#------------------------------------------------------------------------------ #$Date: 2018-01-12 04:17:34 +0200 (Fri, 12 Jan 2018) $ #$Revision: 205102 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/86/1548660.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1548660 loop_ _publ_author_name 'De, Anangsha' 'Zhang, Qian-Fan' 'Mondal, Bijan' 'Cheung, Ling Fung' 'Kar, Sourav' 'Saha, Koushik' 'Varghese, Babu' 'Wang, Lai-Sheng' 'Ghosh, Sundargopal' _publ_section_title ; [(Cp2M)2B9H11] (M = Zr or Hf): early transition metal ‘guarded’ heptaborane with strong covalent and electrostatic bonding ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C7SC05014C _journal_year 2018 _chemical_formula_moiety 'C20 H27 B9 Hf2, C7 H8' _chemical_formula_sum 'C27 H35 B9 Hf2' _chemical_formula_weight 813.82 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2017-08-10 deposited with the CCDC. 2018-01-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 110.082(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.2181(8) _cell_length_b 12.9003(7) _cell_length_c 14.6113(9) _cell_measurement_reflns_used 9034 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 72.60 _cell_measurement_theta_min 4.33 _cell_volume 3048.1(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker apex3 C-MOS Diffractometer' _diffrn_measurement_method '\w and \f scan' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_unetI/netI 0.1126 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 50752 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 64.983 _diffrn_reflns_theta_max 64.983 _diffrn_reflns_theta_min 2.732 _diffrn_source 'micro focus Cu' _exptl_absorpt_coefficient_mu 12.444 _exptl_absorpt_correction_T_max 0.7536 _exptl_absorpt_correction_T_min 0.3970 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.773 _exptl_crystal_description needle _exptl_crystal_F_000 1544 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _refine_diff_density_max 2.619 _refine_diff_density_min -2.412 _refine_diff_density_rms 0.276 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 360 _refine_ls_number_reflns 50752 _refine_ls_number_restraints 349 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0783 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1130P)^2^+16.5730P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2117 _refine_ls_wR_factor_ref 0.2342 _reflns_Friedel_coverage 0.000 _reflns_number_gt 38138 _reflns_number_total 50752 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7sc05014c2.cif _cod_data_source_block NEW _cod_database_code 1548660 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.369 _shelx_estimated_absorpt_t_max 0.575 _shelx_res_file ; TITL HF2CU_a.res in P2(1)/c NEW.res created by SHELXL-2016/6 at 14:42:02 on 20-Jan-2017 CELL 1.54178 17.2181 12.9003 14.6113 90.000 110.082 90.000 ZERR 4.00 0.0008 0.0007 0.0009 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H B HF UNIT 108 140 36 8 MERG 0 OMIT -3.00 130.00 OMIT 5 0 4 OMIT -2 -4 -3 OMIT 2 -4 3 OMIT -2 -2 -6 OMIT -2 -4 -3 DFIX 1.52 0.01 C21 C22 DFIX 1.40 0.01 C22 C23 C23 C24 C24 C25 C25 C26 C26 C27 C27 C22 SADI 0.02 C22 C24 C23 C25 C24 C26 C25 C27 C26 C22 C27 C23 SIMU 0.02 0.04 C22 > C27 SIMU 0.01 0.02 2.6 B1 > B9 DFIX 1.15 0.03 B8 H8A B8 H8B B9 H9A B9 H9B DFIX 1.91 0.02 H8A H8B H9A H9B SIMU 0.01 0.02 C1 > C5 SIMU 0.01 0.02 C6 > C10 SIMU 0.01 0.02 C11 > C15 SIMU 0.01 0.02 C16 > C20 ISOR 0.005 C1 > C5 EADP H9A H9B RIGU 0.001 0.001 B2 B1 RIGU 0.001 0.002 B8 B1 RIGU 0.001 0.002 B3 B1 RIGU 0.001 0.002 B8 B1 RIGU 0.001 0.002 B5 B7 RIGU 0.001 0.0012 B6 B7 FMAP 2 PLAN 20 SIZE 0.05 0.10 0.10 ACTA BOND $H CONF L.S. 11 WGHT 0.113000 16.573000 BASF 0.32188 FVAR 0.20983 C1 1 0.539421 0.669277 0.126804 11.00000 0.10794 0.12507 = 0.06958 0.01072 0.06124 -0.03234 AFIX 43 H1 2 0.581124 0.718866 0.145712 11.00000 -1.20000 AFIX 0 C2 1 0.459457 0.682935 0.090185 11.00000 0.12402 0.11064 = 0.07413 0.02114 0.03789 0.00855 AFIX 43 H2 2 0.434809 0.748065 0.079509 11.00000 -1.20000 AFIX 0 C3 1 0.420804 0.603671 0.071623 11.00000 0.08899 0.11598 = 0.06162 -0.00047 0.02976 0.00122 AFIX 43 H3 2 0.363372 0.604032 0.045107 11.00000 -1.20000 AFIX 0 C4 1 0.458842 0.524025 0.088469 11.00000 0.11400 0.09681 = 0.05682 -0.01212 0.04739 -0.00508 AFIX 43 H4 2 0.437429 0.457175 0.077351 11.00000 -1.20000 AFIX 0 C5 1 0.546913 0.554007 0.130613 11.00000 0.10523 0.13897 = 0.06592 -0.01054 0.06100 0.04263 AFIX 43 H5 2 0.593864 0.512574 0.153189 11.00000 -1.20000 AFIX 0 C6 1 0.614091 0.683541 0.360912 11.00000 0.04726 0.07917 = 0.04950 -0.00582 -0.00343 -0.03205 AFIX 43 H6 2 0.638402 0.736084 0.336468 11.00000 -1.20000 AFIX 0 C7 1 0.559531 0.697229 0.404734 11.00000 0.07571 0.07673 = 0.04908 -0.02715 0.00242 -0.00105 AFIX 43 H7 2 0.539903 0.761291 0.416293 11.00000 -1.20000 AFIX 0 C8 1 0.536025 0.604277 0.430643 11.00000 0.05126 0.09870 = 0.04143 0.00823 0.01612 -0.00253 AFIX 43 H8 2 0.497389 0.594230 0.461313 11.00000 -1.20000 AFIX 0 C9 1 0.580594 0.525608 0.402800 11.00000 0.04666 0.08524 = 0.05439 0.03174 -0.00756 -0.00973 AFIX 43 H9 2 0.578424 0.454541 0.412338 11.00000 -1.20000 AFIX 0 C10 1 0.629424 0.579171 0.357025 11.00000 0.02227 0.10361 = 0.04546 0.00235 -0.00262 0.00599 AFIX 43 H10 2 0.665281 0.549161 0.329411 11.00000 -1.20000 AFIX 0 C11 1 0.054112 0.622116 0.088560 11.00000 0.07593 0.13706 = 0.07083 0.02078 -0.00751 -0.02636 AFIX 43 H11 2 0.072426 0.679235 0.062845 11.00000 -1.20000 AFIX 0 C12 1 0.088554 0.522632 0.102033 11.00000 0.05488 0.13773 = 0.05227 -0.03228 0.01211 -0.01847 AFIX 43 H12 2 0.133109 0.502178 0.084097 11.00000 -1.20000 AFIX 0 C13 1 0.046795 0.458925 0.145917 11.00000 0.05959 0.09865 = 0.06347 -0.03140 0.00273 -0.01684 AFIX 43 H13 2 0.058866 0.390002 0.163829 11.00000 -1.20000 AFIX 0 C14 1 -0.016003 0.517246 0.157918 11.00000 0.02486 0.09943 = 0.07202 -0.01140 -0.00353 -0.02347 AFIX 43 H14 2 -0.054042 0.493795 0.185540 11.00000 -1.20000 AFIX 0 C15 1 -0.013581 0.618901 0.121478 11.00000 0.03987 0.12589 = 0.09356 0.00745 -0.02803 0.00166 AFIX 43 H15 2 -0.049824 0.672925 0.119742 11.00000 -1.20000 AFIX 0 C16 1 0.115970 0.456011 0.387823 11.00000 0.08477 0.10234 = 0.05921 0.01162 0.02873 -0.00820 AFIX 43 H16 2 0.111027 0.387883 0.365742 11.00000 -1.20000 AFIX 0 C17 1 0.051585 0.524724 0.385664 11.00000 0.06713 0.13272 = 0.07466 0.00761 0.04728 -0.00530 AFIX 43 H17 2 -0.004475 0.508648 0.363460 11.00000 -1.20000 AFIX 0 C18 1 0.086081 0.621889 0.422696 11.00000 0.08934 0.13421 = 0.07171 -0.02781 0.03895 0.02278 AFIX 43 H18 2 0.057532 0.681780 0.427172 11.00000 -1.20000 AFIX 0 C19 1 0.171045 0.609904 0.450996 11.00000 0.08572 0.12563 = 0.06092 -0.02940 0.02368 -0.01574 AFIX 43 H19 2 0.210197 0.660632 0.479784 11.00000 -1.20000 AFIX 0 C20 1 0.187613 0.511606 0.429651 11.00000 0.06700 0.11761 = 0.04674 0.01241 0.02630 0.00603 AFIX 43 H20 2 0.240511 0.485357 0.441755 11.00000 -1.20000 AFIX 0 C21 1 -0.160547 0.681314 0.380301 11.00000 0.05983 0.34933 = 0.06706 0.05043 0.01845 -0.04630 AFIX 137 H21A 2 -0.135581 0.615820 0.404883 11.00000 -1.50000 H21B 2 -0.204833 0.694905 0.404459 11.00000 -1.50000 H21C 2 -0.119842 0.735218 0.401479 11.00000 -1.50000 AFIX 0 C22 1 -0.192883 0.678286 0.274585 11.00000 0.03224 0.14738 = 0.15892 0.07412 0.03130 -0.01767 C23 1 -0.226035 0.757461 0.213201 11.00000 0.04847 0.09095 = 0.15663 0.05288 0.02624 -0.00294 AFIX 43 H23 2 -0.228784 0.823157 0.238120 11.00000 -1.20000 AFIX 0 C24 1 -0.256425 0.741380 0.111927 11.00000 0.08043 0.10881 = 0.14817 0.03639 0.02266 -0.00809 AFIX 43 H24 2 -0.279019 0.795847 0.069418 11.00000 -1.20000 AFIX 0 C25 1 -0.251971 0.642057 0.076584 11.00000 0.07283 0.14374 = 0.16237 0.00936 0.06075 -0.02211 AFIX 43 H25 2 -0.268758 0.629881 0.009871 11.00000 -1.20000 AFIX 0 C26 1 -0.222524 0.562596 0.141462 11.00000 0.06134 0.11419 = 0.18502 0.02209 0.05830 0.01827 AFIX 43 H26 2 -0.221557 0.495536 0.118515 11.00000 -1.20000 AFIX 0 C27 1 -0.193806 0.581326 0.242169 11.00000 0.04817 0.03671 = 0.08617 0.02040 0.01941 0.02014 AFIX 43 H27 2 -0.175591 0.526762 0.285926 11.00000 -1.20000 AFIX 0 B1 3 0.348521 0.595735 0.260465 11.00000 0.03889 0.01314 = 0.02984 -0.01091 0.02426 -0.01427 