# Electronic Supplementary Material (ESI) for CrystEngComm # 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_DUT-52(Zr) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H36 O32 Zr6' _chemical_formula_weight 1960.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0060 0.0030 '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' O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -1.2060 0.8400 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Fm-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y, x+1/2, -z+1/2' '-y, -x+1/2, -z+1/2' 'y, -x+1/2, z+1/2' '-y, x+1/2, z+1/2' 'x, z+1/2, -y+1/2' '-x, z+1/2, y+1/2' '-x, -z+1/2, -y+1/2' 'x, -z+1/2, y+1/2' 'z, y+1/2, -x+1/2' 'z, -y+1/2, x+1/2' '-z, y+1/2, x+1/2' '-z, -y+1/2, -x+1/2' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1/2, x, -z+1/2' '-y+1/2, -x, -z+1/2' 'y+1/2, -x, z+1/2' '-y+1/2, x, z+1/2' 'x+1/2, z, -y+1/2' '-x+1/2, z, y+1/2' '-x+1/2, -z, -y+1/2' 'x+1/2, -z, y+1/2' 'z+1/2, y, -x+1/2' 'z+1/2, -y, x+1/2' '-z+1/2, y, x+1/2' '-z+1/2, -y, -x+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1/2, x+1/2, -z' '-y+1/2, -x+1/2, -z' 'y+1/2, -x+1/2, z' '-y+1/2, x+1/2, z' 'x+1/2, z+1/2, -y' '-x+1/2, z+1/2, y' '-x+1/2, -z+1/2, -y' 'x+1/2, -z+1/2, y' 'z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, x' '-z+1/2, y+1/2, x' '-z+1/2, -y+1/2, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' '-x, -y+1/2, -z+1/2' 'x, y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' '-x, y+1/2, z+1/2' '-z, -x+1/2, -y+1/2' '-z, x+1/2, y+1/2' 'z, x+1/2, -y+1/2' 'z, -x+1/2, y+1/2' '-y, -z+1/2, -x+1/2' 'y, -z+1/2, x+1/2' '-y, z+1/2, x+1/2' 'y, z+1/2, -x+1/2' '-y, -x+1/2, z+1/2' 'y, x+1/2, z+1/2' '-y, x+1/2, -z+1/2' 'y, -x+1/2, -z+1/2' '-x, -z+1/2, y+1/2' 'x, -z+1/2, -y+1/2' 'x, z+1/2, y+1/2' '-x, z+1/2, -y+1/2' '-z, -y+1/2, x+1/2' '-z, y+1/2, -x+1/2' 'z, -y+1/2, -x+1/2' 'z, y+1/2, x+1/2' '-x+1/2, -y, -z+1/2' 'x+1/2, y, -z+1/2' 'x+1/2, -y, z+1/2' '-x+1/2, y, z+1/2' '-z+1/2, -x, -y+1/2' '-z+1/2, x, y+1/2' 'z+1/2, x, -y+1/2' 'z+1/2, -x, y+1/2' '-y+1/2, -z, -x+1/2' 'y+1/2, -z, x+1/2' '-y+1/2, z, x+1/2' 'y+1/2, z, -x+1/2' '-y+1/2, -x, z+1/2' 'y+1/2, x, z+1/2' '-y+1/2, x, -z+1/2' 'y+1/2, -x, -z+1/2' '-x+1/2, -z, y+1/2' 'x+1/2, -z, -y+1/2' 'x+1/2, z, y+1/2' '-x+1/2, z, -y+1/2' '-z+1/2, -y, x+1/2' '-z+1/2, y, -x+1/2' 'z+1/2, -y, -x+1/2' 'z+1/2, y, x+1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' '-z+1/2, -x+1/2, -y' '-z+1/2, x+1/2, y' 'z+1/2, x+1/2, -y' 'z+1/2, -x+1/2, y' '-y+1/2, -z+1/2, -x' 'y+1/2, -z+1/2, x' '-y+1/2, z+1/2, x' 'y+1/2, z+1/2, -x' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' '-y+1/2, x+1/2, -z' 