiple related C level errors, Prof. G. Sheldrick was contacted and offered the following response; The space group is P1 and there is one dominant heavy atom. In the old days we would have fixed the x, y and z coordinates of this atom to prevent the structure going for a walk and their esds would have been exactly zero. More recently we use automatic floating origin restraints for the same purpose; roughly speaking, these would fix the center of gravity of the scattering power. The net result is exactly the same, the Hf atom is absolutely nailed down, and this is also a desirable outcome. In this case I would suggest that the esds on the x, y, z coordinates of Hf are indeed meaningless, and the esds on the other coordinates are effectively the esds of the differences between x,y,z of the other atoms and x,y,z of Hf. I could try to detect this situation in SHELXL and insert a meaningless but finite esd for x,y,z of Hf like 0.000001. But maybe zero is a better approximation and the buck should be passed to CheckCIF. ; data_mjs123_0ma_Compound_4 _database_code_depnum_ccdc_archive 'CCDC 911094' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C30 H50 Hf N2 P2 S' _chemical_formula_weight 711.21 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 29.761(2) _cell_length_b 10.3371(7) _cell_length_c 20.9993(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6460.2(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9976 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 3.414 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6322 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57605 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 27.56 _reflns_number_total 13748 _reflns_number_gt 11931 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.011(4) _refine_ls_number_reflns 13748 _refine_ls_number_parameters 665 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0469 _refine_ls_wR_factor_gt 0.0443 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _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 0.409214(5) 1.032718(14) 0.214611(10) 0.01969(4) Uani 1 1 d . . . Hf2 Hf 0.650197(5) 0.555134(14) 0.285526(10) 0.01885(4) Uani 1 1 d . . . S1 S 0.37499(4) 1.27543(11) 0.16353(7) 0.0297(3) Uani 1 1 d . . . S2 S 0.58306(4) 0.39921(10) 0.36234(7) 0.0298(3) Uani 1 1 d . . . P1 P 0.37153(4) 0.84081(11) 0.13556(7) 0.0288(3) Uani 1 1 d . . . P2 P 0.37590(4) 1.01048(10) 0.33479(7) 0.0242(3) Uani 1 1 d . . . P3 P 0.63838(4) 0.80547(10) 0.33650(6) 0.0222(3) Uani 1 1 d . . . P4 P 0.62025(4) 0.50861(11) 0.16202(7) 0.0250(3) Uani 1 1 d . . . N1 N 0.37369(13) 1.0017(3) 0.1318(2) 0.0326(10) Uani 1 1 d . . . N2 N 0.36801(10) 1.1224(3) 0.2797(2) 0.0220(8) Uani 1 1 d . . . N3 N 0.62698(11) 0.6573(3) 0.3634(2) 0.0231(9) Uani 1 1 d . . . N4 N 0.59461(10) 0.5105(3) 0.23232(19) 0.0241(10) Uani 1 1 d . . . C1 C 0.31153(16) 0.7917(5) 0.1351(3) 0.0437(15) Uani 1 1 d . . . H1 H 0.2958 0.8540 0.1639 0.052 Uiso 1 1 calc R . . C2 C 0.39401(17) 0.7795(5) 0.0593(3) 0.0481(15) Uani 1 1 d . . . H2 H 0.3734 0.8093 0.0246 0.058 Uiso 1 1 calc R . . C3 C 0.32061(15) 0.9485(4) 0.3613(3) 0.0318(12) Uani 1 1 d . . . H3 H 0.3023 1.0229 0.3772 0.038 Uiso 1 1 calc R . . C4 C 0.39993(16) 1.0848(4) 0.4068(3) 0.0368(13) Uani 1 1 d . . . H4 H 0.4070 1.0129 0.4371 0.044 Uiso 1 1 calc R . . C5 C 0.3466(2) 1.0811(5) 0.0877(3) 0.067(2) Uani 1 1 d . . . H5A H 0.3508 1.0474 0.0440 0.081 Uiso 1 1 calc R . . H5B H 0.3145 1.0703 0.0987 0.081 Uiso 1 1 calc R . . C6 C 0.35685(18) 1.2156(5) 0.0878(3) 0.0526(16) Uani 1 1 d . . . H6A H 0.3298 1.2643 0.0743 0.063 Uiso 1 1 calc R . . H6B H 0.3808 1.2321 0.0560 0.063 Uiso 1 1 calc R . . C7 C 0.33774(13) 1.2355(4) 0.2791(3) 0.0342(13) Uani 1 1 d . . . H7A H 0.3530 1.3103 0.2991 0.041 Uiso 1 1 calc R . . H7B H 0.3104 1.2159 0.3041 0.041 Uiso 1 1 calc R . . C8 C 0.32509(13) 1.2683(4) 0.2122(3) 0.0398(13) Uani 1 1 d . . . H8A H 0.3095 1.3528 0.2112 0.048 Uiso 1 1 calc R . . H8B H 0.3043 1.2018 0.1952 0.048 Uiso 1 1 calc R . . C9 C 0.3059(2) 0.6561(5) 0.1667(3) 0.071(2) Uani 1 1 d . . . H9A H 0.2741 0.6412 0.1764 0.107 Uiso 1 1 calc R . . H9B H 0.3234 0.6529 0.2062 0.107 Uiso 1 1 calc R . . H9C H 0.3166 0.5891 0.1374 0.107 Uiso 1 1 calc R . . C10 C 0.28677(16) 0.7984(5) 0.0719(3) 0.0613(19) Uani 1 1 d . . . H10A H 0.2988 0.7328 0.0429 0.092 Uiso 1 1 calc R . . H10B H 0.2908 0.8844 0.0531 0.092 Uiso 1 1 calc R . . H10C H 0.2547 0.7824 0.0789 0.092 Uiso 1 1 calc R . . C11 C 0.44007(18) 0.8399(6) 0.0473(3) 0.073(2) Uani 1 1 d . . . H11A H 0.4616 0.8066 0.0785 0.109 Uiso 1 1 calc R . . H11B H 0.4379 0.9341 0.0513 0.109 Uiso 1 1 calc R . . H11C H 0.4502 0.8176 0.0043 0.109 Uiso 1 1 calc R . . C12 C 0.3959(2) 0.6329(5) 0.0566(3) 0.072(2) Uani 1 1 d . . . H12A H 0.4080 0.6057 0.0153 0.108 Uiso 1 1 calc R . . H12B H 0.3656 0.5976 0.0620 0.108 Uiso 1 1 calc R . . H12C H 0.4154 0.6008 0.0908 0.108 Uiso 1 1 calc R . . C13 C 0.32580(18) 0.8501(4) 0.4151(3) 0.0479(15) Uani 1 1 d . . . H13A H 0.2970 0.8070 0.4227 0.072 Uiso 1 1 calc R . . H13B H 0.3354 0.8946 0.4540 0.072 Uiso 1 1 calc R . . H13C H 0.3484 0.7856 0.4032 0.072 Uiso 1 1 calc R . . C14 C 0.29686(15) 0.8890(4) 0.3045(3) 0.0436(15) Uani 1 1 d . . . H14A H 0.3145 0.8161 0.2884 0.065 Uiso 1 1 calc R . . H14B H 0.2936 0.9541 0.2709 0.065 Uiso 1 1 calc R . . H14C H 0.2671 0.8584 0.3176 0.065 Uiso 1 1 calc R . . C15 C 0.44461(15) 1.1491(5) 0.3889(3) 0.0468(16) Uani 1 1 d . . . H15A H 0.4389 1.2221 0.3603 0.070 Uiso 1 1 calc R . . H15B H 0.4640 1.0860 0.3675 0.070 Uiso 1 1 calc R . . H15C H 0.4595 1.1804 0.4276 0.070 Uiso 1 1 calc R . . C16 C 0.36982(17) 1.1793(5) 0.4419(3) 0.0498(15) Uani 1 1 d . . . H16A H 0.3858 1.2137 0.4790 0.075 Uiso 1 1 calc R . . H16B H 0.3425 1.1347 0.4560 0.075 Uiso 1 1 calc R . . H16C H 0.3617 1.2506 0.4134 0.075 Uiso 1 1 calc R . . C17 C 0.46243(13) 0.8750(4) 0.2416(2) 0.0273(11) Uani 1 1 d . . . H17A H 0.4771 0.8484 0.2014 0.033 Uiso 1 1 calc R . . H17B H 0.4857 0.9191 0.2673 0.033 Uiso 1 1 calc R . . C18 C 0.45082(12) 0.7542(4) 0.2761(3) 0.0252(12) Uani 1 1 d . . . C19 C 0.45175(15) 0.7480(4) 0.3412(3) 0.0306(13) Uani 1 1 d . . . H19 H 0.4613 0.8226 0.3640 0.037 Uiso 1 1 calc R . . C20 C 0.43953(16) 0.6388(4) 0.3760(3) 0.0406(14) Uani 1 1 d . . . H20 H 0.4406 0.6399 0.4213 0.049 Uiso 1 1 calc R . . C21 C 0.42582(16) 0.5293(4) 0.3441(4) 0.0458(16) Uani 1 1 d . . . H21 H 0.4169 0.4541 0.3668 0.055 Uiso 1 1 calc R . . C22 C 0.42531(16) 0.5312(4) 0.2785(4) 0.0492(18) Uani 1 1 d . . . H22 H 0.4165 0.4555 0.2561 0.059 Uiso 1 1 calc R . . C23 C 0.43727(14) 