B2 3 0.372556 0.717408 0.253584 11.00000 0.03982 0.02291 = 0.07389 0.00505 0.01815 -0.00596 B3 3 0.270181 0.685141 0.176372 11.00000 0.03908 0.04134 = 0.07242 0.00648 0.01515 -0.00220 AFIX 153 H3A 2 0.244179 0.685244 0.096284 11.00000 -1.20000 AFIX 0 B4 3 0.295070 0.790625 0.256269 11.00000 0.04429 0.03469 = 0.09261 -0.00007 0.02314 0.00232 AFIX 153 H4A 2 0.293484 0.875858 0.254344 11.00000 -1.20000 AFIX 0 B5 3 0.219060 0.716291 0.262301 11.00000 0.02991 0.02948 = 0.08576 -0.00702 0.02339 0.00150 B6 3 0.325630 0.687433 0.342602 11.00000 0.03409 0.03289 = 0.06344 -0.01793 0.01231 -0.00673 AFIX 153 H6A 2 0.352147 0.690123 0.422619 11.00000 -1.20000 AFIX 0 B7 3 0.251680 0.601250 0.259590 11.00000 0.04011 0.01194 = 0.02939 -0.00764 0.02786 -0.01450 B8 3 0.383943 0.469445 0.261027 11.00000 0.03144 0.02630 = 0.05266 -0.00313 0.01910 -0.00386 B9 3 0.135152 0.786176 0.272935 11.00000 0.03308 0.05455 = 0.14862 -0.00892 0.02826 0.01913 HF1 4 0.486417 0.604147 0.250905 11.00000 0.02703 0.03460 = 0.03159 0.00398 0.01351 -0.00044 HF2 4 0.113580 0.594830 0.268675 11.00000 0.02515 0.04530 = 0.05828 -0.00880 0.01403 -0.00331 H8A 2 0.345716 0.423371 0.194197 11.00000 0.05111 H8B 2 0.394573 0.428657 0.333334 11.00000 0.06237 H9A 2 0.103776 0.828590 0.204485 11.00000 0.03789 H9B 2 0.150225 0.831253 0.344201 11.00000 0.03789 HKLF 5 REM HF2CU_a.res in P2(1)/c REM R1 = 0.0783 for 38138 Fo > 4sig(Fo) and 0.1043 for all 50752 data REM 360 parameters refined using 349 restraints END WGHT 0.1129 16.5251 REM Highest difference peak 2.619, deepest hole -2.412, 1-sigma level 0.276 Q1 1 0.6847 0.6030 0.2708 11.00000 0.05 2.62 Q2 1 0.3019 0.6010 0.2626 11.00000 0.05 2.18 Q3 1 -0.2786 0.5986 0.2465 11.00000 0.05 2.05 Q4 1 0.1534 0.6129 0.2590 11.00000 0.05 1.95 Q5 1 0.5621 0.6078 0.1337 11.00000 0.05 1.83 Q6 1 0.0727 0.6062 0.2726 11.00000 0.05 1.79 Q7 1 -0.0833 0.5987 0.2735 11.00000 0.05 1.56 Q8 1 -0.1372 0.5878 0.2730 11.00000 0.05 1.42 Q9 1 0.5203 0.5984 0.2570 11.00000 0.05 1.38 Q10 1 -0.1662 0.5910 0.3357 11.00000 0.05 1.24 Q11 1 0.5101 0.4984 0.1164 11.00000 0.05 1.11 Q12 1 0.4701 0.6994 0.2554 11.00000 0.05 0.94 Q13 1 -0.0095 0.6997 0.2397 11.00000 0.05 0.90 Q14 1 -0.2340 0.6416 0.1682 11.00000 0.05 0.82 Q15 1 0.6079 0.6972 0.2566 11.00000 0.05 0.74 Q16 1 -0.1131 0.4862 0.2284 11.00000 0.05 0.74 Q17 1 -0.1911 0.7749 0.3369 11.00000 0.05 0.73 Q18 1 -0.2306 0.5012 0.2561 11.00000 0.05 0.73 Q19 1 0.2410 0.4819 0.2381 11.00000 0.05 0.73 Q20 1 -0.2018 0.7100 0.2446 11.00000 0.05 0.73 ; _shelx_res_checksum 53661 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp C1 C 0.539(2) 0.669(3) 0.127(2) 0.093(7) Uani 1 1 d . U H1 H 0.581124 0.718866 0.145712 0.111 Uiso 1 1 calc R U C2 C 0.459(2) 0.683(3) 0.090(2) 0.102(8) Uani 1 1 d . U H2 H 0.434809 0.748065 0.079509 0.122 Uiso 1 1 calc R U C3 C 0.421(2) 0.604(3) 0.072(2) 0.088(7) Uani 1 1 d . U H3 H 0.363372 0.604032 0.045107 0.105 Uiso 1 1 calc R U C4 C 0.459(2) 0.524(3) 0.0885(19) 0.085(7) Uani 1 1 d . U H4 H 0.437429 0.457175 0.077351 0.101 Uiso 1 1 calc R U C5 C 0.547(2) 0.554(3) 0.131(2) 0.095(7) Uani 1 1 d . U H5 H 0.593864 0.512574 0.153189 0.114 Uiso 1 1 calc R U C6 C 0.6141(13) 0.684(2) 0.3609(16) 0.064(6) Uani 1 1 d . U H6 H 0.638402 0.736084 0.336468 0.077 Uiso 1 1 calc R U C7 C 0.5595(16) 0.697(2) 0.4047(17) 0.072(6) Uani 1 1 d . U H7 H 0.539903 0.761291 0.416293 0.087 Uiso 1 1 calc R U C8 C 0.5360(14) 0.604(2) 0.4306(15) 0.064(6) Uani 1 1 d . U H8 H 0.497389 0.594230 0.461313 0.076 Uiso 1 1 calc R U C9 C 0.5806(13) 0.526(2) 0.4028(17) 0.069(6) Uani 1 1 d . U H9 H 0.578424 0.454541 0.412338 0.082 Uiso 1 1 calc R U C10 C 0.6294(11) 0.579(2) 0.3570(15) 0.061(5) Uani 1 1 d . U H10 H 0.665281 0.549161 0.329411 0.073 Uiso 1 1 calc R U C11 C 0.054(2) 0.622(3) 0.089(2) 0.103(9) Uani 1 1 d . U H11 H 0.072426 0.679235 0.062845 0.124 Uiso 1 1 calc R U C12 C 0.0886(16) 0.523(3) 0.1020(18) 0.083(7) Uani 1 1 d . U H12 H 0.133109 0.502178 0.084097 0.100 Uiso 1 1 calc R U C13 C 0.0468(16) 0.459(2) 0.1459(19) 0.079(7) Uani 1 1 d . U H13 H 0.058866 0.390002 0.163829 