# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2008 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Greg Robinson' _publ_contact_author_address ; Department of Chemistry University of Georgia Athens GA 30602 UNITED STATES OF AMERICA ; _publ_contact_author_email ROBINSON@CHEM.UGA.EDU _publ_section_title ; Organometallic Compounds Containing new Hf-Ga and Hf-In Bonds: Cp2Hf(ER)2 (Cp = C5H5; E = Ga, In; R = -C6H3-2,6-(2,4,6-i-Pr3C6H2)2) ; loop_ _publ_author_name 'Greg Robinson' 'Brandon Quillian' 'Yuzhong Wang.' 'Pingrong Wei.' data_uga615 _database_code_depnum_ccdc_archive 'CCDC 666750' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H118 Ga2 Hf O' _chemical_formula_weight 1485.74 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' Ga Ga 0.2307 1.6083 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.879(4) _cell_length_b 17.556(4) _cell_length_c 29.381(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8191(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 5363 _cell_measurement_theta_min 2.216 _cell_measurement_theta_max 18.805 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 1.958 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6955 _exptl_absorpt_correction_T_max 0.9084 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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' _diffrn_measurement_method OMEGA-SCAN _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 41723 _diffrn_reflns_av_R_equivalents 0.1355 _diffrn_reflns_av_sigmaI/netI 0.0950 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7217 _reflns_number_gt 3120 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0954P)^2^+34.2000P] 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 7217 _refine_ls_number_parameters 431 _refine_ls_number_restraints 141 _refine_ls_R_factor_all 0.1602 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.2307 _refine_ls_wR_factor_gt 0.1563 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.000 _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 0.0000 0.21574(3) 0.7500 0.0524(2) Uani 1 2 d S . . Ga1 Ga 0.00390(10) 0.12058(7) 0.68135(4) 0.0671(4) Uani 1 1 d . . . C1 C 0.0129(7) 0.0602(6) 0.6230(3) 0.050(3) Uani 1 1 d . . . C2 C -0.0543(7) 0.0153(6) 0.6081(4) 0.052(3) Uani 1 1 d . . . C3 C -0.0473(8) -0.0343(7) 0.5729(4) 0.067(4) Uani 1 1 d . . . H3 H -0.0930 -0.0641 0.5643 0.080 Uiso 1 1 calc R . . C4 C 0.0306(7) -0.0404(7) 0.5490(4) 0.065(3) Uani 1 1 d . . . H4 H 0.0367 -0.0748 0.5252 0.078 Uiso 1 1 calc R . . C5 C 0.0963(7) 0.0056(7) 0.5618(4) 0.058(3) Uani 1 1 d . . . H5 H 0.1469 0.0029 0.5459 0.070 Uiso 1 1 calc R . . C6 C 0.0888(7) 0.0565(6) 0.5983(4) 0.052(3) Uani 1 1 d . . . C7 C 0.1617(7) 0.1089(7) 0.6069(4) 0.054(3) Uani 1 1 d . . . C8 C 0.1577(8) 0.1827(8) 0.5894(4) 0.069(4) Uani 1 1 d . . . C9 C 0.2296(9) 0.2295(7) 0.5955(5) 0.080(4) Uani 1 1 d . . . H9 H 0.2282 0.2786 0.5836 0.096 Uiso 1 1 calc R . . C10 C 0.2992(8) 0.2070(9) 0.6172(5) 0.075(4) Uani 1 1 d . . . C11 C 0.2989(8) 0.1352(9) 0.6348(4) 0.074(4) Uani 1 1 d . . . H11 H 0.3460 0.1192 0.6511 0.088 Uiso 1 1 calc R . . C12 C 0.2318(8) 0.0841(7) 0.6299(4) 0.062(3) Uani 1 1 d . . . C13 C 0.2403(8) 0.0054(8) 0.6483(5) 0.070(3) Uani 1 1 d . . . H13 H 0.1843 -0.0181 0.6476 0.084 Uiso 1 1 calc R . . C14 C 0.2992(9) -0.0448(8) 0.6202(6) 0.110(5) Uani 1 1 d . . . H14A H 0.3010 -0.0950 0.6331 0.164 Uiso 1 1 calc R . . H14B H 0.3548 -0.0232 0.6203 0.164 Uiso 1 1 calc R . . H14C H 0.2789 -0.0476 0.5895 0.164 Uiso 1 1 calc R . . C15 C 0.2723(11) 0.0005(9) 0.6972(5) 0.117(6) Uani 1 1 d . . . H15A H 0.2742 -0.0519 0.7065 0.176 Uiso 1 1 calc R . . H15B H 0.2350 0.0282 0.7169 0.176 Uiso 1 1 calc R . . H15C H 0.3277 0.0220 0.6989 0.176 Uiso 1 1 calc R . . C16 C 0.3752(11) 0.2621(11) 0.6223(7) 0.126(7) Uani 1 1 d . . . H16 H 0.3514 0.3069 0.6071 0.151 Uiso 1 1 calc R . . C17 C 0.4405(12) 0.2461(13) 0.5918(7) 0.170(10) Uani 1 1 d . . . H17A H 0.4172 0.2294 0.5633 0.255 Uiso 1 1 calc R . . H17B H 0.4757 0.2068 0.6041 0.255 Uiso 1 1 calc R . . H17C H 0.4734 0.2912 0.5869 0.255 Uiso 1 1 calc R . . C18 C 0.3849(12) 0.2917(12) 0.6652(7) 0.187(12) Uani 1 1 d . . . H18A H 0.3305 0.3010 0.6783 0.280 Uiso 1 1 calc R . . H18B H 0.4156 0.3388 0.6634 0.280 Uiso 1 1 calc R . . H18C H 0.4153 0.2562 0.6838 0.280 Uiso 1 1 calc R . . C19 C 0.0849(9) 0.2104(8) 0.5612(5) 0.084(4) Uani 1 1 d . . . H19 H 0.0386 0.1741 0.5652 0.100 Uiso 1 1 calc R . . C20 C 0.0534(13) 0.2876(10) 0.5762(7) 0.151(8) Uani 1 1 d . . . H20A H 0.0064 0.3023 0.5577 0.227 