0.6408(4) 0.2444(3) 0.0367(13) Uani 1 1 d . . . H23 H 0.4363 0.6394 0.1992 0.044 Uiso 1 1 calc R . . C24 C 0.47078(12) 1.1666(3) 0.2080(3) 0.0246(11) Uani 1 1 d . . . H24A H 0.4618 1.2556 0.2199 0.030 Uiso 1 1 calc R . . H24B H 0.4938 1.1373 0.2388 0.030 Uiso 1 1 calc R . . C25 C 0.49042(13) 1.1682(4) 0.1437(2) 0.0239(11) Uani 1 1 d . . . C26 C 0.51887(16) 1.0708(4) 0.1220(3) 0.0370(13) Uani 1 1 d . . . H26 H 0.5270 1.0038 0.1507 0.044 Uiso 1 1 calc R . . C27 C 0.53560(19) 1.0668(5) 0.0615(3) 0.0486(16) Uani 1 1 d . . . H27 H 0.5551 0.9982 0.0497 0.058 Uiso 1 1 calc R . . C28 C 0.52476(18) 1.1599(5) 0.0176(3) 0.0497(16) Uani 1 1 d . . . H28 H 0.5359 1.1556 -0.0248 0.060 Uiso 1 1 calc R . . C29 C 0.49689(16) 1.2606(5) 0.0368(3) 0.0471(17) Uani 1 1 d . . . H29 H 0.4891 1.3266 0.0073 0.056 Uiso 1 1 calc R . . C30 C 0.48036(14) 1.2657(4) 0.0986(3) 0.0383(14) Uani 1 1 d . . . H30 H 0.4619 1.3364 0.1109 0.046 Uiso 1 1 calc R . . C31 C 0.58532(14) 0.8979(4) 0.3294(3) 0.0349(13) Uani 1 1 d . . . H31 H 0.5628 0.8365 0.3110 0.042 Uiso 1 1 calc R . . C32 C 0.67000(14) 0.8857(4) 0.4012(3) 0.0279(11) Uani 1 1 d . . . H32 H 0.6507 0.8846 0.4401 0.033 Uiso 1 1 calc R . . C33 C 0.59402(16) 0.6311(4) 0.1090(3) 0.0343(12) Uani 1 1 d . . . H33 H 0.6140 0.6404 0.0710 0.041 Uiso 1 1 calc R . . C34 C 0.60926(15) 0.3514(4) 0.1230(3) 0.0280(12) Uani 1 1 d . . . H34 H 0.5760 0.3393 0.1191 0.034 Uiso 1 1 calc R . . C35 C 0.60205(15) 0.6236(4) 0.4212(3) 0.0315(12) Uani 1 1 d . . . H35A H 0.5920 0.7035 0.4429 0.038 Uiso 1 1 calc R . . H35B H 0.6219 0.5756 0.4508 0.038 Uiso 1 1 calc R . . C36 C 0.56159(14) 0.5409(4) 0.4044(3) 0.0319(12) Uani 1 1 d . . . H36A H 0.5406 0.5899 0.3769 0.038 Uiso 1 1 calc R . . H36B H 0.5454 0.5144 0.4435 0.038 Uiso 1 1 calc R . . C37 C 0.54719(14) 0.4825(4) 0.2471(3) 0.0373(13) Uani 1 1 d . . . H37A H 0.5316 0.4528 0.2080 0.045 Uiso 1 1 calc R . . H37B H 0.5322 0.5624 0.2620 0.045 Uiso 1 1 calc R . . C38 C 0.54368(13) 0.3780(4) 0.2985(3) 0.0334(13) Uani 1 1 d . . . H38A H 0.5488 0.2923 0.2787 0.040 Uiso 1 1 calc R . . H38B H 0.5129 0.3785 0.3162 0.040 Uiso 1 1 calc R . . C39 C 0.59163(14) 1.0046(4) 0.2793(3) 0.0427(15) Uani 1 1 d . . . H39A H 0.5623 1.0412 0.2681 0.064 Uiso 1 1 calc R . . H39B H 0.6057 0.9678 0.2412 0.064 Uiso 1 1 calc R . . H39C H 0.6109 1.0728 0.2967 0.064 Uiso 1 1 calc R . . C40 C 0.56405(16) 0.9514(5) 0.3899(3) 0.0524(17) Uani 1 1 d . . . H40A H 0.5841 1.0158 0.4089 0.079 Uiso 1 1 calc R . . H40B H 0.5591 0.8807 0.4202 0.079 Uiso 1 1 calc R . . H40C H 0.5352 0.9920 0.3795 0.079 Uiso 1 1 calc R . . C41 C 0.68168(16) 1.0282(4) 0.3866(3) 0.0402(14) Uani 1 1 d . . . H41A H 0.7014 1.0621 0.4201 0.060 Uiso 1 1 calc R . . H41B H 0.6540 1.0795 0.3851 0.060 Uiso 1 1 calc R . . H41C H 0.6971 1.0335 0.3455 0.060 Uiso 1 1 calc R . . C42 C 0.71227(16) 0.8097(4) 0.4161(3) 0.0472(16) Uani 1 1 d . . . H42A H 0.7322 0.8107 0.3790 0.071 Uiso 1 1 calc R . . H42B H 0.7043 0.7202 0.4265 0.071 Uiso 1 1 calc R . . H42C H 0.7277 0.8491 0.4525 0.071 Uiso 1 1 calc R . . C43 C 0.54706(17) 0.5960(5) 0.0843(3) 0.0555(18) Uani 1 1 d . . . H43A H 0.5260 0.5919 0.1201 0.083 Uiso 1 1 calc R . . H43B H 0.5482 0.5117 0.0630 0.083 Uiso 1 1 calc R . . H43C H 0.5370 0.6620 0.0540 0.083 Uiso 1 1 calc R . . C44 C 0.59388(16) 0.7612(4) 0.1433(3) 0.0472(16) Uani 1 1 d . . . H44A H 0.5850 0.8295 0.1135 0.071 Uiso 1 1 calc R . . H44B H 0.6241 0.7796 0.1597 0.071 Uiso 1 1 calc R . . H44C H 0.5725 0.7583 0.1788 0.071 Uiso 1 1 calc R . . C45 C 0.62971(19) 0.3481(5) 0.0577(3) 0.0539(17) Uani 1 1 d . . . H45A H 0.6622 0.3617 0.0610 0.081 Uiso 1 1 calc R . . H45B H 0.6165 0.4167 0.0315 0.081 Uiso 1 1 calc R . . H45C H 0.6238 0.2639 0.0380 0.081 Uiso 1 1 calc R . . C46 C 0.62817(16) 0.2438(4) 0.1646(3) 0.0447(15) Uani 1 1 d . . . H46A H 0.6233 0.1602 0.1438 0.067 Uiso 1 1 calc R . . H46B H 0.6130 0.2445 0.2060 0.067 Uiso 1 1 calc R . . H46C H 0.6605 0.2576 0.1708 0.067 Uiso 1 1 calc R . . C47 C 0.71426(13) 0.6390(4) 0.2414(2) 0.0241(11) Uani 1 1 d . . . H47A H 0.7318 0.6765 0.2770 0.029 Uiso 1 1 calc R . . H47B H 0.7318 0.5644 0.2254 0.029 Uiso 1 1 calc R . . C48 C 0.71448(13) 0.7362(4) 0.1902(3) 0.0270(12) Uani 1 1 d . . . C49 C 0.71592(13) 0.7003(4) 0.1261(3) 0.0290(12) Uani 1 1 d . . . H49 H 0.7182 0.6112 0.1156 0.035 Uiso 1 1 calc R . . C50 C 0.71419(14) 0.7910(5) 0.0771(3) 0.0395(14) Uani 1 1 d . . . H50 H 0.7151 0.7631 0.0340 0.047 Uiso 1 1 calc R . . C51 C 0.71115(15) 0.9211(5) 0.0909(3) 0.0443(15) Uani 1 1 d . . . H51 H 0.7092 0.9831 0.0576 0.053 Uiso 1 1 calc R . . C52 C 0.71106(14) 0.9600(4) 0.1536(3) 0.0371(14) Uani 1 1 d . . . H52 H 0.7098 1.0496 0.1635 0.045 Uiso 1 1 calc R . . C53 C 0.71273(12) 0.8702(3) 0.2023(3) 0.0277(13) Uani 1 1 d . . . H53 H 0.7127 0.8997 0.2452 0.033 Uiso 1 1 calc R . . C54 C 0.69134(13) 0.3760(4) 0.3122(2) 0.0266(12) Uani 1 1 d . . . H54A H 0.6713 0.3062 0.3277 0.032 Uiso 1 1 calc R . . H54B H 0.7081 0.3436 0.2748 0.032 Uiso 1 1 calc R . . C55 C 0.72261(14) 0.4158(4) 0.3627(3) 0.0283(12) Uani 1 1 d . . . C56 C 0.76747(14) 0.4539(4) 0.3490(3) 0.0336(12) Uani 1 1 d . . . H56 H 0.7779 0.4486 0.3063 0.040 Uiso 1 1 calc R . . C57 C 0.79605(16) 0.4977(4) 0.3948(3) 0.0421(16) Uani 1 1 d . . . H57 H 0.8260 0.5199 0.3838 0.050 Uiso 1 1 calc R . . C58 C 0.78198(19) 0.5099(5) 0.4564(3) 0.0489(17) Uani 1 1 d . . . H58 H 0.8017 0.5419 0.4883 0.059 Uiso 1 1 calc R . . C59 C 0.73853(18) 0.4748(4) 0.4714(3) 0.0455(15) Uani 1 1 d . . . H59 H 0.7282 0.4830 0.5140 0.055 Uiso 1 1 calc R . . C60 C 0.70999(17) 0.4280(4) 0.4252(3) 0.0377(13) Uani 1 1 d . . . H60 H 0.6804 0.4033 0.4371 0.045 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 0.01717(7) 0.02557(8) 0.01631(10) -0.00306(10) -0.00103(9) -0.00003(7) Hf2 0.01843(8) 0.01912(7) 0.01899(11) 0.00128(10) -0.00099(9) 0.00021(7) S1 0.0272(6) 0.0359(6) 0.0261(8) 0.0058(6) -0.0002(6) 0.0002(5) S2 0.0322(6) 0.0256(6) 0.0317(9) 0.0009(6) 0.0043(6) -0.0015(5) P1 0.0334(7) 0.0336(7) 0.0194(8) -0.0059(6) -0.0020(6) -0.0001(5) P2 0.0270(6) 0.0257(6) 0.0198(8) -0.0011(5) 0.0028(6) 0.0050(5) P3 0.0228(6) 0.0228(6) 0.0210(8) 0.0015(5) -0.0003(5) 0.0013(4) P4 0.0246(6) 0.0269(6) 0.0235(9) 0.0017(6) -0.0029(6) -0.0015(5) N1 0.040(2) 0.039(2) 0.018(3) 0.001(2) -0.006(2) -0.0092(18) N2 0.0246(17) 0.0279(16) 0.013(2) 0.0025(19) 0.0027(19) 0.0066(13) N3 0.0238(19) 0.0201(18) 0.025(3) 0.0011(17) -0.0010(19) -0.0024(14) N4 0.0186(17) 0.0331(19) 0.021(3) 0.0002(16) -0.0031(16) 0.0020(15) C1 0.042(3) 0.050(3) 0.038(4) -0.025(3) 0.006(3) -0.008(2) C2 0.040(3) 0.074(4) 0.030(4) -0.016(3) -0.003(3) 