0.094 Uiso 1 1 calc R U C14 C -0.0160(12) 0.517(2) 0.1579(19) 0.071(6) Uani 1 1 d . U H14 H -0.054042 0.493795 0.185540 0.085 Uiso 1 1 calc R U C15 C -0.0136(16) 0.619(3) 0.121(2) 0.100(9) Uani 1 1 d . U H15 H -0.049824 0.672925 0.119742 0.120 Uiso 1 1 calc R U C16 C 0.1160(18) 0.456(2) 0.388(2) 0.081(7) Uani 1 1 d . U H16 H 0.111027 0.387883 0.365742 0.097 Uiso 1 1 calc R U C17 C 0.0516(17) 0.525(3) 0.386(2) 0.086(7) Uani 1 1 d . U H17 H -0.004475 0.508648 0.363460 0.103 Uiso 1 1 calc R U C18 C 0.086(2) 0.622(3) 0.423(2) 0.095(8) Uani 1 1 d . U H18 H 0.057532 0.681780 0.427172 0.115 Uiso 1 1 calc R U C19 C 0.171(2) 0.610(3) 0.451(2) 0.091(7) Uani 1 1 d . U H19 H 0.210197 0.660632 0.479784 0.109 Uiso 1 1 calc R U C20 C 0.1876(16) 0.512(3) 0.4297(17) 0.075(6) Uani 1 1 d . U H20 H 0.240511 0.485357 0.441755 0.090 Uiso 1 1 calc R U C21 C -0.1605(19) 0.681(4) 0.3803(19) 0.16(2) Uani 1 1 d D . H21A H -0.135581 0.615820 0.404883 0.239 Uiso 1 1 calc R U H21B H -0.204833 0.694905 0.404459 0.239 Uiso 1 1 calc R U H21C H -0.119842 0.735218 0.401479 0.239 Uiso 1 1 calc R U C22 C -0.1929(12) 0.678(2) 0.2746(18) 0.113(12) Uani 1 1 d D U C23 C -0.2260(15) 0.7575(19) 0.213(2) 0.101(10) Uani 1 1 d D U H23 H -0.228784 0.823157 0.238120 0.121 Uiso 1 1 calc R U C24 C -0.256(2) 0.741(2) 0.112(2) 0.117(12) Uani 1 1 d D U H24 H -0.279019 0.795847 0.069418 0.140 Uiso 1 1 calc R U C25 C -0.2520(19) 0.642(3) 0.077(2) 0.121(12) Uani 1 1 d D U H25 H -0.268758 0.629881 0.009871 0.145 Uiso 1 1 calc R U C26 C -0.2225(18) 0.563(2) 0.141(2) 0.116(11) Uani 1 1 d D U H26 H -0.221557 0.495536 0.118515 0.139 Uiso 1 1 calc R U C27 C -0.1938(13) 0.5813(15) 0.2422(18) 0.058(6) Uani 1 1 d D U H27 H -0.175591 0.526762 0.285926 0.070 Uiso 1 1 calc R U B1 B 0.3485(10) 0.5957(12) 0.2605(12) 0.024(3) Uani 1 1 d . U B2 B 0.3726(12) 0.7174(15) 0.254(2) 0.046(4) Uani 1 1 d . U B3 B 0.2702(13) 0.6851(18) 0.176(2) 0.052(5) Uani 1 1 d . U H3A H 0.244179 0.685244 0.096284 0.062 Uiso 1 1 calc R U B4 B 0.2951(13) 0.7906(19) 0.256(2) 0.057(5) Uani 1 1 d . U H4A H 0.293484 0.875858 0.254344 0.069 Uiso 1 1 calc R U B5 B 0.2191(12) 0.7163(16) 0.262(2) 0.047(4) Uani 1 1 d . U B6 B 0.3256(12) 0.6874(16) 0.3426(18) 0.045(4) Uani 1 1 d . U H6A H 0.352147 0.690123 0.422619 0.054 Uiso 1 1 calc R U B7 B 0.2517(11) 0.6012(12) 0.2596(12) 0.023(3) Uani 1 1 d . U B8 B 0.3839(11) 0.4694(14) 0.2610(16) 0.036(4) Uani 1 1 d D U B9 B 0.1352(14) 0.786(2) 0.273(3) 0.080(8) Uani 1 1 d D U Hf1 Hf 0.48642(4) 0.60415(6) 0.25090(6) 0.0302(3) Uani 1 1 d . . Hf2 Hf 0.11358(5) 0.59483(7) 0.26868(7) 0.0430(3) Uani 1 1 d . . H8A H 0.346(11) 0.423(12) 0.194(8) 0.05(6) Uiso 1 1 d D . H8B H 0.395(13) 0.429(13) 0.333(7) 0.06(6) Uiso 1 1 d D . H9A H 0.104(10) 0.829(12) 0.204(7) 0.04(3) Uiso 1 1 d D . H9B H 0.150(10) 0.831(12) 0.344(7) 0.04(3) Uiso 1 1 d 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 C1 0.108(12) 0.125(13) 0.070(11) 0.011(10) 0.061(10) -0.032(11) C2 0.124(13) 0.111(13) 0.074(12) 0.021(11) 0.038(11) 0.009(11) C3 0.089(12) 0.116(13) 0.062(10) 0.000(11) 0.030(10) 0.001(11) C4 0.114(12) 0.097(13) 0.057(10) -0.012(10) 0.047(10) -0.005(11) C5 0.105(12) 0.139(13) 0.066(10) -0.011(10) 0.061(10) 0.043(10) C6 0.047(10) 0.079(13) 0.049(11) -0.006(11) -0.003(9) -0.032(10) C7 0.076(13) 0.077(14) 0.049(11) -0.027(11) 0.002(10) -0.001(12) C8 0.051(10) 0.099(16) 0.041(10) 0.008(11) 0.016(9) -0.003(11) C9 0.047(10) 0.085(15) 0.054(11) 0.032(11) -0.008(9) -0.010(10) C10 0.022(7) 0.104(15) 0.045(10) 0.002(11) -0.003(8) 0.006(9) C11 0.076(15) 0.14(2) 0.071(14) 0.021(16) -0.008(13) -0.026(15) C12 0.055(12) 0.14(2) 0.052(12) -0.032(14) 0.012(10) -0.018(13) C13 0.060(12) 0.099(17) 0.063(13) -0.031(13) 0.003(11) -0.017(12) C14 0.025(8) 0.099(16) 0.072(13) -0.011(12) -0.004(9) -0.023(10) C15 0.040(10) 0.126(19) 0.094(16) 0.007(16) -0.028(12) 0.002(13) C16 0.085(14) 0.102(17) 0.059(13) 0.012(13) 0.029(12) -0.008(13) C17 0.067(13) 0.133(19) 0.075(14) 0.008(14) 0.047(12) -0.005(13) C18 0.089(15) 0.13(2) 0.072(14) -0.028(14) 0.039(13) 0.023(15) C19 0.086(15) 0.126(19) 