Uiso 1 1 calc R . . H20B H 0.0977 0.3244 0.5731 0.227 Uiso 1 1 calc R . . H20C H 0.0362 0.2850 0.6075 0.227 Uiso 1 1 calc R . . C21 C 0.1072(13) 0.2114(11) 0.5106(6) 0.146(8) Uani 1 1 d . . . H21A H 0.0592 0.2277 0.4933 0.219 Uiso 1 1 calc R . . H21B H 0.1234 0.1611 0.5011 0.219 Uiso 1 1 calc R . . H21C H 0.1531 0.2459 0.5055 0.219 Uiso 1 1 calc R . . C22 C -0.1409(7) 0.0254(7) 0.6300(4) 0.056(3) Uani 1 1 d . . . C23 C -0.1927(9) 0.0836(9) 0.6141(5) 0.076(4) Uani 1 1 d . . . C24 C -0.2724(9) 0.0899(9) 0.6325(5) 0.089(5) Uani 1 1 d . . . H24 H -0.3077 0.1282 0.6219 0.107 Uiso 1 1 calc R . . C25 C -0.3011(8) 0.0423(10) 0.6655(5) 0.087(5) Uani 1 1 d . . . C26 C -0.2498(8) -0.0137(9) 0.6791(5) 0.079(4) Uani 1 1 d . . . H26 H -0.2696 -0.0471 0.7012 0.095 Uiso 1 1 calc R . . C27 C -0.1690(7) -0.0252(7) 0.6625(4) 0.066(3) Uani 1 1 d . . . C28 C -0.1160(9) -0.0921(9) 0.6776(6) 0.099(5) Uani 1 1 d . . . H28 H -0.0579 -0.0838 0.6674 0.119 Uiso 1 1 calc R . . C29 C -0.1505(12) -0.1631(9) 0.6540(8) 0.156(9) Uani 1 1 d . . . H29A H -0.1177 -0.2066 0.6627 0.234 Uiso 1 1 calc R . . H29B H -0.1472 -0.1565 0.6216 0.234 Uiso 1 1 calc R . . H29C H -0.2081 -0.1707 0.6627 0.234 Uiso 1 1 calc R . . C30 C -0.1155(12) -0.1029(14) 0.7286(7) 0.176(11) Uani 1 1 d . . . H30A H -0.0812 -0.1461 0.7362 0.265 Uiso 1 1 calc R . . H30B H -0.1720 -0.1114 0.7391 0.265 Uiso 1 1 calc R . . H30C H -0.0930 -0.0581 0.7429 0.265 Uiso 1 1 calc R . . C31 C -0.3917(11) 0.0480(13) 0.6872(7) 0.131(7) Uani 1 1 d . . . H31 H -0.3880 0.0146 0.7139 0.158 Uiso 1 1 calc R . . C32 C -0.4022(13) 0.1261(13) 0.7075(9) 0.198(13) Uani 1 1 d . . . H32A H -0.3537 0.1383 0.7256 0.297 Uiso 1 1 calc R . . H32B H -0.4516 0.1269 0.7264 0.297 Uiso 1 1 calc R . . H32C H -0.4081 0.1629 0.6836 0.297 Uiso 1 1 calc R . . C33 C -0.4538(12) 0.0115(18) 0.6592(10) 0.252(17) Uani 1 1 d . . . H33A H -0.4349 -0.0387 0.6513 0.378 Uiso 1 1 calc R . . H33B H -0.4621 0.0408 0.6320 0.378 Uiso 1 1 calc R . . H33C H -0.5060 0.0080 0.6756 0.378 Uiso 1 1 calc R . . C34 C -0.1686(9) 0.1355(11) 0.5744(6) 0.097(5) Uani 1 1 d . . . H34 H -0.1082 0.1279 0.5693 0.116 Uiso 1 1 calc R . . C35 C -0.1803(15) 0.2211(11) 0.5842(7) 0.164(9) Uani 1 1 d . . . H35A H -0.1499 0.2345 0.6113 0.246 Uiso 1 1 calc R . . H35B H -0.2390 0.2319 0.5884 0.246 Uiso 1 1 calc R . . H35C H -0.1591 0.2502 0.5591 0.246 Uiso 1 1 calc R . . C36 C -0.2119(12) 0.1127(10) 0.5309(6) 0.134(7) Uani 1 1 d . . . H36A H -0.1938 0.1456 0.5067 0.201 Uiso 1 1 calc R . . H36B H -0.2717 0.1170 0.5346 0.201 Uiso 1 1 calc R . . H36C H -0.1976 0.0610 0.5236 0.201 Uiso 1 1 calc R . . C37 C -0.096(3) 0.323(2) 0.7435(17) 0.083(8) Uani 0.50 1 d PDU A 1 H37 H -0.0726 0.3712 0.7390 0.100 Uiso 0.50 1 calc PR A 1 C38 C -0.114(3) 0.290(3) 0.7865(13) 0.080(8) Uani 0.50 1 d PDU A 1 H38 H -0.1044 0.3105 0.8152 0.096 Uiso 0.50 1 calc PR A 1 C39 C -0.150(3) 0.217(3) 0.7751(17) 0.081(8) Uani 0.50 1 d PU A 1 H39 H -0.1691 0.1815 0.7960 0.097 Uiso 0.50 1 calc PR A 1 C40 C -0.152(3) 0.209(3) 0.7290(19) 0.082(8) Uani 0.50 1 d PU A 1 H40 H -0.1711 0.1657 0.7137 0.098 Uiso 0.50 1 calc PR A 1 C41 C -0.120(3) 0.273(3) 0.7089(16) 0.090(9) Uani 0.50 1 d PU A 1 H41 H -0.1158 0.2821 0.6778 0.108 Uiso 0.50 1 calc PR A 1 C37' C -0.103(3) 0.318(3) 0.7659(18) 0.087(8) Uani 0.50 1 d PDU B 2 H37' H -0.0856 0.3638 0.7787 0.105 Uiso 0.50 1 calc PR B 2 C38' C -0.134(3) 0.249(3) 0.7895(14) 0.084(8) Uani 0.50 1 d PU B 2 H38' H -0.1379 0.2421 0.8208 0.100 Uiso 0.50 1 calc PR B 2 C39' C -0.156(3) 0.196(3) 0.7564(18) 0.091(8) Uani 0.50 1 d PU B 2 H39' H -0.1781 0.1480 0.7624 0.109 Uiso 0.50 1 calc PR B 2 C40' C -0.142(4) 0.224(4) 0.7143(15) 0.088(9) Uani 0.50 1 d PU B 2 H40' H -0.1525 0.1997 0.6869 0.106 Uiso 0.50 1 calc PR B 2 C41' C -0.107(3) 0.298(3) 0.7193(17) 0.083(8) Uani 0.50 1 d PDU B 2 H41' H -0.0895 0.3290 0.6954 0.099 Uiso 0.50 1 calc PR B 2 O1 O 0.0000 0.5000 0.5000 0.150 Uiso 1 2 d S . . C42 C -0.0738 0.4632 0.5124 0.160 Uiso 0.50 1 d P C 1 H42A H -0.1061 0.4767 0.4856 0.192 Uiso 0.50 1 calc PR C 1 H42B H -0.0548 0.4118 0.5060 0.192 Uiso 0.50 1 calc PR C 1 C43 C -0.1389 0.4442 0.5386 0.160 Uiso 0.50 1 d P C 1 H43A H -0.1736 0.4079 0.5229 0.240 Uiso 0.50 1 calc PR C 1 H43B H -0.1714 0.4889 0.5454 0.240 Uiso 0.50 1 calc PR C 1 H43C H -0.1186 0.4221 0.5664 0.240 Uiso 0.50 1 calc PR C 1 C42' C -0.0466 0.4513 0.4738 0.160 Uiso 0.50 1 d P C 2 H42C H -0.0139 0.4053 0.4692 0.192 Uiso 0.50 1 calc PR C 2 H42D H -0.0545 0.4747 0.4442 0.192 Uiso 0.50 1 calc PR C 2 C43' C -0.1241 0.4307 0.4901 0.160 