0.005(3) C3 0.036(3) 0.035(3) 0.025(3) 0.002(2) 0.007(2) 0.004(2) C4 0.047(3) 0.041(3) 0.022(3) -0.003(2) -0.005(3) 0.012(2) C5 0.106(6) 0.064(4) 0.032(5) 0.012(3) -0.030(4) -0.016(4) C6 0.061(4) 0.057(4) 0.039(5) 0.002(3) -0.012(3) 0.009(3) C7 0.035(3) 0.036(2) 0.032(4) 0.003(3) 0.017(3) 0.0142(19) C8 0.024(2) 0.043(3) 0.053(4) 0.011(3) 0.003(3) 0.0098(19) C9 0.096(5) 0.061(4) 0.058(6) -0.014(3) 0.018(4) -0.042(3) C10 0.033(3) 0.083(4) 0.068(6) -0.030(4) -0.011(3) -0.009(3) C11 0.051(4) 0.126(6) 0.041(5) -0.020(4) 0.012(3) -0.006(4) C12 0.092(5) 0.071(4) 0.053(5) -0.045(4) -0.014(4) 0.028(4) C13 0.065(4) 0.044(3) 0.035(4) 0.004(3) 0.007(3) -0.008(3) C14 0.037(3) 0.049(3) 0.044(5) 0.001(3) 0.008(3) -0.006(2) C15 0.036(3) 0.052(3) 0.052(5) -0.021(3) -0.016(3) 0.008(2) C16 0.058(4) 0.061(4) 0.031(4) -0.016(3) 0.006(3) -0.001(3) C17 0.022(2) 0.038(3) 0.022(3) -0.001(2) 0.003(2) 0.0012(19) C18 0.017(2) 0.028(2) 0.031(4) -0.004(2) -0.005(2) 0.0064(16) C19 0.035(3) 0.021(2) 0.036(4) -0.005(2) -0.001(3) 0.0029(19) C20 0.043(3) 0.037(3) 0.042(4) 0.005(3) 0.001(3) 0.008(2) C21 0.034(3) 0.029(3) 0.075(6) 0.008(3) 0.000(3) 0.001(2) C22 0.040(3) 0.024(3) 0.084(6) -0.024(3) -0.015(3) 0.0044(19) C23 0.039(3) 0.036(3) 0.034(4) -0.013(2) -0.013(3) 0.012(2) C24 0.0156(19) 0.025(2) 0.033(3) -0.005(2) -0.005(2) -0.0008(15) C25 0.016(2) 0.028(2) 0.027(3) 0.003(2) -0.005(2) -0.0033(18) C26 0.041(3) 0.039(3) 0.032(4) 0.007(3) 0.004(3) -0.001(2) C27 0.062(4) 0.044(3) 0.039(4) 0.000(3) 0.008(3) 0.004(3) C28 0.053(4) 0.066(4) 0.029(4) 0.008(3) -0.007(3) -0.008(3) C29 0.033(3) 0.058(3) 0.051(5) 0.032(3) -0.014(3) -0.009(3) C30 0.021(2) 0.039(3) 0.055(5) 0.014(3) -0.002(3) -0.002(2) C31 0.029(3) 0.028(2) 0.048(4) 0.002(2) -0.001(3) 0.0027(19) C32 0.027(2) 0.030(2) 0.027(3) -0.003(2) 0.003(2) 0.0016(19) C33 0.041(3) 0.036(3) 0.025(3) 0.006(2) -0.014(3) 0.002(2) C34 0.025(2) 0.031(2) 0.027(3) -0.005(2) 0.000(2) -0.0033(19) C35 0.046(3) 0.033(3) 0.016(3) 0.001(2) 0.007(2) -0.005(2) C36 0.033(3) 0.035(3) 0.028(4) 0.001(2) 0.009(2) -0.005(2) C37 0.023(2) 0.057(3) 0.032(4) -0.012(3) -0.002(2) 0.002(2) C38 0.023(2) 0.039(2) 0.039(4) -0.007(3) 0.007(2) -0.0133(19) C39 0.045(3) 0.032(2) 0.051(4) 0.011(3) -0.020(3) 0.009(2) C40 0.041(3) 0.053(3) 0.063(5) -0.002(3) 0.014(3) 0.017(3) C41 0.049(3) 0.031(3) 0.041(4) -0.003(2) -0.003(3) -0.015(2) C42 0.043(3) 0.047(3) 0.052(5) -0.004(3) -0.020(3) 0.002(2) C43 0.060(4) 0.047(3) 0.060(5) 0.019(3) -0.029(3) 0.001(3) C44 0.047(3) 0.035(3) 0.060(5) 0.009(3) -0.012(3) 0.012(2) C45 0.066(4) 0.058(4) 0.038(5) -0.012(3) 0.011(3) -0.011(3) C46 0.052(3) 0.029(3) 0.053(5) -0.004(3) -0.005(3) 0.006(2) C47 0.024(2) 0.021(2) 0.027(3) -0.001(2) -0.001(2) -0.0019(18) C48 0.014(2) 0.032(2) 0.035(4) 0.004(2) 0.002(2) -0.0016(18) C49 0.018(2) 0.035(3) 0.034(4) 0.001(2) 0.000(2) 0.0007(19) C50 0.031(3) 0.058(3) 0.030(4) 0.009(3) -0.005(3) -0.009(2) C51 0.032(3) 0.056(3) 0.045(5) 0.024(3) -0.006(3) -0.003(2) C52 0.030(3) 0.032(3) 0.049(4) 0.003(3) 0.001(3) -0.002(2) C53 0.021(2) 0.024(2) 0.038(4) 0.004(2) 0.004(2) -0.0022(17) C54 0.022(2) 0.020(2) 0.037(4) 0.005(2) 0.003(2) -0.0025(17) C55 0.025(2) 0.021(2) 0.038(4) 0.007(2) -0.001(2) 0.0062(18) C56 0.035(3) 0.028(2) 0.038(4) 0.011(2) -0.004(3) 0.002(2) C57 0.031(3) 0.032(3) 0.063(5) 0.011(3) -0.015(3) 0.000(2) C58 0.062(4) 0.035(3) 0.050(5) 0.010(3) -0.025(4) -0.002(3) C59 0.066(4) 0.039(3) 0.032(4) 0.012(3) -0.005(3) 0.002(3) C60 0.038(3) 0.038(3) 0.037(4) 0.014(3) 0.004(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 N2 2.057(3) . ? Hf1 N1 2.060(4) . ? Hf1 C24 2.300(3) . ? Hf1 C17 2.342(4) . ? Hf1 P2 2.7212(14) . ? Hf1 P1 2.8194(13) . ? Hf1 S1 2.9125(11) . ? Hf2 N4 2.049(3) . ? Hf2 N3 2.066(4) . ? Hf2 C54 2.290(4) . ? Hf2 C47 2.290(4) . ? Hf2 P4 2.7841(15) . ? Hf2 P3 2.8224(11) . ? Hf2 S2 3.0319(12) . ? S1 C6 1.791(6) . ? S1 C8 1.804(5) . ? S2 C38 1.794(5) . ? S2 C36 1.826(4) . ? P1 N1 1.666(4) . ? P1 C2 1.847(6) . ? P1 C1 1.857(5) . ? P2 N2 1.654(4) . ? P2 C4 1.841(5) . ? P2 C3 1.851(5) . ? P3 N3 1.667(3) . ? P3 C32 1.849(5) . ? P3 C31 1.852(4) . ? P4 N4 1.662(4) . ? P4 C34 1.849(4) . ? P4 C33 1.858(5) . ? N1 C5 1.478(7) . ? N2 C7 1.476(4) . ? N3 C35 1.465(6) . ? N4 C37 1.474(5) . ? C1 C10 1.521(8) . ? C1 C9 1.559(7) . ? C1 H1 1.0000 . ? C2 C12 1.517(7) . ? C2 C11 1.527(7) . ? C2 H2 1.0000 . ? C3 C14 1.516(7) . ? C3 C13 1.529(7) . ? C3 H3 1.0000 . ? C4 C16 1.517(6) . ? C4 C15 1.534(6) . ? C4 H4 1.0000 . ? C5 C6 1.423(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.494(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.484(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.370(7) . ? C18 C23 1.406(6) . ? C19 C20 1.393(6) . ? C19 H19 0.9500 . ? C20 C21 1.378(7) . ? C20 H20 0.9500 . ? C21 C22 1.377(9) . ? C21 H21 0.9500 . ? C22 C23 1.388(7) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.472(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.393(6) . ? C25 C30 1.414(6) . ? C26 C27 1.364(8) . ? C26 H26 0.9500 . ? C27 C28 1.372(7) . ? C27 H27 0.9500 . ? C28 C29 1.391(7) . ? C28 H28 0.9500 . ? C29 C30 1.390(8) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C40 1.523(7) . ? C31 C39 1.534(7) . ? C31 H31 1.0000 . ? C32 C42 1.516(6) . ? C32 C41 1.544(5) . ? C32 H32 1.0000 . ? C33 C44 1.526(6) . ? C33 C43 1.535(6) . ? C33 H33 1.0000 . ? C34 C45 1.501(7) . ? C34 C46 1.522(6) . ? C34 H34 1.0000 . ? C35 C36 1.518(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.531(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.471(6) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.396(7) . ? C48 C53 1.410(5) . ? C49 C50 1.394(7) . ? C49 H49 0.9500 . ? C50 C51 1.379(7) . ? C50 H50 0.9500 . ? C51 C52 1.377(8) . ? C51 H51 0.9500 . ? C52 C53 1.382(7) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 C55 1.469(6) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C60 1.372(7) . ? C55 C56 1.421(6) . ? C56 C57 1.362(7) . ? C56 H56 0.9500 . ? C57 C58 1.365(8) . ? C57 H57 0.9500 . ? C58 C59 1.380(7) . ? C58 H58 0.9500 . ? C59 C60 1.377(8) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? 