0.061(13) -0.029(14) 0.024(12) -0.016(15) C20 0.067(12) 0.118(18) 0.047(11) 0.012(12) 0.026(10) 0.006(13) C21 0.060(17) 0.35(7) 0.07(2) 0.05(3) 0.018(16) -0.05(3) C22 0.032(11) 0.15(3) 0.16(3) 0.07(2) 0.031(15) -0.018(14) C23 0.048(13) 0.091(19) 0.16(3) 0.05(2) 0.026(16) -0.003(13) C24 0.080(19) 0.11(2) 0.15(3) 0.04(2) 0.02(2) -0.008(19) C25 0.073(18) 0.14(3) 0.16(3) 0.01(3) 0.06(2) -0.02(2) C26 0.061(16) 0.11(2) 0.19(3) 0.02(2) 0.06(2) 0.018(16) C27 0.048(11) 0.037(12) 0.086(16) 0.020(11) 0.019(12) 0.020(9) B1 0.039(7) 0.013(6) 0.030(7) -0.011(5) 0.024(6) -0.014(5) B2 0.040(8) 0.023(7) 0.074(11) 0.005(8) 0.018(8) -0.006(6) B3 0.039(8) 0.041(9) 0.072(10) 0.006(8) 0.015(8) -0.002(7) B4 0.044(9) 0.035(9) 0.093(12) 0.000(10) 0.023(9) 0.002(8) B5 0.030(7) 0.029(7) 0.086(12) -0.007(8) 0.023(8) 0.002(6) B6 0.034(7) 0.033(8) 0.063(10) -0.018(8) 0.012(7) -0.007(6) B7 0.040(7) 0.012(6) 0.029(7) -0.008(5) 0.028(6) -0.014(5) B8 0.031(8) 0.026(7) 0.053(11) -0.003(8) 0.019(8) -0.004(6) B9 0.033(10) 0.055(14) 0.15(2) -0.009(16) 0.028(13) 0.019(10) Hf1 0.0270(4) 0.0346(5) 0.0316(4) 0.0040(3) 0.0135(3) -0.0004(3) Hf2 0.0251(4) 0.0453(6) 0.0583(6) -0.0088(5) 0.0140(4) -0.0033(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -6.1794 4.9776 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C2 C1 C5 102(3) C2 C1 Hf1 75.0(17) C5 C1 Hf1 71.3(13) C2 C1 H1 128.8 C5 C1 H1 128.8 Hf1 C1 H1 117.6 C3 C2 C1 114(4) C3 C2 Hf1 77(2) C1 C2 Hf1 74.1(18) C3 C2 H2 123.1 C1 C2 H2 123.1 Hf1 C2 H2 117.4 C4 C3 C2 118(4) C4 C3 Hf1 76(2) C2 C3 Hf1 75(2) C4 C3 H3 121.2 C2 C3 H3 121.2 Hf1 C3 H3 118.4 C3 C4 C5 106(3) C3 C4 Hf1 75.6(19) C5 C4 Hf1 70.2(13) C3 C4 H4 127.1 C5 C4 H4 127.1 Hf1 C4 H4 119.2 C4 C5 C1 100(3) C4 C5 Hf1 74.7(13) C1 C5 Hf1 73.0(12) C4 C5 H5 129.7 C1 C5 H5 129.8 Hf1 C5 H5 115.8 C7 C6 C10 109(2) C7 C6 Hf1 75.3(13) C10 C6 Hf1 72.9(11) C7 C6 H6 125.4 C10 C6 H6 125.4 Hf1 C6 H6 118.2 C6 C7 C8 110(2) C6 C7 Hf1 73.7(13) C8 C7 Hf1 73.6(13) C6 C7 H7 124.8 C8 C7 H7 124.8 Hf1 C7 H7 119.5 C7 C8 C9 108(2) C7 C8 Hf1 74.4(13) C9 C8 Hf1 73.6(12) C7 C8 H8 126.0 C9 C8 H8 126.0 Hf1 C8 H8 118.0 C8 C9 C10 105(2) C8 C9 Hf1 73.2(12) C10 C9 Hf1 71.9(11) C8 C9 H9 127.6 C10 C9 H9 127.6 Hf1 C9 H9 119.4 C6 C10 C9 108(2) C6 C10 Hf1 74.4(11) C9 C10 Hf1 74.5(11) C6 C10 H10 126.2 C9 C10 H10 126.2 Hf1 C10 H10 117.1 C12 C11 C15 107(3) C12 C11 Hf2 73.9(16) C15 C11 Hf2 74.0(18) C12 C11 H11 126.7 C15 C11 H11 126.7 Hf2 C11 H11 117.6 C13 C12 C11 110(3) C13 C12 Hf2 73.4(15) C11 C12 Hf2 73.7(17) C13 C12 H12 124.8 C11 C12 H12 124.8 Hf2 C12 H12 119.8 C14 C13 C12 107(3) C14 C13 Hf2 73.3(14) C12 C13 Hf2 74.4(15) C14 C13 H13 126.6 C12 C13 H13 126.6 Hf2 C13 H13 117.9 C13 C14 C15 109(3) C13 C14 Hf2 74.5(12) C15 C14 Hf2 74.7(13) C13 C14 H14 125.3 C15 C14 H14 125.3 Hf2 C14 H14 117.3 C11 C15 C14 107(3) C11 C15 Hf2 73.4(16) C14 C15 Hf2 72.2(13) C11 C15 H15 126.6 C14 C15 H15 126.6 Hf2 C15 H15 119.8 C20 C16 C17 105(3) C20 C16 Hf2 74.5(16) C17 C16 Hf2 73.0(16) C20 C16 H16 127.5 C17 C16 H16 127.5 Hf2 C16 H16 117.4 C16 C17 C18 109(3) C16 C17 Hf2 73.9(14) C18 C17 Hf2 73.5(15) C16 C17 H17 125.5 C18 C17 H17 125.5 Hf2 C17 H17 118.8 C19 C18 C17 106(3) C19 C18 Hf2 75.2(16) C17 C18 Hf2 73.4(14) C19 C18 H18 127.0 C17 C18 H18 127.0 Hf2 C18 H18 116.8 C20 C19 C18 109(3) C20 C19 Hf2 73.8(15) C18 C19 Hf2 72.6(17) C20 C19 H19 125.7 C18 C19 H19 125.7 Hf2 C19 H19 119.7 C19 C20 C16 111(3) C19 C20 Hf2 74.7(17) C16 C20 Hf2 73.5(16) C19 C20 H20 124.4 C16 C20 H20 124.4 Hf2 C20 H20 119.0 C22 C21 H21A 109.5 C22 C21 H21B 109.5 H21A C21 H21B 109.5 C22 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C27 C22 C23 121(2) C27 C22 C21 111(3) C23 C22 C21 127(3) C22 C23 C24 121(2) C22 C23 H23 119.7 C24 C23 H23 119.7 C25 C24 C23 119(2) C25 C24 H24 120.7 C23 C24 H24 120.7 C26 C25 C24 119(2) C26 C25 H25 120.5 C24 C25 H25 120.5 C25 C26 C27 121(2) C25 C26 H26 119.7 C27 C26 H26 119.7 C22 C27 C26 119.4(19) C22 C27 H27 120.3 C26 C27 H27 120.3 B2 B1 B7 103.4(13) B2 B1 B8 143.5(13) B7 B1 B8 112.9(11) B2 B1 B6 62.2(12) B7 B1 B6 62.3(9) B8 B1 B6 139.5(15) B2 B1 B3 60.7(12) B7 B1 B3 58.4(10) B8 B1 