Uiso 0.50 1 d P C 2 H43D H -0.1507 0.3967 0.4689 0.240 Uiso 0.50 1 calc PR C 2 H43E H -0.1583 0.4753 0.4938 0.240 Uiso 0.50 1 calc PR C 2 H43F H -0.1176 0.4057 0.5189 0.240 Uiso 0.50 1 calc PR C 2 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 0.0665(4) 0.0463(3) 0.0444(3) 0.000 0.0061(5) 0.000 Ga1 0.0696(9) 0.0655(8) 0.0662(8) -0.0070(6) 0.0046(9) -0.0005(10) C1 0.057(8) 0.042(5) 0.050(6) -0.010(5) -0.003(6) 0.004(6) C2 0.050(7) 0.054(7) 0.052(7) -0.001(6) 0.004(6) -0.001(6) C3 0.057(8) 0.070(9) 0.075(9) -0.005(7) -0.007(7) -0.019(7) C4 0.058(7) 0.065(8) 0.070(8) -0.013(7) 0.013(6) 0.002(6) C5 0.041(6) 0.070(8) 0.065(8) -0.004(7) 0.013(6) -0.002(6) C6 0.050(7) 0.057(7) 0.051(7) -0.007(6) -0.008(6) 0.011(6) C7 0.046(7) 0.057(8) 0.060(8) -0.006(7) 0.011(6) -0.012(6) C8 0.056(8) 0.073(9) 0.079(9) 0.002(8) -0.001(7) -0.021(7) C9 0.094(11) 0.060(9) 0.086(10) -0.005(7) 0.028(9) -0.022(8) C10 0.050(8) 0.088(11) 0.087(10) -0.030(9) 0.007(7) -0.022(8) C11 0.057(8) 0.092(11) 0.071(9) -0.018(8) 0.000(7) -0.001(8) C12 0.057(8) 0.059(8) 0.070(9) -0.012(7) 0.009(7) -0.014(7) C13 0.054(8) 0.082(9) 0.076(9) -0.002(8) 0.004(7) 0.001(7) C14 0.091(11) 0.085(11) 0.153(16) -0.011(11) -0.002(11) 0.013(9) C15 0.149(16) 0.102(12) 0.101(13) 0.021(11) -0.019(12) 0.006(12) C16 0.092(13) 0.147(17) 0.138(17) -0.062(14) 0.025(12) -0.059(12) C17 0.121(16) 0.22(2) 0.17(2) -0.039(18) 0.061(15) -0.119(17) C18 0.136(17) 0.23(3) 0.19(2) -0.12(2) 0.028(16) -0.111(17) C19 0.087(10) 0.065(9) 0.099(11) 0.022(8) -0.013(9) -0.011(8) C20 0.143(17) 0.120(16) 0.19(2) -0.022(15) -0.075(17) 0.038(13) C21 0.168(19) 0.18(2) 0.089(13) 0.013(13) -0.035(13) -0.043(15) C22 0.042(6) 0.055(7) 0.070(8) -0.013(6) -0.004(6) -0.001(6) C23 0.060(9) 0.094(11) 0.074(10) -0.006(9) -0.003(8) -0.004(9) C24 0.067(10) 0.102(12) 0.098(11) -0.003(10) -0.003(9) 0.033(9) C25 0.039(8) 0.126(14) 0.096(12) -0.010(11) 0.017(8) 0.002(9) C26 0.051(8) 0.109(12) 0.079(10) -0.002(9) 0.008(8) -0.014(8) C27 0.048(7) 0.069(8) 0.080(9) -0.001(7) 0.008(7) -0.007(6) C28 0.060(9) 0.094(12) 0.142(15) 0.030(11) 0.032(9) 0.004(9) C29 0.152(18) 0.074(12) 0.24(3) 0.010(15) 0.043(18) -0.014(12) C30 0.118(16) 0.27(3) 0.144(17) 0.119(19) 0.017(14) 0.068(17) C31 0.081(12) 0.16(2) 0.148(18) 0.007(15) 0.019(12) 0.039(13) C32 0.16(2) 0.17(2) 0.26(3) 0.08(2) 0.14(2) 0.079(18) C33 0.047(11) 0.40(5) 0.31(4) 0.08(3) -0.013(18) -0.03(2) C34 0.063(10) 0.126(15) 0.102(13) 0.018(12) -0.005(9) 0.032(10) C35 0.25(3) 0.115(18) 0.129(17) 0.037(14) 0.011(18) 0.012(18) C36 0.159(18) 0.151(17) 0.093(13) 0.011(12) 0.023(13) 0.047(14) C37 0.103(16) 0.082(13) 0.065(19) -0.007(15) 0.014(18) 0.034(12) C38 0.095(17) 0.075(18) 0.069(13) -0.012(14) 0.034(15) 0.041(15) C39 0.071(16) 0.104(18) 0.066(17) -0.007(16) 0.013(17) 0.016(15) C40 0.057(15) 0.124(17) 0.064(18) 0.006(17) -0.004(18) -0.007(14) C41 0.095(18) 0.11(2) 0.069(13) 0.002(14) -0.003(15) 0.002(17) C37' 0.107(17) 0.084(15) 0.071(19) -0.009(16) 0.02(2) 0.042(14) C38' 0.079(17) 0.10(2) 0.069(14) -0.004(15) 0.026(14) 0.035(17) C39' 0.077(15) 0.121(16) 0.07(2) 0.006(15) 0.009(19) -0.003(14) C40' 0.089(18) 0.106(19) 0.069(15) 0.008(16) -0.012(17) -0.002(16) C41' 0.099(18) 0.081(18) 0.068(16) 0.003(15) -0.003(17) 0.026(15) _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 C41' 2.41(5) 3_556 ? Hf1 C37 2.44(4) 3_556 ? Hf1 C37' 2.48(4) 3_556 ? Hf1 C40 2.49(5) 3_556 ? Hf1 C38 2.47(3) 3_556 ? Hf1 C38' 2.49(4) 3_556 ? Hf1 C40' 2.49(6) 3_556 ? Hf1 C39 2.49(5) 3_556 ? Hf1 C41 2.48(5) 3_556 ? Hf1 C39' 2.51(5) 3_556 ? Hf1 Ga1 2.6199(13) . ? Hf1 Ga1 2.6199(13) 3_556 ? Ga1 C1 2.022(10) . ? C1 C2 1.396(14) . ? C1 C6 1.408(14) . ? C2 C3 1.358(15) . ? C2 C22 1.527(15) . ? C3 C4 1.426(16) . ? C4 C5 1.372(15) . ? C5 C6 1.401(14) . ? C6 C7 1.500(15) . ? C7 C12 1.374(16) . ? C7 C8 1.394(16) . ? C8 C9 1.418(17) . ? C8 C19 1.504(18) . ? C9 C10 1.336(18) . ? C10 C11 1.364(18) . ? C10 C16 1.555(18) . ? C11 C12 1.400(16) . ? C12 C13 1.490(17) . ? C13 C14 1.528(17) . ? C13 C15 1.524(17) . ? C16 C18 1.37(2) . ? C16 C17 1.40(2) . ? C19 C21 1.53(2) . ? C19 C20 1.510(19) . ? C22 C27 1.379(16) . ? C22 C23 1.393(17) . ? C23 C24 1.380(18) . ? C23 C34 1.53(2) . ? C24 C25 1.358(19) . ? C25 C26 1.339(19) . ? C25 C31 1.577(19) . ? C26 C27 1.387(17) . ? C27 C28 1.512(18) . ? C28 C30 1.51(2) . ? C28 C29 1.53(2) . ? C31 C33 1.44(3) . ? C31 C32 1.50(3) . ? C34 C36 1.51(2) . ? C34 C35 1.54(2) . ? C37 C41 1.40(5) . ? C37 C38 1.42(3) . ? C38 C39 1.44(5) . ? C39 C40 1.36(5) . ? C40 C41 1.37(6) . ? C37' C41' 