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 N2 Hf1 N1 108.95(15) . . ? N2 Hf1 C24 104.12(14) . . ? N1 Hf1 C24 116.83(18) . . ? N2 Hf1 C17 123.80(16) . . ? N1 Hf1 C17 116.29(16) . . ? C24 Hf1 C17 83.96(13) . . ? N2 Hf1 P2 37.33(10) . . ? N1 Hf1 P2 125.63(11) . . ? C24 Hf1 P2 113.40(14) . . ? C17 Hf1 P2 87.89(12) . . ? N2 Hf1 P1 118.10(9) . . ? N1 Hf1 P1 35.85(10) . . ? C24 Hf1 P1 134.79(13) . . ? C17 Hf1 P1 85.51(11) . . ? P2 Hf1 P1 109.98(4) . . ? N2 Hf1 S1 69.37(10) . . ? N1 Hf1 S1 69.13(10) . . ? C24 Hf1 S1 74.81(10) . . ? C17 Hf1 S1 157.68(10) . . ? P2 Hf1 S1 106.67(4) . . ? P1 Hf1 S1 104.49(4) . . ? N4 Hf2 N3 106.07(14) . . ? N4 Hf2 C54 112.53(13) . . ? N3 Hf2 C54 113.49(16) . . ? N4 Hf2 C47 122.47(16) . . ? N3 Hf2 C47 113.89(14) . . ? C54 Hf2 C47 87.71(14) . . ? N4 Hf2 P4 36.36(11) . . ? N3 Hf2 P4 135.94(10) . . ? C54 Hf2 P4 105.05(12) . . ? C47 Hf2 P4 87.43(12) . . ? N4 Hf2 P3 108.23(9) . . ? N3 Hf2 P3 35.83(9) . . ? C54 Hf2 P3 135.66(12) . . ? C47 Hf2 P3 84.83(10) . . ? P4 Hf2 P3 118.15(3) . . ? N4 Hf2 S2 68.80(11) . . ? N3 Hf2 S2 68.30(9) . . ? C54 Hf2 S2 78.00(11) . . ? C47 Hf2 S2 164.82(11) . . ? P4 Hf2 S2 101.12(4) . . ? P3 Hf2 S2 101.74(3) . . ? C6 S1 C8 103.9(3) . . ? C6 S1 Hf1 97.76(17) . . ? C8 S1 Hf1 92.52(15) . . ? C38 S2 C36 103.4(2) . . ? C38 S2 Hf2 95.62(15) . . ? C36 S2 Hf2 93.54(14) . . ? N1 P1 C2 106.7(2) . . ? N1 P1 C1 108.1(2) . . ? C2 P1 C1 104.5(2) . . ? N1 P1 Hf1 46.37(15) . . ? C2 P1 Hf1 127.42(17) . . ? C1 P1 Hf1 125.30(17) . . ? N2 P2 C4 109.8(2) . . ? N2 P2 C3 109.03(19) . . ? C4 P2 C3 104.1(2) . . ? N2 P2 Hf1 48.95(13) . . ? C4 P2 Hf1 125.82(17) . . ? C3 P2 Hf1 129.18(18) . . ? N3 P3 C32 105.5(2) . . ? N3 P3 C31 109.14(19) . . ? C32 P3 C31 105.2(2) . . ? N3 P3 Hf2 46.50(14) . . ? C32 P3 Hf2 128.79(13) . . ? C31 P3 Hf2 123.28(16) . . ? N4 P4 C34 108.81(19) . . ? N4 P4 C33 109.3(2) . . ? C34 P4 C33 105.0(2) . . ? N4 P4 Hf2 46.96(12) . . ? C34 P4 Hf2 128.39(16) . . ? C33 P4 Hf2 125.08(16) . . ? C5 N1 P1 124.2(3) . . ? C5 N1 Hf1 136.3(3) . . ? P1 N1 Hf1 97.8(2) . . ? C7 N2 P2 130.3(3) . . ? C7 N2 Hf1 135.7(3) . . ? P2 N2 Hf1 93.72(13) . . ? C35 N3 P3 127.0(3) . . ? C35 N3 Hf2 134.7(3) . . ? P3 N3 Hf2 97.67(19) . . ? C37 N4 P4 128.6(3) . . ? C37 N4 Hf2 134.7(3) . . ? P4 N4 Hf2 96.68(15) . . ? C10 C1 C9 111.1(4) . . ? C10 C1 P1 117.2(4) . . ? C9 C1 P1 110.3(4) . . ? C10 C1 H1 105.7 . . ? C9 C1 H1 105.7 . . ? P1 C1 H1 105.7 . . ? C12 C2 C11 111.6(5) . . ? C12 C2 P1 112.8(4) . . ? C11 C2 P1 109.2(4) . . ? C12 C2 H2 107.7 . . ? C11 C2 H2 107.7 . . ? P1 C2 H2 107.7 . . ? C14 C3 C13 111.0(4) . . ? C14 C3 P2 108.6(4) . . ? C13 C3 P2 111.3(3) . . ? C14 C3 H3 108.6 . . ? C13 C3 H3 108.6 . . ? P2 C3 H3 108.6 . . ? C16 C4 C15 110.6(4) . . ? C16 C4 P2 116.0(4) . . ? C15 C4 P2 108.5(4) . . ? C16 C4 H4 107.1 . . ? C15 C4 H4 107.1 . . ? P2 C4 H4 107.1 . . ? C6 C5 N1 115.1(5) . . ? C6 C5 H5A 108.5 . . ? N1 C5 H5A 108.5 . . ? C6 C5 H5B 108.5 . . ? N1 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C5 C6 S1 113.8(4) . . ? C5 C6 H6A 108.8 . . ? S1 C6 H6A 108.8 . . ? C5 C6 H6B 108.8 . . ? S1 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? N2 C7 C8 109.9(4) . . ? N2 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? N2 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C7 C8 S1 109.6(3) . . ? C7 C8 H8A 109.8 . . ? S1 C8 H8A 109.8 . . ? C7 C8 H8B 109.8 . . ? S1 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 Hf1 123.1(3) . . ? C18 C17 H17A 106.6 . . ? Hf1 C17 H17A 106.6 . . ? C18 C17 H17B 106.6 . . ? Hf1 C17 H17B 106.6 . . ? H17A C17 H17B 106.5 . . ? C19 C18 C23 116.1(4) . . ? C19 C18 C17 121.4(4) . . ? C23 C18 C17 122.5(5) . . ? C18 C19 C20 123.8(5) . . ? C18 C19 H19 118.1 . . ? C20 C19 H19 118.1 . . ? C21 C20 C19 119.2(6) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C22 C21 C20 118.6(5) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C21 C22 C23 121.7(4) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C18 120.6(5) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? C25 C24 Hf1 112.3(3) . . ? C25 C24 H24A 109.1 . . ? Hf1 C24 H24A 109.1 . . ? C25 C24 H24B 109.1 . . ? Hf1 C24 H24B 109.1 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C30 115.2(5) . . ? C26 C25 C24 122.2(4) . . ? C30 C25 C24 122.5(4) . . ? C27 C26 C25 123.2(5) . . ? C27 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? C26 C27 C28 121.3(5) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C27 C28 C29 118.0(6) . . ? C27 C28 H28 121.0 . . ? C29 C28 H28 121.0 . . ? C30 C29 C28 120.8(5) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C25 121.5(5) . . ? C29 C30 H30 119.3 . . ? C25 C30 H30 119.3 . . ? C40 C31 C39 111.2(4) . . ? C40 C31 P3 118.3(4) . . ? C39 C31 P3 108.8(3) . . ? C40 C31 H31 105.9 . . ? C39 C31 H31 105.9 . . ? P3 C31 H31 105.9 . . ? C42 C32 C41 110.4(4) . . ? C42 C32 P3 110.0(3) . . ? C41 C32 P3 113.4(3) . . ? C42 C32 H32 107.6 . . ? C41 C32 H32 107.6 . . ? P3 C32 H32 107.6 . . ? C44 C33 C43 111.4(4) . . ? C44 C33 P4 108.6(4) . . ? C43 C33 P4 115.1(3) . . ? C44 C33 H33 107.1 . . ? C43 C33 H33 107.1 . . ? P4 C33 H33 107.1 . . ? C45 C34 C46 111.0(4) . . ? C45 C34 P4 110.7(3) . . ? C46 C34 P4 108.8(4) . . ? C45 C34 H34 108.8 . . ? C46 C34 H34 108.8 . . ? P4 C34 H34 108.8 . . ? N3 C35 C36 110.1(4) . . ? N3 C35 H35A 109.6 . . ? C36 C35 H35A 109.6 . . ? N3 C35 H35B 109.6 . . ? C36 C35 H35B 109.6 . . ? H35A C35 H35B 108.2 . . ? C35 C36 S2 106.6(3) . . ? C35 C36 H36A 110.4 . . ? S2 C36 H36A 110.4 . . ? C35 C36 H36B 110.4 . . ? S2 C36 H36B 110.4 . . ? H36A C36 H36B 108.6 . . ? N4 C37 C38 110.6(4) . . ? N4 C37 H37A 109.5 . . ? C38 C37 H37A 109.5 . . ? N4 C37 H37B 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? C37 C38 S2 113.3(3) . . ? C37 C38 H38A 108.9 . . ? S2 C38 H38A 108.9 . . ? C37 C38 H38B 108.9 . . ? S2 C38 H38B 108.9 . . ? H38A C38 H38B 107.7 . . ? C31 C39 H39A 109.5 . . ? C31 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C31 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C31 C40 H40A 109.5 . . ? C31 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C31 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C32 C41 H41A 109.5 . . ? C32 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C32 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C32 C42 H42A 109.5 . . ? C32 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C32 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C33 C43 H43A 109.5 . . ? C33 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C33 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C33 C44 H44A 109.5 . . ? C33 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C33 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C34 C45 H45A 109.5 . . ? C34 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C34 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C34 C46 H46A 109.5 . . ? C34 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C34 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 Hf2 123.9(3) . . ? C48 C47 H47A 106.4 . . ? Hf2 C47 H47A 106.4 . . ? C48 C47 H47B 106.4 . . ? Hf2 C47 H47B 106.4 . . ? H47A C47 H47B 106.4 . . ? C49 C48 C53 115.8(5) . . ? C49 C48 C47 121.5(4) . . ? C53 C48 C47 122.6(5) . . ? C50 C49 C48 122.2(5) . . ? C50 C49 H49 118.9 . . ? C48 C49 H49 118.9 . . ? C51 C50 C49 120.1(6) . . ? C51 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? C52 C51 C50 119.1(5) . . ? C52 C51 H51 120.5 . . ? C50 C51 H51 120.5 . . ? C51 C52 C53 120.8(5) . . ? C51 C52 H52 119.6 . . ? C53 C52 H52 119.6 . . ? C52 C53 C48 121.9(5) . . ? C52 C53 H53 119.1 . . ? C48 C53 H53 119.1 . . ? C55 C54 Hf2 106.8(3) . . ? C55 C54 H54A 110.4 . . ? Hf2 C54 H54A 110.4 . . ? C55 C54 H54B 110.4 . . ? Hf2 C54 H54B 110.4 . . ? H54A C54 H54B 108.6 . . ? C60 C55 C56 115.2(5) . . ? C60 C55 C54 122.9(4) . . ? C56 C55 C54 121.8(5) . . ? C57 C56 C55 122.4(6) . . ? C57 C56 H56 118.8 . . ? C55 C56 H56 118.8 . . ? C56 C57 C58 120.6(5) . . ? C56 C57 H57 119.7 . . ? C58 C57 H57 119.7 . . ? C57 C58 C59 118.7(6) . . ? C57 C58 H58 120.7 . . ? C59 C58 H58 120.7 . . ? C60 C59 C58 120.6(6) . . ? C60 C59 H59 119.7 . . ? C58 C59 H59 119.7 . . ? C55 C60 C59 122.5(5) . . ? C55 C60 H60 118.7 . . ? C59 C60 H60 118.7 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.062 _refine_diff_density_min -0.721 _refine_diff_density_rms 0.103 data_mjs112_0m_Compound_5 _database_code_depnum_ccdc_archive 'CCDC 911095' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C66 H40 B Br F20 Hf N2 O2 P2 S' _chemical_formula_weight 1636.21 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8106(6) _cell_length_b 16.6203(7) _cell_length_c 17.2159(7) _cell_angle_alpha 97.123(2) _cell_angle_beta 106.822(2) _cell_angle_gamma 96.886(2) _cell_volume 3702.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9741 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.49 _exptl_crystal_description plate _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 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 2.111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6239 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54901 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.58 _reflns_number_total 17020 _reflns_number_gt 14838 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0374P)^2^+0.9703P] 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 17020 _refine_ls_number_parameters 865 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0732 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.021 -0.028 0.472 908 312 ' ' 2 0.222 0.309 0.464 7 0 ' ' 3 0.778 0.690 0.536 7 0 ' ' _platon_squeeze_details ;PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: During the refinement of the structure, electron density peaks were located that were believed to be highly disordered solvent molecules (possibly bromobenzene). Attempts made to model the solvent molecule were not successful. The SQUEEZE option in PLATON (Spek, 2009) indicated there was a large solvent cavity 923.9 Ang^3. In the final cycles of refinement, this contribution (312) to the electron density was removed from the observed data. The density, the F(000) value, the molecular weight and the formula are given without taking into account the results obtained with the SQUEEZE option PLATON (Spek, 2009). Similar treatments of disordered solvent molecules were carried out by St\"ahler et al. (2001), Cox et al. (2003), Mohamed et al. (2003) and Athimoolam et al. (2005). References: Spek, A. L. (2009). Acta Cryst. D65, 148--155. Athimoolam, S., Kumar, J., Ramakrishnan, V. & Rajaram, R.K. (2005). Acta Cryst. E61, m2014-m2017. Cox, J.P., Kumarasammy, Y., Nahar, L., Sarkar D.S. & Shoeb, M. (2003). Acta Cryst. E59, o975-o977. Mohamed, A.A., Krause Bauer, A.J., Bruce, E.A. & Bruce M.R.M. (2003). Acta Cryst. C59, m84-m86. Stahler, R., Nather, C. & Bensch, W. (2001). Acta Cryst. C57, 26-27. ; 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 0.096059(8) 0.537571(6) 0.428340(6) 0.01327(4) Uani 1 1 d . . . Br1 Br 0.49152(3) 0.39255(2) 0.49727(3) 0.05101(10) Uani 1 1 d . . . S1 S 0.16803(5) 0.63885(4) 0.33770(4) 0.02143(14) Uani 1 1 d . . . P1 P 0.16807(5) 0.66868(4) 0.60725(4) 0.01569(14) Uani 1 1 d . . . P2 P 0.13894(5) 0.50915(4) 0.70118(4) 0.01454(13) Uani 1 1 d . . . F1 F 0.13191(14) 0.23584(9) 1.02907(10) 0.0310(4) Uani 1 1 d . . . F2 F -0.03963(15) 0.17027(11) 1.05049(12) 0.0386(4) Uani 1 1 d . . . F3 F -0.15303(14) 0.02830(12) 0.95393(13) 0.0436(5) Uani 1 1 d . . . F4 F -0.08528(14) -0.04854(11) 0.83547(13) 0.0425(5) Uani 1 1 d . . . F5 F 0.09041(13) 0.01397(9) 0.81459(11) 0.0306(4) Uani 1 1 d . . . F6 F 0.05066(12) 0.15855(10) 0.75384(10) 0.0292(4) Uani 1 1 d . . . F7 F 0.06218(15) 0.16770(13) 0.60447(11) 0.0427(5) Uani 1 1 d . . . F8 F 0.24394(16) 0.17328(13) 0.57258(11) 0.0457(5) Uani 1 1 d . . . F9 F 0.41888(15) 0.17484(12) 0.69786(12) 0.0421(5) Uani 1 1 d . . . F10 F 0.41115(13) 0.17041(11) 0.85023(11) 0.0324(4) Uani 1 1 d . . . F11 F 0.12680(12) 0.29648(9) 0.88146(10) 0.0261(4) Uani 1 1 d . . . F12 F 0.19755(14) 0.45585(9) 0.93679(11) 0.0346(4) Uani 1 1 d . . . F13 F 0.39542(15) 0.50698(10) 1.03445(12) 0.0413(5) Uani 1 1 d . . . F14 F 0.52002(13) 0.39375(10) 1.07475(12) 0.0402(5) Uani 1 1 d . . . F15 F 0.45221(12) 0.23487(9) 1.02088(11) 0.0306(4) Uani 1 1 d . . . F16 F 0.29811(15) 0.00805(10) 0.82626(12) 0.0375(4) Uani 1 1 d . . . F17 F 0.37975(17) -0.10697(12) 0.90202(16) 0.0577(6) Uani 1 1 d . . . F18 F 0.43011(17) -0.09378(13) 1.06856(17) 0.0648(7) Uani 1 1 d . . . F19 F 0.39266(16) 0.04019(13) 1.15778(13) 0.0530(6) Uani 1 1 d . . . F20 F 0.30560(14) 0.15570(10) 1.08267(10) 0.0334(4) Uani 1 1 d . . . O1 O 0.10839(14) 0.51334(9) 0.54364(10) 0.0160(4) Uani 1 1 d . . . O2 O -0.00262(13) 0.42718(10) 0.39334(11) 0.0153(4) Uani 1 1 d . . . N1 N 0.15850(17) 0.65883(12) 0.50963(13) 0.0190(5) Uani 1 1 d . . . N2 N 0.03425(16) 0.44238(12) 0.67478(13) 0.0174(5) Uani 1 1 d . . . C1 C 0.2998(2) 0.68859(15) 0.66982(16) 0.0194(5) Uani 1 1 d . . . C2 C 0.0974(2) 0.74328(14) 0.63916(16) 0.0191(6) Uani 1 1 d . . . C3 C 0.2476(2) 0.45709(14) 0.70860(17) 0.0187(5) Uani 1 1 d . . . C4 C 0.1609(2) 0.57946(15) 0.79456(16) 0.0175(5) Uani 1 1 d . . . C5 C 0.2093(3) 0.73428(16) 0.48940(18) 0.0294(7) Uani 1 1 d . . . H5A H 0.2639 0.7643 0.5391 0.035 Uiso 1 1 calc R . . H5B H 0.1585 0.7709 0.4718 0.035 Uiso 1 1 calc R . . C6 C 0.2553(2) 0.71231(19) 0.42159(19) 0.0323(7) Uani 1 1 d . . . H6A H 0.3185 0.6893 0.4443 0.039 Uiso 1 1 calc R . . H6B H 0.2746 0.7628 0.4007 0.039 Uiso 1 1 calc R . . C7 C 0.0362(2) 0.37804(17) 0.72754(19) 0.0290(7) Uani 1 1 d . . . H7A H 0.0359 0.4028 0.7828 0.035 Uiso 1 