'y+1/2, -x+1/2, -z' '-x+1/2, -z+1/2, y' 'x+1/2, -z+1/2, -y' 'x+1/2, z+1/2, y' '-x+1/2, z+1/2, -y' '-z+1/2, -y+1/2, x' '-z+1/2, y+1/2, -x' 'z+1/2, -y+1/2, -x' 'z+1/2, y+1/2, x' _cell_length_a 23.910(3) _cell_length_b 23.910(3) _cell_length_c 23.910(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13669(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1373 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 31.53 _exptl_crystal_description octahedron _exptl_crystal_colour colorless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.953 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3856 _exptl_absorpt_coefficient_mu 0.872 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9743 _exptl_absorpt_correction_T_max 0.9743 _exptl_absorpt_process_details Scala _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.88561 _diffrn_source synchrotron _diffrn_source_type 'BESSY BL MX-14.2' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'MX-225 CCD' _diffrn_measurement_method '\D\f scans' _diffrn_reflns_number 1270 _diffrn_reflns_av_R_equivalents 0.1041 _diffrn_reflns_av_sigmaI/netI 0.1483 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 2 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 4.63 _diffrn_reflns_theta_max 34.09 _reflns_number_total 752 _reflns_number_gt 689 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marCCD 1994-2002' _computing_cell_refinement 'mosflm 1.0.5' _computing_data_reduction scala _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material WinGX _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^)+(0.0677P)^2^+85.8191P] 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 SHELXL _refine_ls_extinction_coef 0.0025(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 752 _refine_ls_number_parameters 48 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.1934 _refine_ls_wR_factor_gt 0.1881 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.093 _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 Zr1 Zr 0.0000 0.0000 0.10347(2) 0.0219(6) Uani 1 8 d S . . O1 O 0.0509(2) 0.0509(2) 0.0509(2) 0.063(3) Uani 1 6 d S . . O2 O 0.0000 0.0805(3) 0.1496(2) 0.0805(18) Uani 1 2 d SD . . C1 C 0.0000 0.1319(2) 0.1319(2) 0.085(5) Uani 1 4 d SD . . C2 C 0.0000 0.1679(6) 0.1847(6) 0.124(11) Uani 0.50 2 d SPD . . C3 C 0.0000 0.2243(5) 0.1774(4) 0.081(6) Uani 0.50 2 d SPD . . H3A H 0.0000 0.2390 0.1414 0.097 Uiso 0.50 2 calc SPR . . C4 C 0.0000 0.1475(6) 0.2371(5) 0.20(3) Uani 0.50 2 d SPD . . H4A H 0.0000 0.1088 0.2417 0.244 Uiso 0.50 2 calc SPR . . C5 C 0.0000 0.1804(5) 0.2844(5) 0.174(19) Uani 0.50 2 d SPD . . H5A H 0.0000 