1.41(4) . ? C37' C38' 1.48(5) . ? C38' C39' 1.39(5) . ? C39' C40' 1.35(5) . ? C40' C41' 1.41(6) . ? O1 C42' 1.36788(18) 5_566 ? O1 C42' 1.36789(17) . ? O1 C42 1.3869(2) 5_566 ? O1 C42 1.3869(2) . ? C42 C43 1.3313(2) . ? C42' C43' 1.3691(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C41' Hf1 C37 20.3(11) 3_556 3_556 ? C41' Hf1 C37' 33.6(10) 3_556 3_556 ? C37 Hf1 C37' 15.7(9) 3_556 3_556 ? C41' Hf1 C40 41.8(15) 3_556 3_556 ? C37 Hf1 C40 54.0(17) 3_556 3_556 ? C37' Hf1 C40 56.1(17) 3_556 3_556 ? C41' Hf1 C38 47.9(14) 3_556 3_556 ? C37 Hf1 C38 33.6(9) 3_556 3_556 ? C37' Hf1 C38 18.5(10) 3_556 3_556 ? C40 Hf1 C38 55.0(15) 3_556 3_556 ? C41' Hf1 C38' 55.3(14) 3_556 3_556 ? C37 Hf1 C38' 47.1(12) 3_556 3_556 ? C37' Hf1 C38' 34.7(12) 3_556 3_556 ? C40 Hf1 C38' 45.6(15) 3_556 3_556 ? C38 Hf1 C38' 18.4(11) 3_556 3_556 ? C41' Hf1 C40' 33.5(13) 3_556 3_556 ? C37 Hf1 C40' 49.6(15) 3_556 3_556 ? C37' Hf1 C40' 55.6(17) 3_556 3_556 ? C40 Hf1 C40' 12.4(12) 3_556 3_556 ? C38 Hf1 C40' 59.3(17) 3_556 3_556 ? C38' Hf1 C40' 53.8(15) 3_556 3_556 ? C41' Hf1 C39 55.2(17) 3_556 3_556 ? C37 Hf1 C39 54.2(16) 3_556 3_556 ? C37' Hf1 C39 45.9(14) 3_556 3_556 ? C40 Hf1 C39 31.7(12) 3_556 3_556 ? C38 Hf1 C39 33.7(11) 3_556 3_556 ? C38' Hf1 C39 17.1(11) 3_556 3_556 ? C40' Hf1 C39 42.3(14) 3_556 3_556 ? C41' Hf1 C41 13.3(12) 3_556 3_556 ? C37 Hf1 C41 33.0(11) 3_556 3_556 ? C37' Hf1 C41 44.3(14) 3_556 3_556 ? C40 Hf1 C41 32.1(13) 3_556 3_556 ? C38 Hf1 C41 55.4(14) 3_556 3_556 ? C38' Hf1 C41 58.2(17) 3_556 3_556 ? C40' Hf1 C41 21.7(14) 3_556 3_556 ? C39 Hf1 C41 53.3(16) 3_556 3_556 ? C41' Hf1 C39' 54.0(16) 3_556 3_556 ? C37 Hf1 C39' 59.5(15) 3_556 3_556 ? C37' Hf1 C39' 55.3(15) 3_556 3_556 ? C40 Hf1 C39' 19.2(11) 3_556 3_556 ? C38 Hf1 C39' 47.0(12) 3_556 3_556 ? C38' Hf1 C39' 32.2(11) 3_556 3_556 ? C40' Hf1 C39' 31.4(11) 3_556 3_556 ? C39 Hf1 C39' 15.4(10) 3_556 3_556 ? C41 Hf1 C39' 47.9(14) 3_556 3_556 ? C41' Hf1 Ga1 130.9(11) 3_556 . ? C37 Hf1 Ga1 122.7(10) 3_556 . ? C37' Hf1 Ga1 107.6(13) 3_556 . ? C40 Hf1 Ga1 97.8(11) 3_556 . ? C38 Hf1 Ga1 89.2(12) 3_556 . ? C38' Hf1 Ga1 76.7(11) 3_556 . ? C40' Hf1 Ga1 110.0(12) 3_556 . ? C39 Hf1 Ga1 75.9(11) 3_556 . ? C41 Hf1 Ga1 128.1(14) 3_556 . ? C39' Hf1 Ga1 80.3(12) 3_556 . ? C41' Hf1 Ga1 96.4(12) 3_556 3_556 ? C37 Hf1 Ga1 116.6(12) 3_556 3_556 ? C37' Hf1 Ga1 128.5(11) 3_556 3_556 ? C40 Hf1 Ga1 78.5(13) 3_556 3_556 ? C38 Hf1 Ga1 133.4(10) 3_556 3_556 ? C38' Hf1 Ga1 121.8(13) 3_556 3_556 ? C40' Hf1 Ga1 74.7(13) 3_556 3_556 ? C39 Hf1 Ga1 104.9(12) 3_556 3_556 ? C41 Hf1 Ga1 84.4(11) 3_556 3_556 ? C39' Hf1 Ga1 89.7(11) 3_556 3_556 ? Ga1 Hf1 Ga1 100.76(6) . 3_556 ? C1 Ga1 Hf1 171.6(3) . . ? C2 C1 C6 117.9(9) . . ? C2 C1 Ga1 120.4(8) . . ? C6 C1 Ga1 121.4(8) . . ? C3 C2 C1 122.5(10) . . ? C3 C2 C22 118.0(10) . . ? C1 C2 C22 119.5(10) . . ? C2 C3 C4 119.7(11) . . ? C5 C4 C3 118.7(11) . . ? C6 C5 C4 121.4(11) . . ? C5 C6 C1 119.7(10) . . ? C5 C6 C7 117.0(10) . . ? C1 C6 C7 123.1(10) . . ? C12 C7 C8 120.8(11) . . ? C12 C7 C6 120.9(11) . . ? C8 C7 C6 118.2(11) . . ? C7 C8 C9 117.1(13) . . ? C7 C8 C19 122.6(12) . . ? C9 C8 C19 120.0(13) . . ? C10 C9 C8 123.7(13) . . ? C9 C10 C11 116.9(12) . . ? C9 C10 C16 120.4(16) . . ? C11 C10 C16 122.8(15) . . ? C10 C11 C12 123.7(13) . . ? C7 C12 C11 117.7(12) . . ? C7 C12 C13 123.1(12) . . ? C11 C12 C13 119.2(13) . . ? C12 C13 C14 113.1(12) . . ? C12 C13 C15 115.1(12) . . ? C14 C13 C15 105.8(12) . . ? C18 C16 C17 125.6(18) . . ? C18 C16 C10 114.2(15) . . ? C17 C16 C10 112.9(14) . . ? C8 C19 C21 111.2(14) . . ? C8 C19 C20 112.5(13) . . ? C21 C19 C20 110.6(14) . . ? C27 C22 C23 120.9(12) . . ? C27 C22 C2 120.5(10) . . ? C23 C22 C2 118.4(11) . . ? C24 C23 C22 118.0(14) . . ? C24 C23 C34 118.8(14) . . ? C22 C23 C34 123.0(13) . . ? C23 C24 C25 122.6(14) . . ? C26 C25 C24 117.5(13) . . ? C26 C25 C31 118.7(16) . . ? C24 C25 C31 123.8(16) . . ? C25 C26 C27 124.4(14) . . ? C22 C27 C26 116.7(12) . . ? C22 C27 C28 121.6(11) . . ? C26 C27 C28 121.7(13) . . ? C27 C28 C30 113.1(14) . . ? C27 C28 C29 107.4(14) . . ? C30 C28 C29 110.5(16) . . ? C33 C31 C32 124(2) . . ? C33 C31 C25 111.4(18) . . ? C32 C31 C25 108.6(17) . . ? C36 C34 C23 112.0(15) . . ? C36 C34 C35 111.3(15) . . ? C23 C34 C35 114.1(15) . . ? C41 C37 C38 110(4) . . ? C37 C38 C39 104(4) . . ? C40 C39 C38 110(4) . . ? C39 C40 C41 109(5) . . ? C40 C41 C37 108(5) . . ? C41' C37' C38' 104(4) . . ? C39' C38' C37' 108(4) . . ? C40' C39' C38' 111(4) . . ? C39' C40' C41' 108(4) . . ? C37' C41' C40' 110(4) . . ? C42' O1 C42' 180.0 5_566 . ? C42' O1 C42 53.099(10) 5_566 5_566 ? C42' O1 C42 126.901(10) . 