1 calc R . . H7B H 0.0996 0.3539 0.7340 0.035 Uiso 1 1 calc R . . C8 C -0.0554(2) 0.31249(17) 0.6891(2) 0.0302(7) Uani 1 1 d . . . H8A H -0.0613 0.2747 0.7282 0.036 Uiso 1 1 calc R . . H8B H -0.0485 0.2802 0.6392 0.036 Uiso 1 1 calc R . . C9 C 0.3573(2) 0.62627(16) 0.66032(18) 0.0230(6) Uani 1 1 d . . . H9 H 0.3270 0.5785 0.6200 0.028 Uiso 1 1 calc R . . C10 C 0.4576(2) 0.63384(19) 0.7091(2) 0.0329(7) Uani 1 1 d . . . H10 H 0.4959 0.5909 0.7034 0.039 Uiso 1 1 calc R . . C11 C 0.5027(2) 0.7048(2) 0.7670(2) 0.0384(8) Uani 1 1 d . . . H11 H 0.5716 0.7100 0.8011 0.046 Uiso 1 1 calc R . . C12 C 0.4478(2) 0.7675(2) 0.7747(2) 0.0368(8) Uani 1 1 d . . . H12 H 0.4796 0.8162 0.8133 0.044 Uiso 1 1 calc R . . C13 C 0.3465(2) 0.76019(17) 0.72694(19) 0.0278(7) Uani 1 1 d . . . H13 H 0.3090 0.8036 0.7329 0.033 Uiso 1 1 calc R . . C14 C 0.1082(2) 0.77012(15) 0.72149(17) 0.0235(6) Uani 1 1 d . . . H14 H 0.1584 0.7523 0.7634 0.028 Uiso 1 1 calc R . . C15 C 0.0463(2) 0.82248(17) 0.74237(19) 0.0298(7) Uani 1 1 d . . . H15 H 0.0549 0.8415 0.7987 0.036 Uiso 1 1 calc R . . C16 C -0.0285(3) 0.84759(18) 0.6816(2) 0.0348(7) Uani 1 1 d . . . H16 H -0.0711 0.8838 0.6961 0.042 Uiso 1 1 calc R . . C17 C -0.0407(3) 0.8199(2) 0.6002(2) 0.0378(8) Uani 1 1 d . . . H17 H -0.0923 0.8365 0.5585 0.045 Uiso 1 1 calc R . . C18 C 0.0219(2) 0.76768(17) 0.57855(18) 0.0278(7) Uani 1 1 d . . . H18 H 0.0129 0.7487 0.5222 0.033 Uiso 1 1 calc R . . C19 C 0.2529(2) 0.40984(16) 0.63726(19) 0.0268(6) Uani 1 1 d . . . H19 H 0.2002 0.4063 0.5866 0.032 Uiso 1 1 calc R . . C20 C 0.3344(3) 0.36827(19) 0.6402(2) 0.0355(8) Uani 1 1 d . . . H20 H 0.3383 0.3369 0.5915 0.043 Uiso 1 1 calc R . . C21 C 0.4103(3) 0.37231(19) 0.7140(2) 0.0395(8) Uani 1 1 d . . . H21 H 0.4670 0.3447 0.7156 0.047 Uiso 1 1 calc R . . C22 C 0.4043(2) 0.41586(19) 0.7851(2) 0.0372(8) Uani 1 1 d . . . H22 H 0.4558 0.4170 0.8358 0.045 Uiso 1 1 calc R . . C23 C 0.3230(2) 0.45827(16) 0.78286(19) 0.0260(6) Uani 1 1 d . . . H23 H 0.3188 0.4882 0.8322 0.031 Uiso 1 1 calc R . . C24 C 0.0777(2) 0.58899(17) 0.82380(17) 0.0239(6) Uani 1 1 d . . . H24 H 0.0126 0.5560 0.7965 0.029 Uiso 1 1 calc R . . C25 C 0.0910(2) 0.64731(18) 0.89334(18) 0.0294(7) Uani 1 1 d . . . H25 H 0.0350 0.6533 0.9140 0.035 Uiso 1 1 calc R . . C26 C 0.1850(2) 0.69627(18) 0.93227(18) 0.0305(7) Uani 1 1 d . . . H26 H 0.1928 0.7367 0.9788 0.037 Uiso 1 1 calc R . . C27 C 0.2680(2) 0.68706(17) 0.90415(17) 0.0261(6) Uani 1 1 d . . . H27 H 0.3327 0.7204 0.9317 0.031 Uiso 1 1 calc R . . C28 C 0.2562(2) 0.62880(15) 0.83539(16) 0.0201(6) Uani 1 1 d . . . H28 H 0.3131 0.6224 0.8160 0.024 Uiso 1 1 calc R . . C29 C 0.2279(2) 0.47577(16) 0.41692(17) 0.0224(6) Uani 1 1 d . . . H29A H 0.2916 0.5156 0.4449 0.027 Uiso 1 1 calc R . . H29B H 0.2297 0.4296 0.4483 0.027 Uiso 1 1 calc R . . C30 C 0.2324(2) 0.44288(16) 0.33429(17) 0.0204(6) Uani 1 1 d . . . C31 C 0.1672(2) 0.37088(17) 0.28762(19) 0.0281(6) Uani 1 1 d . . . H31 H 0.1186 0.3438 0.3090 0.034 Uiso 1 1 calc R . . C32 C 0.1723(2) 0.3385(2) 0.2111(2) 0.0345(7) Uani 1 1 d . . . H32 H 0.1284 0.2891 0.1812 0.041 Uiso 1 1 calc R . . C33 C 0.2413(3) 0.3782(2) 0.1781(2) 0.0362(8) Uani 1 1 d . . . H33 H 0.2446 0.3562 0.1254 0.043 Uiso 1 1 calc R . . C34 C 0.3052(2) 0.44954(19) 0.2220(2) 0.0319(7) Uani 1 1 d . . . H34 H 0.3525 0.4769 0.1995 0.038 Uiso 1 1 calc R . . C35 C 0.3007(2) 0.48141(17) 0.29881(19) 0.0261(6) Uani 1 1 d . . . H35 H 0.3452 0.5307 0.3282 0.031 Uiso 1 1 calc R . . C36 C 0.10136(19) 0.56452(14) 0.61088(15) 0.0143(5) Uani 1 1 d . . . C37 C 0.1206(2) 0.12971(15) 0.91864(16) 0.0177(5) Uani 1 1 d . . . C38 C 0.0823(2) 0.16514(15) 0.97831(17) 0.0213(6) Uani 1 1 d . . . C39 C -0.0075(2) 0.13260(17) 0.99156(18) 0.0260(6) Uani 1 1 d . . . C40 C -0.0651(2) 0.06049(18) 0.9426(2) 0.0284(7) Uani 1 1 d . . . C41 C -0.0305(2) 0.02235(16) 0.88282(19) 0.0268(6) Uani 1 1 d . . . C42 C 0.0601(2) 0.05634(16) 0.87288(17) 0.0215(6) Uani 1 1 d . . . C43 C 0.2306(2) 0.16024(15) 0.81075(17) 0.0205(6) Uani 1 1 d . . . C44 C 0.1451(2) 0.16158(16) 0.74467(17) 0.0225(6) Uani 1 1 d . . . C45 C 0.1486(2) 0.16650(18) 0.66553(18) 0.0284(7) Uani 1 1 d . . . C46 C 0.2401(3) 0.17019(18) 0.64908(19) 0.0320(7) Uani 1 1 d . . . C47 C 0.3278(2) 0.17069(17) 0.7128(2) 0.0295(7) Uani 1 1 d . . . C48 C 0.3213(2) 0.16714(16) 0.79073(18) 0.0245(6) Uani 1 1 d . . . C49 C 0.2843(2) 0.25605(15) 0.94999(16) 0.0204(6) Uani 1 1 d . . . C50 C 0.2255(2) 0.31766(16) 0.93087(17) 0.0216(6) Uani 1 1 d . . . C51 C 0.2596(2) 0.40068(16) 0.95811(18) 0.0251(6) Uani 1 1 d . . . C52 C 0.3593(2) 0.42640(16) 1.00701(18) 0.0276(7) Uani 1 1 d . . . C53 C 0.4218(2) 0.36896(17) 1.02706(18) 0.0257(6) Uani 1 1 d . . . C54 C 0.3841(2) 0.28635(16) 0.99847(17) 0.0226(6) Uani 1 1 d . . . C55 C 0.2999(2) 0.09071(16) 0.95064(18) 0.0212(6) Uani 1 1 d . . . C56 C 0.3204(2) 0.02067(17) 0.9089(2) 0.0288(7) Uani 1 1 d . . . C57 C 0.3626(3) -0.04039(18) 0.9474(2) 0.0384(8) Uani 1 1 d . . . C58 C 0.3884(2) -0.0344(2) 1.0312(3) 0.0409(9) Uani 1 1 d . . . C59 C 0.3699(2) 0.03289(19) 1.0755(2) 0.0360(8) Uani 1 1 d . . . C60 C 0.3259(2) 0.09309(16) 1.03494(19) 0.0254(6) Uani 1 1 d . . . C61 C 0.4256(3) 0.2836(2) 0.4497(3) 0.0476(10) Uani 1 1 d . . . C62 C 0.3651(3) 0.2683(3) 0.3694(3) 0.0596(12) Uani 1 1 d . . . H62 H 0.3564 0.3119 0.3386 0.072 Uiso 1 1 calc R . . C63 C 0.3163(4) 0.1888(3) 0.3330(4) 0.0880(18) Uani 1 1 d . . . H63 H 0.2737 0.1783 0.2773 0.106 Uiso 1 1 calc R . . C64 C 0.3287(6) 0.1266(4) 0.3758(7) 0.128(3) Uani 1 1 d . . . H64 H 0.2968 0.0720 0.3505 0.154 Uiso 1 1 calc R . . C65 C 0.3921(6) 0.1443(3) 0.4620(6) 0.112(3) Uani 1 1 d . . . H65 H 0.4000 0.1010 0.4934 0.134 Uiso 1 1 calc R . . C66 C 0.4407(4) 0.2233(3) 0.4982(4) 0.0709(14) Uani 1 1 d . . . H66 H 0.4826 0.2355 0.5541 0.085 Uiso 1 1 calc R . . B1 B 0.2338(2) 0.15940(17) 0.90712(19) 0.0186(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 0.01415(6) 0.01475(5) 0.01059(6) 0.00047(4) 0.00391(4) 0.00268(4) Br1 0.0401(2) 0.0518(2) 0.0606(3) 0.00552(18) 0.01785(19) 0.00345(16) S1 0.0218(4) 0.0263(3) 0.0189(3) 0.0064(3) 0.0096(3) 0.0037(3) P1 0.0175(3) 0.0140(3) 0.0134(3) -0.0006(2) 0.0033(3) 0.0007(2) P2 0.0151(3) 0.0168(3) 0.0112(3) 0.0017(2) 0.0031(3) 0.0036(2) F1 0.0391(11) 0.0265(8) 0.0235(9) -0.0081(7) 0.0118(8) -0.0019(7) F2 0.0429(12) 0.0439(10) 0.0388(11) 0.0012(9) 0.0270(9) 0.0141(9) F3 0.0290(11) 0.0495(11) 0.0589(14) 0.0090(10) 0.0264(10) -0.0005(8) F4 0.0353(11) 0.0334(9) 0.0495(12) -0.0106(8) 0.0140(9) -0.0143(8) F5 0.0338(10) 0.0236(8) 0.0333(10) -0.0107(7) 0.0170(8) -0.0007(7) F6 0.0218(9) 