0.1647 0.3200 0.209 Uiso 0.50 2 calc SPR . . C6 C 0.0000 0.2398(3) 0.2766(3) 0.077(6) Uani 0.50 2 d SPD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0318(6) 0.0318(6) 0.0022(6) 0.000 0.000 0.000 O1 0.063(3) 0.063(3) 0.063(3) 0.041(3) 0.041(3) 0.041(3) O2 0.094(4) 0.088(4) 0.060(3) -0.068(3) 0.000 0.000 C1 0.082(8) 0.087(7) 0.087(7) -0.080(9) 0.000 0.000 C2 0.121(13) 0.13(2) 0.12(2) -0.114(19) 0.000 0.000 C3 0.19(2) 0.043(8) 0.011(5) -0.009(6) 0.000 0.000 C4 0.53(8) 0.029(9) 0.048(10) 0.004(9) 0.000 0.000 C5 0.46(6) 0.030(7) 0.034(7) 0.002(7) 0.000 0.000 C6 0.153(15) 0.036(7) 0.042(8) -0.010(8) 0.000 0.000 _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 Zr1 O1 2.131(3) . ? Zr1 O1 2.131(3) 2 ? Zr1 O1 2.131(3) 100 ? Zr1 O1 2.131(3) 99 ? Zr1 O2 2.217(5) . ? Zr1 O2 2.217(5) 110 ? Zr1 O2 2.217(5) 109 ? Zr1 O2 2.217(5) 2 ? Zr1 Zr1 3.4988(9) 105 ? Zr1 Zr1 3.4988(9) 101 ? Zr1 Zr1 3.4988(9) 5 ? Zr1 Zr1 3.4988(9) 9 ? O1 Zr1 2.131(3) 9 ? O1 Zr1 2.131(3) 5 ? O2 C1 1.301(8) . ? C1 O2 1.301(8) 18 ? C1 C2 1.527(12) 18 ? C1 C2 1.527(12) . ? C2 C2 0.57(3) 18 ? C2 C3 0.974(16) 18 ? C2 C4 1.345(16) . ? C2 C3 1.358(16) . ? C2 C4 1.88(2) 18 ? C3 C6 1.395(11) 121 ? C3 H3A 0.9300 . ? C4 C5 1.379(14) . ? C4 H4A 0.9300 . ? C5 C6 1.431(13) . ? C5 H5A 0.9300 . ? C6 C6 0.555(16) 138 ? C6 C5 1.178(13) 138 ? C6 C6 1.247(15) 18 ? C6 C6 1.365(15) 121 ? C6 C3 1.395(11) 121 ? C6 C4 1.897(17) 138 ? C6 C3 1.947(12) 18 ? C6 C3 1.980(14) 138 ? 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 Zr1 O1 107.6(5) . 2 ? O1 Zr1 O1 69.6(3) . 100 ? O1 Zr1 O1 69.6(3) 2 100 ? O1 Zr1 O1 69.6(3) . 99 ? O1 Zr1 O1 69.6(3) 2 99 ? O1 Zr1 O1 107.6(5) 100 99 ? O1 Zr1 O2 78.4(3) . . ? O1 Zr1 O2 142.07(7) 2 . ? O1 Zr1 O2 78.4(3) 100 . ? O1 Zr1 O2 142.07(7) 99 . ? O1 Zr1 O2 78.4(3) . 110 ? O1 Zr1 O2 142.07(7) 2 110 ? O1 Zr1 O2 142.07(7) 100 110 ? O1 Zr1 O2 78.4(3) 99 110 ? O2 Zr1 O2 75.68(17) . 110 ? O1 Zr1 O2 142.07(7) . 109 ? O1 Zr1 O2 78.4(3) 2 109 ? O1 Zr1 O2 78.4(3) 100 109 ? O1 Zr1 O2 142.07(7) 99 109 ? O2 Zr1 O2 75.68(17) . 109 ? O2 Zr1 O2 120.4(4) 110 109 ? O1 Zr1 O2 142.07(7) . 2 ? O1 Zr1 O2 78.4(3) 2 2 ? O1 Zr1 O2 142.07(7) 100 2 ? O1 Zr1 O2 78.4(3) 99 2 ? O2 Zr1 O2 120.4(4) . 2 ? O2 Zr1 O2 75.68(17) 110 2 ? O2 Zr1 O2 75.68(17) 109 2 ? O1 Zr1 Zr1 89.2(2) . 105 ? O1 Zr1 Zr1 34.82(13) 2 105 ? O1 Zr1 Zr1 89.2(2) 100 105 ? O1 Zr1 Zr1 34.82(13) 99 105 ? O2 Zr1 Zr1 164.82(19) . 105 ? O2 Zr1 Zr1 110.59(12) 110 105 ? O2 Zr1 Zr1 110.59(12) 109 105 ? O2 Zr1 Zr1 74.82(19) 2 105 ? O1 Zr1 Zr1 89.2(2) . 101 ? O1 Zr1 Zr1 34.82(13) 2 101 ? O1 Zr1 Zr1 34.82(13) 100 101 ? O1 Zr1 Zr1 89.2(2) 99 101 ? O2 Zr1 Zr1 110.59(12) . 