5_566 ? C42' O1 C42 126.901(10) 5_566 . ? C42' O1 C42 53.099(10) . . ? C42 O1 C42 180.0 5_566 . ? C43 C42 O1 157.623(4) . . ? O1 C42' C43' 117.031(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.979 _refine_diff_density_min -2.310 _refine_diff_density_rms 0.113 # Attachment 'Compound_2_B718429H.cif' data_j1 _database_code_depnum_ccdc_archive 'CCDC 666751' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H118 Hf In2 O' _chemical_formula_weight 1575.94 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' In In -0.7276 1.3100 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.748(4) _cell_length_b 17.855(5) _cell_length_c 29.708(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8354(4) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3482 _cell_measurement_theta_min 2.203 _cell_measurement_theta_max 17.729 _exptl_crystal_description plate _exptl_crystal_colour black-blue _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3248 _exptl_absorpt_coefficient_mu 1.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8828 _exptl_absorpt_correction_T_max 0.8983 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 64198 _diffrn_reflns_av_R_equivalents 0.2256 _diffrn_reflns_av_sigmaI/netI 0.1174 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7353 _reflns_number_gt 2891 _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^)+(0.0764P)^2^+37.8513P] 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 7353 _refine_ls_number_parameters 431 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.1882 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.2080 _refine_ls_wR_factor_gt 0.1452 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hf1 Hf 0.0000 0.22980(4) 0.7500 0.0461(2) Uani 1 2 d S . . In1 In 0.00240(8) 0.12539(5) 0.68121(3) 0.0485(3) Uani 1 1 d . . . C1 C 0.0140(9) 0.0561(7) 0.6206(4) 0.045(3) Uani 1 1 d . . . C2 C -0.0537(9) 0.0115(8) 0.6056(4) 0.051(4) Uani 1 1 d . . . C3 C -0.0450(9) -0.0361(8) 0.5707(4) 0.052(4) Uani 1 1 d . . . H3 H -0.0901 -0.0665 0.5620 0.062 Uiso 1 1 calc R . . C4 C 0.0320(9) -0.0397(8) 0.5476(5) 0.051(4) Uani 1 1 d . . . H4 H 0.0378 -0.0732 0.5239 0.061 Uiso 1 1 calc R . . C5 C 0.0992(8) 0.0050(8) 0.5590(4) 0.052(4) Uani 1 1 d . . . H5 H 0.1497 0.0029 0.5428 0.062 Uiso 1 1 calc R . . C6 C 0.0907(8) 0.0533(8) 0.5951(4) 0.048(3) Uani 1 1 d . . . C7 C 0.1635(10) 0.1055(9) 0.6060(5) 0.050(4) Uani 1 1 d . . . C8 C 0.1608(10) 0.1783(10) 0.5889(5) 0.061(5) Uani 1 1 d . . . C9 C 0.2321(11) 0.2244(9) 0.5965(5) 0.072(5) Uani 1 1 d . . . H9 H 0.2323 0.2728 0.5849 0.086 Uiso 1 1 calc R . . C10 C 0.2999(11) 0.2002(11) 0.6201(5) 0.071(5) Uani 1 1 d . . . C11 C 0.3015(10) 0.1300(10) 0.6363(5) 0.068(5) Uani 1 1 d . . . H11 H 0.3494 0.1141 0.6518 0.081 Uiso 1 1 calc R . . C12 C 0.2342(11) 0.0798(11) 0.6307(5) 0.065(5) Uani 1 1 d . . . C13 C 0.2397(9) 0.0011(9) 0.6476(6) 0.065(4) Uani 1 1 d . . . H13 H 0.1837 -0.0218 0.6435 0.079 Uiso 1 1 calc R . . C14 C 0.3026(10) -0.0457(10) 0.6220(6) 0.108(7) Uani 1 1 d . . . H14A H 0.3020 -0.0959 0.6335 0.162 Uiso 1 1 calc R . . H14B H 0.3584 -0.0248 0.6254 0.162 Uiso 1 1 calc R . . H14C H 0.2875 -0.0462 0.5907 0.162 Uiso 1 1 calc R . . C15 C 0.2616(14) -0.0038(11) 0.6968(6) 0.116(8) Uani 1 1 d . . . H15A H 0.2212 0.0246 0.7139 0.174 Uiso 1 1 calc R . . H15B H 0.3175 0.0160 0.7016 0.174 Uiso 1 1 calc R . . H15C H 0.2600 -0.0552 0.7062 0.174 Uiso 1 1 calc R . . C16 C 0.3743(17) 0.2566(19) 0.6284(8) 0.128(9) Uani 1 1 d . . . H16 H 0.4108 0.2156 0.6387 0.5(5) Uiso 1 1 calc R . . C17 C 0.4243(19) 0.2667(18) 0.5922(9) 0.24(2) Uani 1 1 d . . . H17A H 0.4059 0.2343 0.5683 0.360 Uiso 1 1 calc R . . H17B H 0.4820 0.2552 0.6000 0.360 Uiso 1 1 calc R . . H17C H 0.4207 0.3179 0.5825 0.360 Uiso 1 1 calc R . . C18 C 0.3775(15) 0.2879(14) 0.6691(9) 0.172(12) Uani 1 1 d . . . H18A H 0.3329 0.2677 0.6875 0.258 Uiso 1 1 calc R . . H18B H 0.3703 0.3411 0.6664 0.258 Uiso 1 1 calc R . . H18C H 0.4314 0.2774 0.6827 0.258 Uiso 1 1 calc R . . C19 C 0.0882(10) 0.2072(9) 0.5608(6) 0.070(5) Uani 1 1 d . . . H19 H 0.0404 0.1727 0.5647 0.084 Uiso 1 1 calc R . . C20 C 0.0580(13) 0.2841(10) 0.5742(7) 0.127(8) Uani 1 1 d . . . H20A H 0.0119 0.2990 0.5550 0.190 Uiso 1 1 calc R . . H20B H 0.1038 0.3192 0.5712 0.190 Uiso 1 1 calc R . . H20C H 0.0390 0.2832 0.6049 0.190 Uiso 1 1 calc R . . C21 C 0.1144(14) 0.2042(11) 0.5113(6) 0.123(8) Uani 1 1 d . . . H21A H 0.0685 0.2218 0.4929 0.184 Uiso 1 1 calc R . . H21B H 0.1279 0.1535 