B3 138.7(14) B6 B1 B3 76.3(13) B2 B1 Hf1 71.4(9) B7 B1 Hf1 173.9(11) B8 B1 Hf1 72.2(8) B6 B1 Hf1 116.5(9) B3 B1 Hf1 115.6(10) B1 B2 B4 109.0(15) B1 B2 B3 66.4(12) B4 B2 B3 61.1(14) B1 B2 B6 64.0(11) B4 B2 B6 62.3(14) B3 B2 B6 79.3(13) B1 B2 Hf1 69.5(9) B4 B2 Hf1 178.5(14) B3 B2 Hf1 118.1(13) B6 B2 Hf1 116.4(13) B7 B3 B4 94.6(17) B7 B3 B2 94.7(16) B4 B3 B2 55.5(13) B7 B3 B5 53.3(11) B4 B3 B5 55.2(12) B2 B3 B5 96.9(17) B7 B3 B1 54.7(10) B4 B3 B1 94.9(16) B2 B3 B1 53.0(10) B5 B3 B1 95.4(15) B7 B3 H3A 129.8 B4 B3 H3A 128.8 B2 B3 H3A 128.7 B5 B3 H3A 128.4 B1 B3 H3A 129.5 B2 B4 B5 109.4(17) B2 B4 B3 63.4(14) B5 B4 B3 64.3(14) B2 B4 B6 62.9(14) B5 B4 B6 64.9(14) B3 B4 B6 80.6(15) B2 B4 H4A 125.9 B5 B4 H4A 124.7 B3 B4 H4A 139.7 B6 B4 H4A 139.7 B7 B5 B4 104.3(14) B7 B5 B9 142.1(17) B4 B5 B9 113.5(17) B7 B5 B3 61.0(11) B4 B5 B3 60.5(14) B9 B5 B3 142(2) B7 B5 B6 63.0(11) B4 B5 B6 61.1(13) B9 B5 B6 136(2) B3 B5 B6 77.4(13) B7 B5 Hf2 71.0(9) B4 B5 Hf2 175.3(14) B9 B5 Hf2 71.2(12) B3 B5 Hf2 115.6(13) B6 B5 Hf2 116.1(13) B4 B6 B2 54.8(12) B4 B6 B7 90.9(15) B2 B6 B7 92.0(14) B4 B6 B1 95.5(16) B2 B6 B1 53.8(10) B7 B6 B1 54.6(9) B4 B6 B5 54.0(12) B2 B6 B5 95.3(16) B7 B6 B5 51.7(10) B1 B6 B5 96.0(14) B4 B6 H6A 129.9 B2 B6 H6A 129.7 B7 B6 H6A 132.2 B1 B6 H6A 128.0 B5 B6 H6A 129.0 B5 B7 B1 113.6(12) B5 B7 B3 65.7(13) B1 B7 B3 66.9(10) B5 B7 B6 65.4(12) B1 B7 B6 63.1(10) B3 B7 B6 80.2(13) B5 B7 Hf2 70.7(9) B1 B7 Hf2 174.5(11) B3 B7 Hf2 118.6(11) B6 B7 Hf2 117.5(10) B1 B8 Hf1 66.7(7) B1 B8 H8A 113(9) Hf1 B8 H8A 121(9) B1 B8 H8B 112(10) Hf1 B8 H8B 119(10) H8A B8 H8B 115(9) B5 B9 Hf2 67.0(11) B5 B9 H9A 110(9) Hf2 B9 H9A 116(9) B5 B9 H9B 114(9) Hf2 B9 H9B 121(9) H9A B9 H9B 117(9) C5 Hf1 B1 134.7(9) C5 Hf1 C10 80.4(10) B1 Hf1 C10 138.7(7) C5 Hf1 C1 35.7(11) B1 Hf1 C1 132.9(9) C10 Hf1 C1 88.0(10) C5 Hf1 C2 53.3(12) B1 Hf1 C2 101.9(10) C10 Hf1 C2 118.8(11) C1 Hf1 C2 31.0(11) C5 Hf1 B2 135.7(10) B1 Hf1 B2 39.1(6) C10 Hf1 B2 134.9(8) C1 Hf1 B2 108.1(10) C2 Hf1 B2 83.1(11) C5 Hf1 C6 94.3(11) B1 Hf1 C6 130.8(7) C10 Hf1 C6 32.7(8) C1 Hf1 C6 82.2(10) C2 Hf1 C6 106.6(11) B2 Hf1 C6 106.3(8) C5 Hf1 C8 134.1(10) B1 Hf1 C8 85.8(7) C10 Hf1 C8 54.4(8) C1 Hf1 C8 135.2(10) C2 Hf1 C8 154.4(11) B2 Hf1 C8 88.2(9) C6 Hf1 C8 53.0(8) C5 Hf1 C3 51.9(11) B1 Hf1 C3 87.7(9) C10 Hf1 C3 131.9(10) C1 Hf1 C3 50.6(11) C2 Hf1 C3 28.2(11) B2 Hf1 C3 86.6(10) C6 Hf1 C3 132.5(10) C8 Hf1 C3 173.5(9) C5 Hf1 C9 103.3(10) B1 Hf1 C9 106.4(7) C10 Hf1 C9 33.6(7) C1 Hf1 C9 120.7(10) C2 Hf1 C9 151.6(11) B2 Hf1 C9 120.7(9) C6 Hf1 C9 54.5(8) C8 Hf1 C9 33.3(9) C3 Hf1 C9 150.6(11) C5 Hf1 C7 125.3(11) B1 Hf1 C7 99.9(7) C10 Hf1 C7 53.1(8) C1 Hf1 C7 107.7(11) C2 Hf1 C7 122.6(12) B2 Hf1 C7 81.8(9) C6 Hf1 C7 31.0(8) C8 Hf1 C7 31.9(8) C3 Hf1 C7 150.2(10) C9 Hf1 C7 54.0(9) C5 Hf1 C4 35.1(10) B1 Hf1 C4 99.6(8) C10 Hf1 C4 111.9(10) C1 Hf1 C4 55.3(11) C2 Hf1 C4 49.1(12) B2 Hf1 C4 111.8(10) C6 Hf1 C4 129.3(10) C8 Hf1 C4 154.3(10) C3 Hf1 C4 28.0(9) C9 Hf1 C4 122.6(11) C7 Hf1 C4 160.2(10) B5 Hf2 B7 38.3(6) B5 Hf2 C14 139.1(9) B7 Hf2 C14 131.2(7) B5 Hf2 C17 140.2(10) B7 Hf2 C17 135.4(8) C14 Hf2 C17 78.4(10) B5 Hf2 C18 108.8(11) B7 Hf2 C18 122.7(9) C14 Hf2 C18 103.9(10) C17 Hf2 C18 33.1(11) B5 Hf2 C16 131.3(9) B7 Hf2 C16 106.4(8) C14 Hf2 C16 87.8(10) C17 Hf2 C16 33.0(9) C18 Hf2 C16 55.1(11) B5 Hf2 C13 126.5(9) B7 Hf2 C13 101.7(7) C14 Hf2 C13 32.2(9) C17 Hf2 C13 92.2(10) C18 Hf2 C13 124.6(11) C16 Hf2 C13 83.7(10) B5 Hf2 B9 41.8(7) B7 Hf2 B9 80.1(6) C14 Hf2 B9 120.7(10) C17 Hf2 B9 116.1(12) C18 Hf2 B9 84.9(13) C16 Hf2 B9 136.8(12) C13 Hf2 B9 138.0(12) B5 Hf2 C11 84.8(10) B7 Hf2 C11 89.6(9) C14 Hf2 C11 54.3(10) C17 Hf2 C11 131.3(11) C18 Hf2 C11 143.1(12) C16 Hf2 C11 137.8(11) C13 Hf2 C11 54.5(11) B9 Hf2 C11 83.7(13) B5 Hf2 C20 99.6(9) B7 Hf2 C20 82.7(7) C14 Hf2 C20 119.7(9) C17 Hf2 C20 52.8(9) C18 Hf2 C20 53.2(10) C16 Hf2 C20 32.0(9) C13 Hf2 C20 109.6(10) B9 Hf2 C20 112.2(12) C11 Hf2 C20 160.6(12) B5 Hf2 C12 94.8(9) B7 Hf2 C12 78.7(7) C14 Hf2 C12 53.0(8) C17 Hf2 C12 124.4(11) C18 Hf2 C12 156.0(11) C16 Hf2 C12 111.6(11) C13 Hf2 C12 32.2(9) B9 Hf2 C12 111.5(13) C11 Hf2 C12 