101 ? O2 Zr1 Zr1 164.82(19) 110 101 ? O2 Zr1 Zr1 74.82(19) 109 101 ? O2 Zr1 Zr1 110.59(12) 2 101 ? Zr1 Zr1 Zr1 60.0 105 101 ? O1 Zr1 Zr1 34.82(13) . 5 ? O1 Zr1 Zr1 89.2(2) 2 5 ? O1 Zr1 Zr1 89.2(2) 100 5 ? O1 Zr1 Zr1 34.82(13) 99 5 ? O2 Zr1 Zr1 110.59(12) . 5 ? O2 Zr1 Zr1 74.82(19) 110 5 ? O2 Zr1 Zr1 164.82(19) 109 5 ? O2 Zr1 Zr1 110.59(12) 2 5 ? Zr1 Zr1 Zr1 60.0 105 5 ? Zr1 Zr1 Zr1 90.0 101 5 ? O1 Zr1 Zr1 34.82(13) . 9 ? O1 Zr1 Zr1 89.2(2) 2 9 ? O1 Zr1 Zr1 34.82(13) 100 9 ? O1 Zr1 Zr1 89.2(2) 99 9 ? O2 Zr1 Zr1 74.82(19) . 9 ? O2 Zr1 Zr1 110.59(12) 110 9 ? O2 Zr1 Zr1 110.59(12) 109 9 ? O2 Zr1 Zr1 164.82(19) 2 9 ? Zr1 Zr1 Zr1 90.0 105 9 ? Zr1 Zr1 Zr1 60.0 101 9 ? Zr1 Zr1 Zr1 60.0 5 9 ? Zr1 O1 Zr1 110.4(3) 9 5 ? Zr1 O1 Zr1 110.4(3) 9 . ? Zr1 O1 Zr1 110.4(3) 5 . ? C1 O2 Zr1 131.2(5) . . ? O2 C1 O2 127.9(7) 18 . ? O2 C1 C2 105.4(7) 18 18 ? O2 C1 C2 126.7(7) . 18 ? O2 C1 C2 126.7(7) 18 . ? O2 C1 C2 105.4(7) . . ? C2 C1 C2 21.4(12) 18 . ? C2 C2 C3 121.5(12) 18 18 ? C2 C2 C4 156.3(8) 18 . ? C3 C2 C4 34.8(9) 18 . ? C2 C2 C3 37.7(7) 18 . ? C3 C2 C3 83.8(14) 18 . ? C4 C2 C3 118.6(11) . . ? C2 C2 C1 79.3(6) 18 . ? C3 C2 C1 159.2(17) 18 . ? C4 C2 C1 124.4(12) . . ? C3 C2 C1 117.0(11) . . ? C2 C2 C4 16.7(5) 18 18 ? C3 C2 C4 104.8(14) 18 18 ? C4 C2 C4 139.6(12) . 18 ? C3 C2 C4 21.0(5) . 18 ? C1 C2 C4 96.0(8) . 18 ? C2 C3 C6 120.7(10) . 121 ? C2 C3 H3A 119.6 . . ? C6 C3 H3A 119.6 121 . ? C2 C4 C5 123.8(12) . . ? C2 C4 H4A 118.1 . . ? C5 C4 H4A 118.1 . . ? C4 C5 C6 117.4(9) . . ? C4 C5 H5A 121.3 . . ? C6 C5 H5A 121.3 . . ? C6 C6 C5 105.6(8) 138 138 ? C6 C6 C6 90.000(2) 138 18 ? C5 C6 C6 164.4(8) 138 18 ? C6 C6 C6 66.0(7) 138 121 ? C5 C6 C6 171.6(13) 138 121 ? C6 C6 C6 24.0(7) 18 121 ? C6 C6 C3 173.1(6) 138 121 ? C5 C6 C3 67.4(9) 138 121 ? C6 C6 C3 96.9(6) 18 121 ? C6 C6 C3 120.9(9) 121 121 ? C6 C6 C5 52.5(6) 138 . ? C5 C6 C5 53.2(12) 138 . ? C6 C6 C5 142.5(6) 18 . ? C6 C6 C5 118.5(10) 121 . ? C3 C6 C5 120.6(10) 121 . ? C6 C6 C4 152.0(5) 138 138 ? C5 C6 C4 46.4(7) 138 138 ? C6 C6 C4 118.0(5) 18 138 ? C6 C6 C4 142.0(10) 121 138 ? C3 C6 C4 21.1(6) 121 138 ? C5 C6 C4 99.5(9) . 138 ? C6 C6 C3 5.0(4) 138 18 ? C5 C6 C3 100.7(9) 138 18 ? C6 C6 C3 95.0(4) 18 18 ? C6 C6 C3 71.0(8) 121 18 ? C3 C6 C3 168.1(10) 121 18 ? C5 C6 C3 47.5(6) . 18 ? C4 C6 C3 147.0(7) 138 18 ? C6 C6 C3 134.4(4) 138 138 ? C5 C6 C3 120.0(9) 138 138 ? C6 C6 C3 44.4(4) 18 138 ? C6 C6 C3 68.4(8) 121 138 ? C3 C6 C3 52.6(8) 121 138 ? C5 C6 C3 173.2(7) . 