0.5033 0.184 Uiso 1 1 calc R . . H21C H 0.1633 0.2354 0.5067 0.184 Uiso 1 1 calc R . . C22 C -0.1410(8) 0.0234(9) 0.6286(4) 0.049(4) Uani 1 1 d . . . C23 C -0.1919(11) 0.0840(10) 0.6142(6) 0.062(5) Uani 1 1 d . . . C24 C -0.2696(11) 0.0924(11) 0.6354(6) 0.079(6) Uani 1 1 d . . . H24 H -0.3046 0.1319 0.6270 0.094 Uiso 1 1 calc R . . C25 C -0.2972(10) 0.0433(11) 0.6691(6) 0.072(5) Uani 1 1 d . . . C26 C -0.2465(11) -0.0134(11) 0.6798(6) 0.082(6) Uani 1 1 d . . . H26 H -0.2648 -0.0466 0.7019 0.099 Uiso 1 1 calc R . . C27 C -0.1677(9) -0.0261(9) 0.6601(5) 0.057(4) Uani 1 1 d . . . C28 C -0.1158(10) -0.0942(10) 0.6737(6) 0.078(5) Uani 1 1 d . . . H28 H -0.0574 -0.0870 0.6631 0.094 Uiso 1 1 calc R . . C29 C -0.1527(13) -0.1660(10) 0.6505(7) 0.122(8) Uani 1 1 d . . . H29A H -0.1200 -0.2089 0.6593 0.183 Uiso 1 1 calc R . . H29B H -0.1499 -0.1602 0.6184 0.183 Uiso 1 1 calc R . . H29C H -0.2107 -0.1728 0.6594 0.183 Uiso 1 1 calc R . . C30 C -0.1129(14) -0.1083(12) 0.7248(7) 0.132(9) Uani 1 1 d . . . H30A H -0.0794 -0.1521 0.7308 0.199 Uiso 1 1 calc R . . H30B H -0.1696 -0.1158 0.7358 0.199 Uiso 1 1 calc R . . H30C H -0.0880 -0.0658 0.7395 0.199 Uiso 1 1 calc R . . C31 C -0.3830(13) 0.0532(16) 0.6920(8) 0.132(9) Uani 1 1 d . . . H31 H -0.3808 0.0188 0.7177 0.158 Uiso 1 1 calc R . . C32 C -0.3891(14) 0.1318(13) 0.7138(8) 0.157(11) Uani 1 1 d . . . H32A H -0.3394 0.1408 0.7317 0.235 Uiso 1 1 calc R . . H32B H -0.4387 0.1342 0.7325 0.235 Uiso 1 1 calc R . . H32C H -0.3930 0.1691 0.6906 0.235 Uiso 1 1 calc R . . C33 C -0.4509(13) 0.0236(19) 0.6640(12) 0.236(18) Uani 1 1 d . . . H33A H -0.5044 0.0303 0.6790 0.354 Uiso 1 1 calc R . . H33B H -0.4415 -0.0288 0.6587 0.354 Uiso 1 1 calc R . . H33C H -0.4517 0.0498 0.6357 0.354 Uiso 1 1 calc R . . C34 C -0.1674(11) 0.1333(12) 0.5747(6) 0.080(6) Uani 1 1 d . . . H34 H -0.1076 0.1232 0.5680 0.096 Uiso 1 1 calc R . . C35 C -0.1743(15) 0.2157(12) 0.5862(7) 0.124(9) Uani 1 1 d . . . H35A H -0.1402 0.2263 0.6122 0.187 Uiso 1 1 calc R . . H35B H -0.2324 0.2279 0.5924 0.187 Uiso 1 1 calc R . . H35C H -0.1545 0.2450 0.5612 0.187 Uiso 1 1 calc R . . C36 C -0.2168(14) 0.1137(11) 0.5340(6) 0.118(8) Uani 1 1 d . . . H36A H -0.1995 0.1452 0.5095 0.177 Uiso 1 1 calc R . . H36B H -0.2762 0.1210 0.5398 0.177 Uiso 1 1 calc R . . H36C H -0.2067 0.0622 0.5264 0.177 Uiso 1 1 calc R . . C37 C -0.094(3) 0.3370(16) 0.7474(17) 0.070(7) Uani 0.50 1 d PDU A 1 H37 H -0.0655 0.3824 0.7440 0.084 Uiso 0.50 1 calc PR A 1 C38 C -0.114(3) 0.301(3) 0.7878(12) 0.076(8) Uani 0.50 1 d PDU A 1 H38 H -0.1047 0.3201 0.8164 0.091 Uiso 0.50 1 calc PR A 1 C39 C -0.152(4) 0.230(3) 0.7791(15) 0.075(9) Uani 0.50 1 d PDU A 1 H39 H -0.1697 0.1951 0.8001 0.090 Uiso 0.50 1 calc PR A 1 C40 C -0.156(4) 0.224(2) 0.7320(15) 0.076(8) Uani 0.50 1 d PDU A 1 H40 H -0.1759 0.1823 0.7165 0.091 Uiso 0.50 1 calc PR A 1 C41 C -0.126(4) 0.288(3) 0.7121(10) 0.078(8) Uani 0.50 1 d PDU A 1 H41 H -0.1266 0.2988 0.6814 0.094 Uiso 0.50 1 calc PR A 1 C37' C -0.103(3) 0.3282(19) 0.7670(15) 0.080(9) Uani 0.50 1 d PDU B 2 H37' H -0.0867 0.3740 0.7789 0.096 Uiso 0.50 1 calc PR B 2 C38' C -0.130(3) 0.264(3) 0.7909(10) 0.075(9) Uani 0.50 1 d PDU B 2 H38' H -0.1292 0.2596 0.8221 0.090 Uiso 0.50 1 calc PR B 2 C39' C -0.157(3) 0.209(2) 0.7606(15) 0.072(8) Uani 0.50 1 d PDU B 2 H39' H -0.1788 0.1618 0.7679 0.086 Uiso 0.50 1 calc PR B 2 C40' C -0.145(4) 0.238(3) 0.7171(13) 0.080(9) Uani 0.50 1 d PDU B 2 H40' H -0.1597 0.2134 0.6905 0.096 Uiso 0.50 1 calc PR B 2 C41' C -0.108(4) 0.307(3) 0.7198(12) 0.085(9) Uani 0.50 1 d PDU B 2 H41' H -0.0892 0.3362 0.6957 0.101 Uiso 0.50 1 calc PR B 2 O1 O 0.0000 0.5000 0.5000 0.150 Uiso 1 2 d S . . C42 C -0.0738 0.4632 0.5124 0.160 Uiso 0.50 1 d P C 1 H42A H -0.1068 0.4761 0.4859 0.192 Uiso 0.50 1 calc PR C 1 H42B H -0.0542 0.4128 0.5061 0.192 Uiso 0.50 1 calc PR C 1 C43 C -0.1389 0.4442 0.5386 0.160 Uiso 0.50 1 d P C 1 H43A H -0.1737 0.4082 0.5233 0.240 Uiso 0.50 1 calc PR C 1 H43B H -0.1720 0.4879 0.5453 0.240 Uiso 0.50 1 calc PR C 1 H43C H -0.1179 0.4228 0.5661 0.240 Uiso 0.50 1 calc PR C 1 C42' C -0.0466 0.4513 0.4738 0.160 Uiso 0.50 1 d P C 2 H42C H -0.0549 0.4742 0.4445 0.192 Uiso 0.50 1 calc PR C 2 H42D H -0.0132 0.4063 0.4693 0.192 Uiso 0.50 1 calc PR C 2 C43' C -0.1241 0.4307 0.4901 0.160 Uiso 0.50 1 d P C 2 H43D H -0.1508 0.3970 0.4693 0.240 Uiso 0.50 1 calc PR C 2 H43E H -0.1589 0.4744 0.4938 0.240 Uiso 0.50 1 calc PR C 2 H43F H -0.1171 0.4063 0.5186 0.240 Uiso 0.50 1 calc PR C 2 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 