32.5(11) C20 Hf2 C12 128.1(11) B5 Hf2 C15 109.4(10) B7 Hf2 C15 122.2(9) C14 Hf2 C15 33.2(9) C17 Hf2 C15 100.4(11) C18 Hf2 C15 112.3(11) C16 Hf2 C15 119.3(11) C13 Hf2 C15 54.4(11) B9 Hf2 C15 88.7(11) C11 Hf2 C15 32.6(11) C20 Hf2 C15 150.9(10) C12 Hf2 C15 53.4(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.31(5) C1 C5 1.49(5) C1 Hf1 2.44(2) C1 H1 0.9300 C2 C3 1.20(5) C2 Hf1 2.45(3) C2 H2 0.9300 C3 C4 1.20(4) C3 Hf1 2.47(3) C3 H3 0.9300 C4 C5 1.48(4) C4 Hf1 2.48(3) C4 H4 0.9300 C5 Hf1 2.42(2) C5 H5 0.9300 C6 C7 1.32(3) C6 C10 1.38(3) C6 Hf1 2.457(19) C6 H6 0.9300 C7 C8 1.36(4) C7 Hf1 2.48(2) C7 H7 0.9300 C8 C9 1.41(4) C8 Hf1 2.47(2) C8 H8 0.9300 C9 C10 1.42(3) C9 Hf1 2.47(2) C9 H9 0.9300 C10 Hf1 2.439(18) C10 H10 0.9300 C11 C12 1.40(5) C11 C15 1.41(5) C11 Hf2 2.50(3) C11 H11 0.9300 C12 C13 1.39(4) C12 Hf2 2.50(2) C12 H12 0.9300 C13 C14 1.38(4) C13 Hf2 2.49(2) C13 H13 0.9300 C14 C15 1.42(4) C14 Hf2 2.474(19) C14 H14 0.9300 C15 Hf2 2.51(2) C15 H15 0.9300 C16 C20 1.38(4) C16 C17 1.41(4) C16 Hf2 2.49(3) C16 H16 0.9300 C17 C18 1.41(4) C17 Hf2 2.48(2) C17 H17 0.9300 C18 C19 1.39(4) C18 Hf2 2.48(3) C18 H18 0.9300 C19 C20 1.36(4) C19 Hf2 2.51(3) C19 H19 0.9300 C20 Hf2 2.50(3) C20 H20 0.9300 C21 C22 1.45(2) C21 H21A 0.9600 C21 H21B 0.9600 C21 H21C 0.9600 C22 C27 1.34(2) C22 C23 1.35(2) C23 C24 1.41(3) C23 H23 0.9300 C24 C25 1.39(3) C24 H24 0.9300 C25 C26 1.37(3) C25 H25 0.9300 C26 C27 1.40(3) C26 H26 0.9300 C27 H27 0.9300 B1 B2 1.64(2) B1 B7 1.66(2) B1 B8 1.74(2) B1 B6 1.82(3) B1 B3 1.88(3) B1 Hf1 2.428(15) B2 B4 1.65(3) B2 B3 1.79(3) B2 B6 1.79(3) B2 Hf1 2.46(2) B3 B7 1.74(3) B3 B4 1.75(4) B3 B5 1.81(3) B3 H3A 1.1000 B4 B5 1.65(3) B4 B6 1.78(4) B4 H4A 1.1000 B5 B7 1.59(3) B5 B9 1.75(3) B5 B6 1.84(3) B5 Hf2 2.42(2) B6 B7 1.81(2) B6 H6A 1.1000 B7 Hf2 2.428(15) B8 Hf1 2.517(17) B8 H8A 1.14(8) B8 H8B 1.14(8) B9 Hf2 2.49(3) B9 H9A 1.10(8) B9 H9B 1.14(8) 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 C5 C1 C2 C3 -1(4) Hf1 C1 C2 C3 -67(3) C5 C1 C2 Hf1 66.4(16) C1 C2 C3 C4 0(5) Hf1 C2 C3 C4 -66(3) C1 C2 C3 Hf1 66(3) C2 C3 C4 C5 1(4) Hf1 C3 C4 C5 -64.1(17) C2 C3 C4 Hf1 65(3) C3 C4 C5 C1 -1(3) Hf1 C4 C5 C1 -69.0(14) C3 C4 C5 Hf1 68(2) C2 C1 C5 C4 1(3) Hf1 C1 C5 C4 70.3(15) C2 C1 C5 Hf1 -69(2) C10 C6 C7 C8 -1(3) Hf1 C6 C7 C8 65.1(17) C10 C6 C7 Hf1 -65.6(15) C6 C7 C8 C9 1(3) Hf1 C7 C8 C9 66.4(16) C6 C7 C8 Hf1 -65.1(17) C7 C8 C9 C10 -2(2) Hf1 C8 C9 C10 65.5(14) C7 C8 C9 Hf1 -67.0(16) C7 C6 C10 C9 0(3) Hf1 C6 C10 C9 -67.6(14) C7 C6 C10 Hf1 67.2(17) C8 C9 C10 C6 1(2) Hf1 C9 C10 C6 67.6(15) C8 C9 C10 Hf1 -66.4(14) C15 C11 C12 C13 -3(3) Hf2 C11 C12 C13 64.8(19) C15 C11 C12 Hf2 -67(2) C11 C12 C13 C14 2(3) Hf2 C12 C13 C14 66.6(17) C11 C12 C13 Hf2 -65(2) C12 C13 C14 C15 0(3) Hf2 C13 C14 C15 67.2(18) C12 C13 C14 Hf2 -67.4(17) C12 C11 C15 C14 2(3) Hf2 C11 C15 C14 -64.9(19) C12 C11 C15 Hf2 67(2) C13 C14 C15 C11 -1(3) Hf2 C14 C15 C11 66(2) C13 C14 C15 Hf2 -67.1(17) C20 C16 C17 C18 2(3) Hf2 C16 C17 C18 -66(2) C20 C16 C17 Hf2 68.2(18) C16 C17 C18 C19 -3(3) Hf2 C17 C18 C19 -69(2) C16 C17 C18 Hf2 66.0(19) C17 C18 C19 C20 2(3) Hf2 C18 C19 C20 -66(2) C17 C18 C19 Hf2 67.4(19) C18 C19 C20 C16 0(3) Hf2 C19 C20 C16 -65.0(19) C18 C19 C20 Hf2 65(2) C17 C16 C20 C19 -1(3) Hf2 C16 C20 C19 66(2) C17 C16 C20 Hf2 -67.1(18) C27 C22 C23 C24 -5(4) C21 C22 C23 C24 -179(3) C22 C23 C24 C25 0(5) C23 C24 C25 C26 4(5) C24 C25 C26 C27 -3(5) C23 C22 C27 C26 6(4) C21 C22 C27 C26 -180(2) C25 C26 C27 C22 -2(4) B7 B1 B2 B4 4(2) B8 B1 B2 B4 178(2) B6 B1 B2 B4 -44.5(18) B3 B1 B2 B4 44.9(18) Hf1 B1 B2 B4 -180(2) B7 B1 B2 B3 -41.2(14) B8 B1 B2 B3 134(3) B6 B1 B2 B3 -89.4(13) Hf1 B1 B2 B3 135.5(13) B7 B1 B2 B6 48.2(13) B8 B1 B2 B6 -137(3) B3 B1 B2 B6 89.4(13) Hf1 B1 B2 B6 -135.2(12) B7 B1 B2 Hf1 -176.6(11) B8 B1 B2 Hf1 -2(3) B6 B1 B2 Hf1 135.2(12) B3 B1 B2 Hf1 -135.5(13) B1 B2 B3 B7 38.0(12) B4 B2 B3 B7 -92.3(17) B6 B2 B3 B7 -28.2(13) Hf1 B2 B3 B7 86.2(15) B1 B2 B3 B4 130.3(18) B6 B2 B3 B4 64.2(15) Hf1 B2 B3 B4 178.5(19) B1 B2 B3 B5 91.6(15) B4 B2 B3 B5 -38.8(15) B6 B2 B3 B5 25.4(14) Hf1 B2 B3 B5 139.7(14) B4 B2 B3 B1 -130.3(18) B6 B2 B3 