0.0434(9) 0.0212(9) 0.0049(7) 0.0030(7) 0.0111(7) F7 0.0407(12) 0.0662(13) 0.0186(9) 0.0090(9) 0.0009(8) 0.0174(10) F8 0.0560(13) 0.0636(13) 0.0235(10) 0.0121(9) 0.0198(9) 0.0090(10) F9 0.0347(11) 0.0576(12) 0.0443(12) 0.0138(10) 0.0258(9) 0.0082(9) F10 0.0198(9) 0.0468(10) 0.0332(10) 0.0136(8) 0.0082(8) 0.0082(7) F11 0.0201(9) 0.0259(8) 0.0270(9) 0.0056(7) -0.0024(7) 0.0057(6) F12 0.0370(11) 0.0217(8) 0.0430(11) 0.0069(7) 0.0056(9) 0.0118(7) F13 0.0446(12) 0.0198(8) 0.0479(12) 0.0003(8) 0.0022(9) -0.0039(7) F14 0.0239(10) 0.0358(9) 0.0447(12) 0.0047(8) -0.0085(8) -0.0078(7) F15 0.0178(9) 0.0289(8) 0.0385(10) 0.0086(7) -0.0032(7) 0.0052(7) F16 0.0484(12) 0.0298(9) 0.0418(12) 0.0023(8) 0.0231(10) 0.0154(8) F17 0.0586(15) 0.0346(10) 0.0983(19) 0.0198(11) 0.0408(14) 0.0290(10) F18 0.0471(13) 0.0543(13) 0.106(2) 0.0551(14) 0.0192(13) 0.0270(10) F19 0.0469(13) 0.0621(13) 0.0406(12) 0.0322(10) -0.0069(10) -0.0005(10) F20 0.0392(11) 0.0352(9) 0.0200(9) 0.0059(7) 0.0013(8) 0.0024(8) O1 0.0221(10) 0.0129(7) 0.0113(9) -0.0014(7) 0.0042(7) 0.0027(7) O2 0.0155(9) 0.0168(8) 0.0136(9) 0.0022(7) 0.0042(7) 0.0034(7) N1 0.0251(13) 0.0155(9) 0.0149(11) 0.0011(8) 0.0065(10) -0.0015(9) N2 0.0169(12) 0.0178(10) 0.0166(11) 0.0050(9) 0.0032(9) 0.0021(8) C1 0.0176(14) 0.0224(12) 0.0166(14) 0.0009(10) 0.0050(11) 0.0001(10) C2 0.0239(15) 0.0137(11) 0.0190(14) -0.0001(10) 0.0072(11) 0.0015(10) C3 0.0177(14) 0.0167(11) 0.0220(14) 0.0040(10) 0.0060(11) 0.0040(10) C4 0.0207(14) 0.0211(12) 0.0119(13) 0.0032(10) 0.0051(11) 0.0075(10) C5 0.0436(19) 0.0193(12) 0.0226(16) 0.0027(11) 0.0113(14) -0.0074(12) C6 0.0319(18) 0.0374(16) 0.0251(16) 0.0076(13) 0.0084(14) -0.0047(13) C7 0.0267(16) 0.0295(14) 0.0312(17) 0.0168(13) 0.0046(13) 0.0042(12) C8 0.0310(17) 0.0276(14) 0.0363(18) 0.0164(13) 0.0118(14) 0.0059(12) C9 0.0207(15) 0.0252(13) 0.0215(15) -0.0009(11) 0.0073(12) 0.0007(11) C10 0.0224(16) 0.0378(16) 0.0390(19) 0.0039(14) 0.0103(14) 0.0081(13) C11 0.0188(17) 0.0524(19) 0.0340(19) -0.0028(16) -0.0003(14) -0.0008(14) C12 0.0260(18) 0.0376(16) 0.0348(19) -0.0097(14) 0.0023(14) -0.0065(13) C13 0.0268(16) 0.0230(13) 0.0280(16) -0.0020(12) 0.0049(13) -0.0024(11) C14 0.0316(17) 0.0194(12) 0.0184(14) 0.0002(11) 0.0062(12) 0.0063(11) C15 0.0384(19) 0.0266(14) 0.0229(16) -0.0042(12) 0.0088(14) 0.0103(13) C16 0.041(2) 0.0300(15) 0.0352(19) -0.0014(13) 0.0128(15) 0.0178(14) C17 0.041(2) 0.0397(17) 0.0276(18) -0.0016(14) 0.0000(15) 0.0216(15) C18 0.0321(17) 0.0292(14) 0.0183(15) -0.0009(12) 0.0016(13) 0.0102(12) C19 0.0338(17) 0.0255(13) 0.0256(16) 0.0073(12) 0.0121(13) 0.0119(12) C20 0.045(2) 0.0353(16) 0.040(2) 0.0101(14) 0.0265(17) 0.0215(15) C21 0.0277(18) 0.0348(16) 0.062(3) 0.0087(16) 0.0175(17) 0.0175(14) C22 0.0239(17) 0.0331(16) 0.046(2) 0.0040(15) -0.0044(15) 0.0114(13) C23 0.0261(16) 0.0243(13) 0.0247(16) 0.0026(12) 0.0028(12) 0.0077(11) C24 0.0207(15) 0.0305(14) 0.0193(15) 0.0021(11) 0.0036(12) 0.0081(11) C25 0.0299(17) 0.0393(16) 0.0232(16) 0.0006(13) 0.0134(13) 0.0134(13) C26 0.0383(19) 0.0334(15) 0.0169(15) -0.0043(12) 0.0037(13) 0.0152(13) C27 0.0284(16) 0.0265(13) 0.0176(14) -0.0011(11) -0.0011(12) 0.0072(12) C28 0.0213(15) 0.0231(12) 0.0157(14) 0.0038(10) 0.0038(11) 0.0071(10) C29 0.0196(15) 0.0278(13) 0.0200(14) 0.0011(11) 0.0065(12) 0.0064(11) C30 0.0196(14) 0.0253(12) 0.0174(14) -0.0002(11) 0.0063(11) 0.0103(11) C31 0.0218(16) 0.0306(14) 0.0306(17) -0.0022(13) 0.0093(13) 0.0044(12) C32 0.0278(18) 0.0386(16) 0.0306(18) -0.0113(14) 0.0058(14) 0.0055(13) C33 0.0355(19) 0.0521(19) 0.0222(17) -0.0041(14) 0.0129(14) 0.0131(15) C34 0.0314(18) 0.0415(16) 0.0287(17) 0.0075(14) 0.0166(14) 0.0093(13) C35 0.0229(16) 0.0283(13) 0.0279(16) 0.0006(12) 0.0103(13) 0.0053(11) C36 0.0166(13) 0.0143(10) 0.0111(12) 0.0001(9) 0.0037(10) 0.0021(9) C37 0.0175(14) 0.0198(11) 0.0154(13) 0.0035(10) 0.0034(11) 0.0057(10) C38 0.0243(15) 0.0202(12) 0.0183(14) 0.0023(10) 0.0044(12) 0.0054(10) C39 0.0307(17) 0.0291(14) 0.0242(16) 0.0052(12) 0.0143(13) 0.0122(12) C40 0.0199(15) 0.0344(15) 0.0333(18) 0.0097(13) 0.0100(13) 0.0050(12) C41 0.0219(16) 0.0245(13) 0.0300(17) -0.0009(12) 0.0062(13) -0.0022(11) C42 0.0234(15) 0.0224(12) 0.0203(14) 0.0024(11) 0.0087(12) 0.0064(11) C43 0.0208(15) 0.0201(12) 0.0204(14) 0.0020(11) 0.0060(11) 0.0056(10) C44 0.0231(15) 0.0249(13) 0.0223(15) 0.0024(11) 0.0102(12) 0.0080(11) C45 0.0300(17) 0.0341(15) 0.0183(15) 0.0045(12) 0.0017(13) 0.0087(13) C46 0.043(2) 0.0342(15) 0.0233(16) 0.0075(13) 0.0155(15) 0.0061(14) C47 0.0271(17) 0.0305(14) 0.0368(18) 0.0095(13) 0.0175(14) 0.0042(12) C48 0.0220(15) 0.0252(13) 0.0253(16) 0.0066(12) 0.0047(12) 0.0047(11) C49 0.0217(15) 0.0211(12) 0.0165(14) 0.0051(10) 0.0030(11) 0.0021(10) C50 0.0193(14) 0.0239(12) 0.0175(14) 0.0041(11) -0.0005(11) 0.0022(10) C51 0.0298(16) 0.0241(13) 0.0235(15) 0.0092(11) 0.0081(13) 0.0074(11) C52 0.0332(17) 0.0193(12) 0.0252(16) 0.0012(11) 0.0054(13) -0.0032(11) C53 0.0193(15) 0.0289(14) 0.0211(15) 0.0034(12) -0.0024(12) -0.0036(11) C54 0.0187(14) 0.0260(13) 0.0203(14) 0.0074(11) -0.0001(11) 0.0046(11) C55 0.0133(13) 0.0232(12) 0.0269(15) 0.0074(11) 0.0049(11) 0.0017(10) C56 0.0200(15) 0.0274(14) 0.045(2) 0.0112(13) 0.0146(14) 0.0084(11) C57 0.0279(18) 0.0269(15) 0.071(3) 0.0170(16) 0.0237(18) 0.0128(13) C58 0.0203(17) 0.0389(17) 0.069(3) 0.0334(18) 0.0105(16) 0.0102(13) C59 0.0218(16) 0.0411(17) 0.041(2) 0.0239(15) -0.0022(14) -0.0001(13) C60 0.0174(14) 0.0256(13) 0.0304(17) 0.0095(12) 0.0020(12) 0.0010(11) C61 0.039(2) 0.0423(19) 0.074(3) 0.0134(19) 0.034(2) 0.0074(16) C62 0.039(2) 0.051(2) 0.087(4) 0.002(2) 0.023(2) -0.0008(18) C63 0.056(3) 0.070(3) 0.131(5) -0.004(3) 0.035(3) -0.013(2) C64 0.104(6) 0.050(3) 0.248(10) -0.012(5) 0.106(7) -0.010(3) C65 0.134(6) 0.054(3) 0.201(8) 0.052(4) 0.119(6) 0.024(3) C66 0.081(3) 0.063(3) 0.100(4) 0.035(3) 0.062(3) 0.026(2) B1 0.0181(16) 0.0206(13) 0.0165(15) 0.0028(11) 0.0044(12) 0.0028(11) _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 O1 2.0373(17) . ? Hf1 O2 2.0586(16) . ? Hf1 N2 2.223(2) 2_566 ? Hf1 N1 2.225(2) . ? Hf1 C29 2.240(3) . ? Hf1 S1 2.7211(6) . ? Br1 C61 1.893(4) . ? S1 C6 1.798(3) . ? S1 C8 1.807(3) 2_566 ? P1 N1 1.633(2) . ? P1 C1 1.793(3) . ? P1 C2 1.795(3) . ? P1 C36 1.878(2) . ? P2 N2 1.624(2) . ? P2 C4 1.791(3) . ? P2 C3 1.802(3) . ? P2 C36 1.880(2) . ? F1 C38 1.349(3) . ? F2 C39 1.337(3) . ? F3 C40 1.344(3) . ? F4 C41 1.348(3) . ? F5 C42 1.348(3) . ? F6 C44 1.355(3) . ? F7 C45 1.347(3) . ? F8 C46 1.340(3) . ? F9 C47 1.351(3) . ? F10 C48 1.351(3) . ? F11 C50 1.359(3) . ? F12 C51 1.342(3) . ? F13 C52 1.346(3) . ? F14 