0.0561(5) 0.0427(4) 0.0396(4) 0.000 0.0065(7) 0.000 In1 0.0525(6) 0.0494(5) 0.0435(5) -0.0057(4) 0.0033(8) 0.0008(8) C1 0.046(10) 0.041(6) 0.047(7) 0.013(5) 0.001(7) 0.000(7) C2 0.042(9) 0.066(10) 0.044(8) 0.005(8) 0.001(7) -0.011(8) C3 0.051(9) 0.058(10) 0.046(9) -0.016(8) 0.001(8) -0.011(8) C4 0.059(9) 0.052(9) 0.043(8) -0.024(7) 0.003(7) -0.001(7) C5 0.035(8) 0.076(11) 0.044(8) -0.015(8) 0.009(6) 0.000(8) C6 0.041(8) 0.055(9) 0.048(8) 0.005(7) 0.002(7) 0.005(7) C7 0.057(10) 0.056(10) 0.037(9) -0.012(8) 0.020(8) -0.002(8) C8 0.055(10) 0.072(12) 0.055(10) -0.017(9) 0.014(8) -0.025(10) C9 0.076(13) 0.073(12) 0.067(11) 0.006(9) 0.012(10) -0.020(11) C10 0.058(11) 0.093(14) 0.061(11) -0.009(10) 0.013(9) -0.022(10) C11 0.038(10) 0.090(14) 0.075(11) -0.004(11) 0.001(9) -0.005(10) C12 0.042(10) 0.089(14) 0.066(11) 0.000(10) 0.002(9) 0.005(11) C13 0.037(9) 0.074(12) 0.085(12) 0.013(10) -0.005(9) -0.010(8) C14 0.072(13) 0.101(15) 0.151(19) -0.017(14) 0.020(13) 0.028(12) C15 0.14(2) 0.100(17) 0.108(17) 0.028(14) -0.002(15) 0.020(15) C16 0.12(2) 0.16(2) 0.099(18) -0.020(17) 0.003(16) -0.073(19) C17 0.22(3) 0.37(5) 0.13(2) -0.01(3) 0.02(2) -0.23(4) C18 0.13(2) 0.18(3) 0.21(3) -0.06(2) -0.04(2) -0.086(19) C19 0.061(11) 0.060(10) 0.089(12) 0.036(9) -0.031(10) -0.029(8) C20 0.128(19) 0.091(17) 0.16(2) 0.008(15) -0.058(17) 0.025(14) C21 0.16(2) 0.118(18) 0.090(15) 0.002(13) -0.052(15) -0.028(16) C22 0.036(8) 0.075(10) 0.036(7) -0.008(7) -0.003(6) -0.012(8) C23 0.055(12) 0.076(13) 0.056(11) 0.007(10) -0.004(9) 0.002(10) C24 0.060(13) 0.088(16) 0.088(13) 0.006(12) -0.018(11) 0.006(11) C25 0.046(10) 0.103(15) 0.068(11) 0.009(10) 0.017(9) 0.003(10) C26 0.063(12) 0.099(16) 0.085(14) 0.013(12) 0.004(11) -0.009(11) C27 0.043(9) 0.078(11) 0.048(8) -0.006(8) 0.006(7) -0.010(8) C28 0.044(10) 0.079(12) 0.113(15) 0.016(11) 0.017(10) 0.002(9) C29 0.14(2) 0.068(14) 0.16(2) 0.007(14) 0.032(17) 0.009(14) C30 0.122(19) 0.16(2) 0.111(16) 0.060(16) 0.004(15) 0.034(17) C31 0.068(14) 0.19(3) 0.14(2) -0.005(19) 0.034(15) 0.013(17) C32 0.12(2) 0.14(2) 0.21(3) 0.03(2) 0.11(2) 0.046(17) C33 0.040(13) 0.34(5) 0.33(4) 0.05(4) 0.03(2) -0.01(2) C34 0.059(11) 0.119(17) 0.063(12) 0.020(12) -0.009(9) 0.023(12) C35 0.17(3) 0.095(19) 0.111(17) 0.011(15) 0.017(17) -0.015(17) C36 0.16(2) 0.121(18) 0.069(13) 0.013(12) 0.011(14) 0.025(16) C37 0.096(17) 0.053(12) 0.061(18) 0.006(15) 0.020(19) 0.049(11) C38 0.091(19) 0.069(19) 0.068(12) 0.006(15) 0.030(17) 0.035(17) C39 0.070(18) 0.086(18) 0.070(16) 0.009(17) 0.021(18) 0.020(16) C40 0.066(17) 0.094(16) 0.068(17) 0.020(16) 0.01(2) 0.009(14) C41 0.08(2) 0.084(19) 0.069(11) 0.020(14) 0.000(16) 0.017(17) C37' 0.101(18) 0.070(16) 0.070(19) 0.008(15) 0.04(2) 0.036(15) C38' 0.072(19) 0.08(2) 0.070(12) 0.009(14) 0.031(15) 0.023(18) C39' 0.052(14) 0.090(16) 0.07(2) 0.020(14) 0.009(19) 0.018(14) C40' 0.080(19) 0.087(18) 0.073(14) 0.018(15) 0.011(18) 0.015(16) C41' 0.10(2) 0.080(18) 0.070(15) 0.015(15) 0.014(18) 0.018(16) _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 C41' 2.37(6) 3_556 ? Hf1 C37 2.42(4) 3_556 ? Hf1 C40' 2.49(6) 3_556 ? Hf1 C38' 2.46(5) 3_556 ? Hf1 C38 2.47(4) 3_556 ? Hf1 C39' 2.52(5) 3_556 ? Hf1 C37' 2.45(5) 3_556 ? Hf1 C40 2.51(5) 3_556 ? Hf1 C39 2.54(5) 3_556 ? Hf1 C41 2.51(6) 3_556 ? Hf1 In1 2.7665(10) . ? Hf1 In1 2.7665(10) 3_556 ? In1 C1 2.192(13) . ? C1 C2 1.403(17) . ? C1 C6 1.428(17) . ? C2 C3 1.348(18) . ? C2 C22 1.549(17) . ? C3 C4 1.394(17) . ? C4 C5 1.367(17) . ? C5 C6 1.382(17) . ? C6 C7 1.515(19) . ? C7 C8 1.40(2) . ? C7 C12 1.41(2) . ? C8 C9 1.41(2) . ? C8 C19 1.51(2) . ? C9 C10 1.35(2) . ? C10 C11 1.34(2) . ? C10 C16 1.56(3) . ? C11 C12 1.40(2) . ? C12 C13 1.50(2) . ? C13 C14 1.50(2) . ? C13 C15 1.51(2) . ? C16 C17 1.34(3) . ? C16 C18 1.33(3) . ? C19 C20 1.51(2) . ? C19 C21 1.53(2) . ? C22 C27 1.355(18) . ? C22 C23 1.414(19) . ? C23 C24 1.38(2) . ? C23 C34 1.52(2) . ? C24 C25 1.40(2) . ? C25 C26 1.33(2) . ? C25 C31 1.52(2) . ? C26 C27 1.39(2) . ? C27 C28 1.52(2) . ? C28 C30 1.54(2) . ? C28 C29 1.57(2) . ? C31 C33 1.46(3) . ? C31 C32 1.55(3) . ? C34 C36 1.48(2) . ? C34 C35 1.51(2) . ? C37 C38 1.40(3) . ? C37 C41 1.46(3) . ? C38 C39 1.41(3) . ? C39 C40 1.40(3) . ? C40 C41 1.37(3) . ? C37' C38' 1.40(3) . ? C37' C41' 1.45(3) . ? C38' C39' 1.41(3) . ? C39' C40' 1.40(3) . ? C40' C41' 1.38(3) . ? O1 C42' 1.3786(2) 5_566 ? O1 C42' 1.3786(2) . ? O1 C42 1.3850(3) 5_566 ? O1 C42 1.3850(3) . ? C42 C43 1.3312(2) . ? C42' C43' 1.3636(3) . ? 