138 ? C4 C6 C3 73.7(6) 138 138 ? C3 C6 C3 139.3(4) 18 138 ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 34.09 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.303 _refine_diff_density_min -1.259 _refine_diff_density_rms 0.126 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 -0.009 -0.006 0.407 7663 1235 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 937877' ####################################################################### # # 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_immm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H24 Hf6 O32' _chemical_formula_weight 2183.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0060 0.0030 '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' Hf Hf -1.6680 8.8820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Immm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x, y, z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 16.994(3) _cell_length_b 18.454(4) _cell_length_c 22.477(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7049(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 452 _cell_measurement_theta_min 3.26 _cell_measurement_theta_max 26.34 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.029 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 7.782 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8001 _exptl_absorpt_correction_T_max 0.8599 _exptl_absorpt_process_details Scala _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.88561 _diffrn_source synchrotron _diffrn_source_type 'BESSY BL MX-14.2' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'MX-225 CCD' _diffrn_measurement_method '\D\f scans' _diffrn_reflns_number 29050 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 36.99 _reflns_number_total 4554 _reflns_number_gt 4153 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marCCD 1994-2002' _computing_cell_refinement 'mosflm 1.0.5' _computing_data_reduction scala _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material WinGX _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^)+(0.0926P)^2^+114.6673P] 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 4554 _refine_ls_number_parameters 93 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.175 _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 0.5000 0.0000 0.109319(17) 0.00874(14) Uani 1 4 d S . . Hf2 Hf 0.39648(2) 0.09492(2) 0.0000 0.01781(15) Uani 1 2 d S . . O1 O 0.3976(8) 0.0000 0.0537(4) 0.069(3) Uani 1 2 d S . . O2 O 0.5000 -0.0950(8) 0.0529(4) 0.073(3) Uani 1 2 d S . . O3 O 0.2706(5) 0.0845(7) 0.0000 0.073(3) Uani 1 2 d S . . O4 O 0.4040(8) 0.2124(5) 0.0000 0.069(3) Uani 1 2 d S . . O5 O 0.3537(3) 0.1331(3) 0.0896(2) 0.0324(9) Uani 1 1 d U . . O6 O 0.4214(3) 0.0730(3) 0.1596(2) 0.0324(9) Uani 1 1 d U . . C1 C 0.3739(5) 0.1190(5) 