B1 -66.2(11) Hf1 B2 B3 B1 48.2(11) B2 B1 B3 B7 -131.2(16) B8 B1 B3 B7 89.5(19) B6 B1 B3 B7 -65.7(11) Hf1 B1 B3 B7 -178.7(11) B2 B1 B3 B4 -39.1(14) B7 B1 B3 B4 92.1(14) B8 B1 B3 B4 -178.4(16) B6 B1 B3 B4 26.5(12) Hf1 B1 B3 B4 -86.6(14) B7 B1 B3 B2 131.2(16) B8 B1 B3 B2 -139(2) B6 B1 B3 B2 65.6(13) Hf1 B1 B3 B2 -47.5(13) B2 B1 B3 B5 -94.6(16) B7 B1 B3 B5 36.7(11) B8 B1 B3 B5 126.2(18) B6 B1 B3 B5 -29.0(12) Hf1 B1 B3 B5 -142.0(10) B1 B2 B4 B5 -1(3) B3 B2 B4 B5 46.3(19) B6 B2 B4 B5 -46.7(18) B1 B2 B4 B3 -47.6(17) B6 B2 B4 B3 -92.9(14) B1 B2 B4 B6 45.3(16) B3 B2 B4 B6 92.9(14) B7 B3 B4 B2 92.6(16) B5 B3 B4 B2 130.8(19) B1 B3 B4 B2 37.7(13) B7 B3 B4 B5 -38.3(14) B2 B3 B4 B5 -130.8(19) B1 B3 B4 B5 -93.2(15) B7 B3 B4 B6 28.3(12) B2 B3 B4 B6 -64.3(13) B5 B3 B4 B6 66.5(14) B1 B3 B4 B6 -26.6(12) B2 B4 B5 B7 -2(3) B3 B4 B5 B7 44.1(16) B6 B4 B5 B7 -47.4(16) B2 B4 B5 B9 176(2) B3 B4 B5 B9 -138(2) B6 B4 B5 B9 131(2) B2 B4 B5 B3 -45.8(19) B6 B4 B5 B3 -91.5(14) B2 B4 B5 B6 45.6(18) B3 B4 B5 B6 91.5(14) B4 B3 B5 B7 -129.6(18) B2 B3 B5 B7 -90.7(14) B1 B3 B5 B7 -37.4(11) B7 B3 B5 B4 129.6(18) B2 B3 B5 B4 38.9(15) B1 B3 B5 B4 92.2(16) B7 B3 B5 B9 -139(3) B4 B3 B5 B9 91(3) B2 B3 B5 B9 130(3) B1 B3 B5 B9 -177(2) B7 B3 B5 B6 65.9(12) B4 B3 B5 B6 -63.8(14) B2 B3 B5 B6 -24.8(13) B1 B3 B5 B6 28.4(12) B7 B3 B5 Hf2 -47.2(13) B4 B3 B5 Hf2 -176.9(19) B2 B3 B5 Hf2 -137.9(13) B1 B3 B5 Hf2 -84.7(14) B5 B4 B6 B2 130.7(18) B3 B4 B6 B2 64.8(13) B2 B4 B6 B7 -91.8(14) B5 B4 B6 B7 38.9(13) B3 B4 B6 B7 -27.0(12) B2 B4 B6 B1 -37.3(13) B5 B4 B6 B1 93.4(14) B3 B4 B6 B1 27.5(12) B2 B4 B6 B5 -130.7(18) B3 B4 B6 B5 -65.9(14) B1 B2 B6 B4 -131.6(17) B3 B2 B6 B4 -62.8(14) Hf1 B2 B6 B4 -179.1(18) B1 B2 B6 B7 -41.9(12) B4 B2 B6 B7 89.7(15) B3 B2 B6 B7 26.9(12) Hf1 B2 B6 B7 -89.4(14) B4 B2 B6 B1 131.6(17) B3 B2 B6 B1 68.8(12) Hf1 B2 B6 B1 -47.5(11) B1 B2 B6 B5 -93.6(14) B4 B2 B6 B5 38.0(14) B3 B2 B6 B5 -24.8(13) Hf1 B2 B6 B5 -141.1(12) B2 B1 B6 B4 37.9(13) B7 B1 B6 B4 -87.2(13) B8 B1 B6 B4 179.3(17) B3 B1 B6 B4 -25.9(12) Hf1 B1 B6 B4 86.1(13) B7 B1 B6 B2 -125.0(15) B8 B1 B6 B2 141(2) B3 B1 B6 B2 -63.8(12) Hf1 B1 B6 B2 48.2(12) B2 B1 B6 B7 125.0(15) B8 B1 B6 B7 -93.5(19) B3 B1 B6 B7 61.2(11) Hf1 B1 B6 B7 173.3(13) B2 B1 B6 B5 92.2(16) B7 B1 B6 B5 -32.8(11) B8 B1 B6 B5 -126.3(19) B3 B1 B6 B5 28.4(12) Hf1 B1 B6 B5 140.4(11) B7 B5 B6 B4 126.8(17) B9 B5 B6 B4 -95(3) B3 B5 B6 B4 63.1(15) Hf2 B5 B6 B4 175.7(19) B7 B5 B6 B2 88.3(13) B4 B5 B6 B2 -38.4(15) B9 B5 B6 B2 -133(2) B3 B5 B6 B2 24.6(13) Hf2 B5 B6 B2 137.2(13) B4 B5 B6 B7 -126.8(17) B9 B5 B6 B7 138(3) B3 B5 B6 B7 -63.7(11) Hf2 B5 B6 B7 48.9(11) B7 B5 B6 B1 34.3(11) B4 B5 B6 B1 -92.5(16) B9 B5 B6 B1 173(2) B3 B5 B6 B1 -29.4(13) Hf2 B5 B6 B1 83.2(15) B4 B5 B7 B1 4(2) B9 B5 B7 B1 -173(3) B3 B5 B7 B1 48.1(15) B6 B5 B7 B1 -42.0(15) Hf2 B5 B7 B1 -176.3(13) B4 B5 B7 B3 -43.8(18) B9 B5 B7 B3 139(4) B6 B5 B7 B3 -90.1(13) Hf2 B5 B7 B3 135.6(12) B4 B5 B7 B6 46.4(17) B9 B5 B7 B6 -131(4) B3 B5 B7 B6 90.1(13) Hf2 B5 B7 B6 -134.3(12) B4 B5 B7 Hf2 -179(2) B9 B5 B7 Hf2 3(3) B3 B5 B7 Hf2 -135.6(12) B6 B5 B7 Hf2 134.3(12) B2 B1 B7 B5 -5(2) B8 B1 B7 B5 178.3(15) B6 B1 B7 B5 43.0(16) B3 B1 B7 B5 -47.5(16) B2 B1 B7 B3 42.4(15) B8 B1 B7 B3 -134.2(16) B6 B1 B7 B3 90.5(14) B2 B1 B7 B6 -48.1(15) B8 B1 B7 B6 135.3(16) B3 B1 B7 B6 -90.5(14) B4 B3 B7 B5 39.4(13) B2 B3 B7 B5 95.1(16) B1 B3 B7 B5 132.1(14) B4 B3 B7 B1 -92.8(13) B2 B3 B7 B1 -37.0(11) B5 B3 B7 B1 -132.1(14) B4 B3 B7 B6 -27.9(12) B2 B3 B7 B6 27.8(13) B5 B3 B7 B6 -67.3(12) B1 B3 B7 B6 64.9(10) B4 B3 B7 Hf2 88.2(14) B2 B3 B7 Hf2 143.9(11) B5 B3 B7 Hf2 48.8(13) B1 B3 B7 Hf2 -179.1(12) B4 B6 B7 B5 -40.4(14) B2 B6 B7 B5 -95.2(15) B1 B6 B7 B5 -136.6(15) B4 B6 B7 B1 96.2(14) B2 B6 B7 B1 41.4(11) B5 B6 B7 B1 136.6(15) B4 B6 B7 B3 27.2(13) B2 B6 B7 B3 -27.6(13) B1 B6 B7 B3 -69.0(11) B5 B6 B7 B3 67.6(13) B4 B6 B7 Hf2 -90.0(13) B2 B6 B7 Hf2 -144.8(11) B1 B6 B7 Hf2 173.8(13) B5 B6 B7 Hf2 -49.6(13) B2 B1 B8 Hf1 2(3) B7 B1 B8 Hf1 176.3(13) B6 B1 B8 Hf1 -110.1(18) B3 B1 B8 Hf1 108.8(17) B7 B5 B9 Hf2 -3(3) B4 B5 B9 Hf2 179(2) B3 B5 B9 Hf2 108(3) B6 B5 B9 Hf2 -108(2)