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 C41' Hf1 C37 24.1(13) 3_556 3_556 ? C41' Hf1 C40' 32.9(9) 3_556 3_556 ? C37 Hf1 C40' 51.9(14) 3_556 3_556 ? C41' Hf1 C38' 56.2(12) 3_556 3_556 ? C37 Hf1 C38' 46.3(12) 3_556 3_556 ? C40' Hf1 C38' 54.3(13) 3_556 3_556 ? C41' Hf1 C38 49.4(12) 3_556 3_556 ? C37 Hf1 C38 33.3(8) 3_556 3_556 ? C40' Hf1 C38 58.7(15) 3_556 3_556 ? C38' Hf1 C38 16.2(10) 3_556 3_556 ? C41' Hf1 C39' 55.3(12) 3_556 3_556 ? C37 Hf1 C39' 61.6(13) 3_556 3_556 ? C40' Hf1 C39' 32.5(9) 3_556 3_556 ? C38' Hf1 C39' 32.9(9) 3_556 3_556 ? C38 Hf1 C39' 46.0(13) 3_556 3_556 ? C41' Hf1 C37' 35.0(9) 3_556 3_556 ? C37 Hf1 C37' 14.7(10) 3_556 3_556 ? C40' Hf1 C37' 55.3(12) 3_556 3_556 ? C38' Hf1 C37' 33.3(9) 3_556 3_556 ? C38 Hf1 C37' 18.9(10) 3_556 3_556 ? C39' Hf1 C37' 55.2(11) 3_556 3_556 ? C41' Hf1 C40 40.8(15) 3_556 3_556 ? C37 Hf1 C40 55.3(11) 3_556 3_556 ? C40' Hf1 C40 12.2(10) 3_556 3_556 ? C38' Hf1 C40 45.9(13) 3_556 3_556 ? C38 Hf1 C40 53.6(12) 3_556 3_556 ? C39' Hf1 C40 20.4(10) 3_556 3_556 ? C37' Hf1 C40 54.8(15) 3_556 3_556 ? C41' Hf1 C39 56.8(15) 3_556 3_556 ? C37 Hf1 C39 55.6(11) 3_556 3_556 ? C40' Hf1 C39 43.1(13) 3_556 3_556 ? C38' Hf1 C39 18.0(11) 3_556 3_556 ? C38 Hf1 C39 32.7(9) 3_556 3_556 ? C39' Hf1 C39 15.3(10) 3_556 3_556 ? C37' Hf1 C39 45.7(13) 3_556 3_556 ? C40 Hf1 C39 32.3(9) 3_556 3_556 ? C41' Hf1 C41 11.3(13) 3_556 3_556 ? C37 Hf1 C41 34.3(9) 3_556 3_556 ? C40' Hf1 C41 22.2(13) 3_556 3_556 ? C38' Hf1 C41 57.3(13) 3_556 3_556 ? C38 Hf1 C41 54.2(11) 3_556 3_556 ? C39' Hf1 C41 48.9(12) 3_556 3_556 ? C37' Hf1 C41 42.9(16) 3_556 3_556 ? C40 Hf1 C41 31.7(9) 3_556 3_556 ? C39 Hf1 C41 53.7(12) 3_556 3_556 ? C41' Hf1 In1 131.6(10) 3_556 . ? C37 Hf1 In1 123.3(11) 3_556 . ? C40' Hf1 In1 108.4(11) 3_556 . ? C38' Hf1 In1 78.0(10) 3_556 . ? C38 Hf1 In1 89.9(12) 3_556 . ? C39' Hf1 In1 78.1(9) 3_556 . ? C37' Hf1 In1 108.8(10) 3_556 . ? C40 Hf1 In1 96.7(10) 3_556 . ? C39 Hf1 In1 74.8(10) 3_556 . ? C41 Hf1 In1 126.9(9) 3_556 . ? C41' Hf1 In1 97.2(12) 3_556 3_556 ? C37 Hf1 In1 121.2(11) 3_556 3_556 ? C40' Hf1 In1 76.1(10) 3_556 3_556 ? C38' Hf1 In1 123.1(11) 3_556 3_556 ? C38 Hf1 In1 133.7(10) 3_556 3_556 ? C39' Hf1 In1 90.3(10) 3_556 3_556 ? C37' Hf1 In1 130.2(10) 3_556 3_556 ? C40 Hf1 In1 80.1(10) 3_556 3_556 ? C39 Hf1 In1 105.4(12) 3_556 3_556 ? C41 Hf1 In1 87.7(11) 3_556 3_556 ? In1 Hf1 In1 95.27(4) . 3_556 ? C1 In1 Hf1 171.2(3) . . ? C2 C1 C6 117.0(12) . . ? C2 C1 In1 121.2(10) . . ? C6 C1 In1 121.8(10) . . ? C3 C2 C1 121.7(13) . . ? C3 C2 C22 121.0(13) . . ? C1 C2 C22 117.1(12) . . ? C2 C3 C4 119.7(13) . . ? C5 C4 C3 121.7(12) . . ? C4 C5 C6 118.7(13) . . ? C5 C6 C1 121.1(13) . . ? C5 C6 C7 118.6(12) . . ? C1 C6 C7 120.3(12) . . ? C8 C7 C12 121.2(16) . . ? C8 C7 C6 118.1(14) . . ? C12 C7 C6 120.7(15) . . ? C7 C8 C9 117.3(16) . . ? C7 C8 C19 123.0(14) . . ? C9 C8 C19 119.6(16) . . ? C10 C9 C8 121.8(16) . . ? C11 C10 C9 120.0(16) . . ? C11 C10 C16 122(2) . . ? C9 C10 C16 118(2) . . ? C10 C11 C12 122.8(17) . . ? C11 C12 C7 116.9(17) . . ? C11 C12 C13 121.2(16) . . ? C7 C12 C13 121.8(16) . . ? C14 C13 C12 113.0(15) . . ? C14 C13 C15 108.0(15) . . ? C12 C13 C15 113.2(15) . . ? C17 C16 C18 130(2) . . ? C17 C16 C10 114(2) . . ? C18 C16 C10 116(2) . . ? C8 C19 C20 113.9(15) . . ? C8 C19 C21 108.4(15) . . ? C20 C19 C21 111.8(15) . . ? C27 C22 C23 122.2(14) . . ? C27 C22 C2 119.4(14) . . ? C23 C22 C2 118.4(13) . . ? C24 C23 C22 116.5(16) . . ? C24 C23 C34 121.0(16) . . ? C22 C23 C34 122.3(16) . . ? C23 C24 C25 122.2(17) . . ? C26 C25 C24 117.5(16) . . ? C26 C25 C31 120.9(18) . . ? C24 C25 C31 121.5(19) . . ? C25 C26 C27 124.0(18) . . ? C22 C27 C26 117.5(16) . . ? C22 C27 C28 122.6(14) . . ? C26 C27 C28 119.8(15) . . ? C27 C28 C30 114.2(15) . . ? C27 C28 C29 109.7(14) . . ? C30 C28 C29 108.2(16) . . ? C33 C31 C25 111(2) . . ? C33 C31 C32 122(2) . . ? C25 C31 C32 110(2) . . ? C36 C34 C23 111.1(16) . . ? C36 C34 C35 112.2(17) . . ? C23 C34 C35 111.8(16) . . ? C38 C37 C41 105(2) . . ? C39 C38 C37 111(3) . . ? C38 C39 C40 106(3) . . ? C39 C40 C41 110(3) . . ? C40 C41 C37 108(2) . . ? C38' C37' C41' 105(2) . . ? C39' C38' C37' 110(3) . . ? C40' C39' C38' 107(3) . . ? C39' C40' C41' 110(3) . . ? C40' C41' C37' 108(3) . . ? C42' O1 C42' 180.0 5_566 . ? C42' O1 C42 53.432(12) 5_566 5_566 ? C42' O1 C42 126.568(12) . 5_566 ? C42' O1 C42 126.568(12) 5_566 . ? C42' O1 C42 53.432(12) . . ? C42 O1 C42 180.0 5_566 . ? C43 C42 O1 157.326(5) . . ? C43' C42' O1 116.493(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.771 _refine_diff_density_min -2.770 _refine_diff_density_rms 0.121