0.1427(3) 0.0334(17) Uani 1 1 d U . . C2 C 0.3338(6) 0.1628(5) 0.1906(3) 0.047(2) Uani 1 1 d U . . C3 C 0.3533(9) 0.1523(8) 0.2496(4) 0.094(6) Uani 1 1 d U . . H3 H 0.3910 0.1178 0.2596 0.112 Uiso 1 1 calc R . . C4 C 0.2773(7) 0.2132(6) 0.1758(3) 0.061(3) Uani 1 1 d U . . H4 H 0.2639 0.2200 0.1361 0.073 Uiso 1 1 calc R . . C5 C 0.2396(7) 0.2546(6) 0.2199(4) 0.058(3) Uani 1 1 d U . . C6 C 0.1824(10) 0.3076(9) 0.2061(4) 0.107(7) Uani 1 1 d U . . H6 H 0.1687 0.3156 0.1666 0.129 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 0.0133(2) 0.0115(2) 0.0014(2) 0.000 0.000 0.000 Hf2 0.0248(2) 0.0231(2) 0.00554(19) 0.000 0.000 0.01522(14) O1 0.144(9) 0.021(3) 0.041(4) 0.000 -0.068(5) 0.000 O2 0.018(3) 0.159(9) 0.042(4) -0.072(6) 0.000 0.000 O3 0.018(3) 0.159(9) 0.042(4) -0.072(6) 0.000 0.000 O4 0.144(9) 0.021(3) 0.041(4) 0.000 -0.068(5) 0.000 O5 0.044(2) 0.041(2) 0.0129(15) -0.0043(15) 0.0040(15) 0.0371(18) O6 0.044(2) 0.041(2) 0.0129(15) -0.0043(15) 0.0040(15) 0.0371(18) C1 0.047(4) 0.044(4) 0.010(3) -0.007(3) 0.009(3) 0.017(4) C2 0.070(6) 0.056(5) 0.015(3) -0.009(3) 0.014(4) 0.040(5) C3 0.140(12) 0.123(11) 0.018(4) -0.017(5) 0.002(6) 0.117(11) C4 0.092(8) 0.080(7) 0.010(3) -0.008(4) 0.001(4) 0.068(6) C5 0.086(7) 0.070(6) 0.019(4) -0.005(4) 0.008(4) 0.059(6) C6 0.157(14) 0.153(13) 0.012(4) -0.022(6) 0.002(6) 0.119(12) _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 2.143(10) 2_655 ? Hf1 O1 2.143(10) . ? Hf1 O2 2.163(10) 2_655 ? Hf1 O2 2.163(10) . ? Hf1 O6 2.207(4) 11_655 ? Hf1 O6 2.207(4) 12 ? Hf1 O6 2.207(4) 2_655 ? Hf1 O6 2.207(4) . ? Hf1 Hf2 3.4929(5) . ? Hf1 Hf2 3.4930(5) 3 ? Hf1 Hf2 3.4930(5) 9_655 ? Hf1 Hf2 3.4930(5) 11_655 ? Hf2 O2 2.124(6) 2_655 ? Hf2 O2 2.124(6) 9_655 ? Hf2 O1 2.128(6) 10 ? Hf2 O1 2.128(6) . ? Hf2 O3 2.147(9) . ? Hf2 O4 2.172(9) . ? Hf2 O5 2.253(4) 10 ? Hf2 O5 2.253(4) . ? Hf2 Hf1 3.4930(5) 9_655 ? Hf2 Hf2 3.5032(10) 3 ? Hf2 Hf2 3.5186(10) 11_655 ? O1 Hf2 2.128(6) 3 ? O2 Hf2 2.124(6) 3 ? O2 Hf2 2.124(6) 9_655 ? O5 C1 1.269(9) . ? O6 C1 1.232(10) . ? C1 C2 1.510(9) . ? C2 C4 1.378(11) . ? C2 C3 1.380(12) . ? C3 C6 1.381(11) 13 ? C3 H3 0.9300 . ? C4 C5 1.406(10) . ? C4 H4 0.9300 . ? C5 C5 1.408(16) 13 ? C5 C6 1.413(14) . ? C6 C3 1.381(11) 13 ? C6 H6 0.9300 . ? 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 O1 108.7(7) 2_655 . ? O1 Hf1 O2 70.0(3) 2_655 2_655 ? O1 Hf1 O2 70.0(3) . 2_655 ? O1 Hf1 O2 70.0(3) 2_655 . ? O1 Hf1 O2 70.0(3) . . ? O2 Hf1 O2 108.3(8) 2_655 . ? O1 Hf1 O6 78.9(3) 2_655 11_655 ? O1 Hf1 O6 142.17(17) . 11_655 ? O2 Hf1 O6 78.8(3) 2_655 11_655 ? O2 Hf1 O6 142.57(17) . 11_655 ? O1 Hf1 O6 142.17(17) 2_655 12 ? O1 Hf1 O6 78.9(3) . 