C53 1.350(3) . ? F15 C54 1.353(3) . ? F16 C56 1.350(4) . ? F17 C57 1.359(4) . ? F18 C58 1.341(3) . ? F19 C59 1.345(4) . ? F20 C60 1.352(3) . ? O1 C36 1.383(3) . ? O2 C36 1.369(3) 2_566 ? N1 C5 1.492(3) . ? N2 C7 1.484(3) . ? N2 Hf1 2.223(2) 2_566 ? C1 C13 1.399(4) . ? C1 C9 1.400(4) . ? C2 C18 1.385(4) . ? C2 C14 1.391(4) . ? C3 C23 1.391(4) . ? C3 C19 1.399(4) . ? C4 C24 1.399(4) . ? C4 C28 1.401(4) . ? C5 C6 1.509(4) . ? C7 C8 1.494(4) . ? C8 S1 1.807(3) 2_566 ? C9 C10 1.378(4) . ? C10 C11 1.395(4) . ? C11 C12 1.375(5) . ? C12 C13 1.384(4) . ? C14 C15 1.377(4) . ? C15 C16 1.387(4) . ? C16 C17 1.373(5) . ? C17 C18 1.387(4) . ? C19 C20 1.382(4) . ? C20 C21 1.381(5) . ? C21 C22 1.371(5) . ? C22 C23 1.390(4) . ? C24 C25 1.396(4) . ? C25 C26 1.380(4) . ? C26 C27 1.385(4) . ? C27 C28 1.390(4) . ? C29 C30 1.480(4) . ? C30 C35 1.400(4) . ? C30 C31 1.404(4) . ? C31 C32 1.384(4) . ? C32 C33 1.387(5) . ? C33 C34 1.378(5) . ? C34 C35 1.383(4) . ? C36 O2 1.369(3) 2_566 ? C37 C38 1.386(4) . ? C37 C42 1.394(4) . ? C37 B1 1.657(4) . ? C38 C39 1.384(4) . ? C39 C40 1.383(4) . ? C40 C41 1.373(4) . ? C41 C42 1.375(4) . ? C43 C44 1.386(4) . ? C43 C48 1.389(4) . ? C43 B1 1.648(4) . ? C44 C45 1.389(4) . ? C45 C46 1.370(5) . ? C46 C47 1.377(4) . ? C47 C48 1.378(4) . ? C49 C54 1.383(4) . ? C49 C50 1.394(4) . ? C49 B1 1.659(4) . ? C50 C51 1.379(4) . ? C51 C52 1.373(4) . ? C52 C53 1.372(4) . ? C53 C54 1.382(4) . ? C55 C60 1.385(4) . ? C55 C56 1.393(4) . ? C55 B1 1.662(4) . ? C56 C57 1.376(4) . ? C57 C58 1.370(5) . ? C58 C59 1.367(5) . ? C59 C60 1.390(4) . ? C61 C62 1.366(6) . ? C61 C66 1.380(6) . ? C62 C63 1.390(6) . ? C63 C64 1.341(10) . ? C64 C65 1.459(10) . ? C65 C66 1.381(8) . ? 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 O1 Hf1 O2 82.92(7) . . ? O1 Hf1 N2 133.32(8) . 2_566 ? O2 Hf1 N2 75.10(7) . 2_566 ? O1 Hf1 N1 75.65(7) . . ? O2 Hf1 N1 151.53(8) . . ? N2 Hf1 N1 106.53(8) 2_566 . ? O1 Hf1 C29 94.42(9) . . ? O2 Hf1 C29 91.59(8) . . ? N2 Hf1 C29 126.33(9) 2_566 . ? N1 Hf1 C29 108.36(9) . . ? O1 Hf1 S1 145.69(5) . . ? O2 Hf1 S1 131.08(5) . . ? N2 Hf1 S1 70.71(5) 2_566 . ? N1 Hf1 S1 73.33(6) . . ? C29 Hf1 S1 81.84(7) . . ? C6 S1 C8 102.57(16) . 2_566 ? C6 S1 Hf1 97.93(10) . . ? C8 S1 Hf1 95.09(9) 2_566 . ? N1 P1 C1 110.96(13) . . ? N1 P1 C2 113.75(12) . . ? C1 P1 C2 111.49(13) . . ? N1 P1 C36 100.34(11) . . ? C1 P1 C36 112.43(11) . . ? C2 P1 C36 107.36(12) . . ? N2 P2 C4 114.85(12) . . ? N2 P2 C3 109.95(11) . . ? C4 P2 C3 109.66(12) . . ? N2 P2 C36 96.67(11) . . ? C4 P2 C36 109.46(11) . . ? C3 P2 C36 115.91(12) . . ? C36 O1 Hf1 128.74(14) . . ? C36 O2 Hf1 112.95(13) 2_566 . ? C5 N1 P1 111.76(17) . . ? C5 N1 Hf1 127.45(17) . . ? P1 N1 Hf1 120.17(10) . . ? C7 N2 P2 114.54(18) . . ? C7 N2 Hf1 128.08(17) . 2_566 ? P2 N2 Hf1 117.23(10) . 2_566 ? C13 C1 C9 119.3(3) . . ? C13 C1 P1 124.6(2) . . ? C9 C1 P1 116.1(2) . . ? C18 C2 C14 119.4(3) . . ? C18 C2 P1 117.7(2) . . ? C14 C2 P1 122.6(2) . . ? C23 C3 C19 119.0(3) . . ? C23 C3 P2 122.7(2) . . ? C19 C3 P2 118.2(2) . . ? C24 C4 C28 119.5(2) . . ? C24 C4 P2 118.3(2) . . ? C28 C4 P2 122.1(2) . . ? N1 C5 C6 110.7(2) . . ? C5 C6 S1 112.1(2) . . ? N2 C7 C8 109.6(2) . . ? C7 C8 S1 108.3(2) . 2_566 ? C10 C9 C1 120.4(3) . . ? C9 C10 C11 119.7(3) . . ? C12 C11 C10 120.2(3) . . ? C11 C12 C13 120.7(3) . . ? C12 C13 C1 119.7(3) . . ? C15 C14 C2 120.2(3) . . ? C14 C15 C16 120.3(3) . . ? C17 C16 C15 119.6(3) . . ? C16 C17 C18 120.5(3) . . ? C2 C18 C17 120.0(3) . . ? C20 C19 C3 120.2(3) . . ? C21 C20 C19 120.0(3) . . ? C22 C21 C20 120.5(3) . . ? C21 C22 C23 120.0(3) . . ? C22 C23 C3 120.2(3) . . ? C25 C24 C4 119.6(3) . . ? C26 C25 C24 120.4(3) . . ? C25 C26 C27 120.6(3) . . ? C26 C27 C28 119.7(3) . . ? C27 C28 C4 120.3(3) . . ? C30 C29 Hf1 119.61(18) . . ? C35 C30 C31 116.8(3) . . ? C35 C30 C29 122.2(2) . . ? C31 C30 C29 121.0(3) . . ? C32 C31 C30 121.5(3) . . ? C31 C32 C33 120.1(3) . . ? C34 C33 C32 119.7(3) . . ? C33 C34 C35 120.2(3) . . ? C34 C35 C30 121.7(3) . . ? O2 C36 O1 113.3(2) 2_566 . ? O2 C36 P1 106.59(15) 2_566 . ? O1 C36 P1 105.28(16) . . ? O2 C36 P2 101.59(15) 2_566 . ? O1 C36 P2 106.54(15) . . ? P1 C36 P2 123.80(13) . . ? C38 C37 C42 113.2(2) . . ? C38 C37 B1 126.4(2) . . ? C42 C37 B1 119.8(2) . . ? F1 C38 C39 114.5(2) . . ? F1 C38 C37 121.2(2) . . ? C39 C38 C37 124.3(2) . . ? F2 C39 C40 119.6(3) . . ? F2 C39 C38 120.9(3) . . ? C40 C39 C38 119.5(3) . . ? F3 C40 C41 120.8(3) . . ? F3 C40 C39 120.4(3) . . ? C41 C40 C39 118.8(3) . . ? F4 C41 C40 119.4(3) . . ? F4 C41 C42 121.0(3) . . ? C40 C41 C42 119.6(3) . . ? F5 C42 C41 116.1(2) . . ? F5 C42 C37 119.4(2) . . ? C41 C42 C37 124.6(3) . . ? C44 C43 C48 113.2(3) . . ? C44 C43 B1 126.8(2) . . ? C48 C43 B1 119.8(2) . . ? F6 C44 C43 121.2(2) . . ? F6 C44 C45 115.0(3) . . ? C43 C44 C45 123.9(3) . . ? F7 C45 C46 119.5(3) . . ? F7 C45 C44 120.4(3) . . ? C46 C45 C44 120.1(3) . . ? F8 C46 C45 120.5(3) . . ? F8 C46 C47 121.0(3) . . ? C45 C46 C47 118.5(3) . . ? F9 C47 C46 119.3(3) . . ? F9 C47 C48 121.0(3) . . ? C46 C47 C48 119.6(3) . . ? F10 C48 C47 115.9(3) . . ? F10 C48 C43 119.5(3) . . ? C47 C48 C43 124.6(3) . . ? C54 C49 C50 113.1(2) . . ? C54 C49 B1 127.7(2) . . ? C50 C49 B1 118.9(2) . . ? F11 C50 C51 115.8(2) . . ? F11 C50 C49 119.2(2) . . ? C51 C50 C49 125.1(3) . . ? F12 C51 C52 120.2(2) . . ? F12 C51 C50 121.1(3) . . ? C52 C51 C50 118.8(3) . . ? F13 C52 C53 120.4(3) . . ? F13 C52 C51 120.4(3) . . ? C53 C52 C51 119.1(2) . . ? F14 C53 C52 119.5(2) . . ? F14 C53 C54 120.4(3) . . ? C52 C53 C54 120.1(3) . . ? F15 C54 C53 115.4(2) . . ? F15 C54 C49 120.7(2) . . ? C53 C54 C49 123.9(3) . . ? C60 C55 C56 113.5(3) . . ? C60 C55 B1 120.1(2) . . ? C56 C55 B1 125.7(3) . . ? F16 C56 C57 115.3(3) . . ? F16 C56 C55 121.1(2) . . ? C57 C56 C55 123.5(3) . . ? F17 C57 C58 119.6(3) . . ? F17 C57 C56 119.8(3) . . ? C58 C57 C56 120.6(3) . . ? F18 C58 C59 120.9(4) . . ? F18 C58 C57 120.5(3) . . ? C59 C58 C57 118.5(3) . . ? F19 C59 C58 120.2(3) . . ? F19 C59 C60 120.2(3) . . ? C58 C59 C60 119.6(3) . . ? F20 C60 C55 119.8(2) . . ? F20 C60 C59 116.0(3) . . ? C55 C60 C59 124.2(3) . . ? C62 C61 C66 123.0(4) . . ? C62 C61 Br1 118.8(3) . . ? C66 C61 Br1 118.2(4) . . ? C61 C62 C63 119.9(5) . . ? C64 C63 C62 120.5(7) . . ? C63 C64 C65 118.9(6) . . ? C66 C65 C64 120.6(6) . . ? C61 C66 C65 117.0(6) . . ? C43 B1 C37 114.1(2) . . ? C43 B1 C49 101.7(2) . . ? C37 B1 C49 113.5(2) . . ? C43 B1 C55 113.6(2) . . ? C37 B1 C55 100.75(19) . . ? C49 B1 C55 113.9(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.312 _refine_diff_density_min -1.560 _refine_diff_density_rms 0.091