12 ? O2 Hf1 O6 142.57(17) 2_655 12 ? O2 Hf1 O6 78.8(3) . 12 ? O6 Hf1 O6 118.5(2) 11_655 12 ? O1 Hf1 O6 78.9(3) 2_655 2_655 ? O1 Hf1 O6 142.17(17) . 2_655 ? O2 Hf1 O6 142.57(17) 2_655 2_655 ? O2 Hf1 O6 78.8(3) . 2_655 ? O6 Hf1 O6 75.2(3) 11_655 2_655 ? O6 Hf1 O6 74.5(3) 12 2_655 ? O1 Hf1 O6 142.17(17) 2_655 . ? O1 Hf1 O6 78.9(3) . . ? O2 Hf1 O6 78.8(3) 2_655 . ? O2 Hf1 O6 142.57(17) . . ? O6 Hf1 O6 74.5(3) 11_655 . ? O6 Hf1 O6 75.2(3) 12 . ? O6 Hf1 O6 118.5(2) 2_655 . ? O1 Hf1 Hf2 89.9(3) 2_655 . ? O1 Hf1 Hf2 34.98(18) . . ? O2 Hf1 Hf2 35.07(18) 2_655 . ? O2 Hf1 Hf2 89.7(3) . . ? O6 Hf1 Hf2 111.02(15) 11_655 . ? O6 Hf1 Hf2 111.16(16) 12 . ? O6 Hf1 Hf2 166.06(12) 2_655 . ? O6 Hf1 Hf2 75.47(12) . . ? O1 Hf1 Hf2 89.9(3) 2_655 3 ? O1 Hf1 Hf2 34.98(18) . 3 ? O2 Hf1 Hf2 89.7(3) 2_655 3 ? O2 Hf1 Hf2 35.07(18) . 3 ? O6 Hf1 Hf2 166.06(12) 11_655 3 ? O6 Hf1 Hf2 75.47(12) 12 3 ? O6 Hf1 Hf2 111.02(15) 2_655 3 ? O6 Hf1 Hf2 111.16(16) . 3 ? Hf2 Hf1 Hf2 60.194(18) . 3 ? O1 Hf1 Hf2 34.98(18) 2_655 9_655 ? O1 Hf1 Hf2 89.9(3) . 9_655 ? O2 Hf1 Hf2 89.7(3) 2_655 9_655 ? O2 Hf1 Hf2 35.07(18) . 9_655 ? O6 Hf1 Hf2 111.16(16) 11_655 9_655 ? O6 Hf1 Hf2 111.02(15) 12 9_655 ? O6 Hf1 Hf2 75.47(12) 2_655 9_655 ? O6 Hf1 Hf2 166.06(12) . 9_655 ? Hf2 Hf1 Hf2 90.589(18) . 9_655 ? Hf2 Hf1 Hf2 60.486(17) 3 9_655 ? O1 Hf1 Hf2 34.98(18) 2_655 11_655 ? O1 Hf1 Hf2 89.9(3) . 11_655 ? O2 Hf1 Hf2 35.07(18) 2_655 11_655 ? O2 Hf1 Hf2 89.7(3) . 11_655 ? O6 Hf1 Hf2 75.47(12) 11_655 11_655 ? O6 Hf1 Hf2 166.06(12) 12 11_655 ? O6 Hf1 Hf2 111.16(16) 2_655 11_655 ? O6 Hf1 Hf2 111.02(15) . 11_655 ? Hf2 Hf1 Hf2 60.485(17) . 11_655 ? Hf2 Hf1 Hf2 90.590(17) 3 11_655 ? Hf2 Hf1 Hf2 60.194(18) 9_655 11_655 ? O2 Hf2 O2 68.2(5) 2_655 9_655 ? O2 Hf2 O1 108.2(5) 2_655 10 ? O2 Hf2 O1 71.1(4) 9_655 10 ? O2 Hf2 O1 71.1(4) 2_655 . ? O2 Hf2 O1 108.2(5) 9_655 . ? O1 Hf2 O1 69.2(4) 10 . ? O2 Hf2 O3 145.6(2) 2_655 . ? O2 Hf2 O3 145.6(2) 9_655 . ? O1 Hf2 O3 86.3(5) 10 . ? O1 Hf2 O3 86.3(5) . . ? O2 Hf2 O4 87.2(5) 2_655 . ? O2 Hf2 O4 87.2(5) 9_655 . ? O1 Hf2 O4 145.2(2) 10 . ? O1 Hf2 O4 145.2(2) . . ? O3 Hf2 O4 98.5(5) . . ? O2 Hf2 O5 140.1(3) 2_655 10 ? O2 Hf2 O5 76.5(3) 9_655 10 ? O1 Hf2 O5 75.7(3) 10 10 ? O1 Hf2 O5 140.1(2) . 10 ? O3 Hf2 O5 73.0(2) . 10 ? O4 Hf2 O5 72.97(19) . 10 ? O2 Hf2 O5 76.5(3) 2_655 . ? O2 Hf2 O5 140.1(3) 9_655 . ? O1 Hf2 O5 140.1(2) 10 . ? O1 Hf2 O5 75.7(3) . . ? O3 Hf2 O5 73.0(2) . . ? O4 Hf2 O5 72.97(19) . . ? O5 Hf2 O5 126.6(2) 10 . ? O2 Hf2 Hf1 35.8(3) 2_655 . ? O2 Hf2 Hf1 88.7(3) 9_655 . ? O1 Hf2 Hf1 89.0(3) 10 . ? O1 Hf2 Hf1 35.3(3) . . ? O3 Hf2 Hf1 117.2(2) . . ? O4 Hf2 Hf1 118.1(2) . . ? O5 Hf2 Hf1 161.38(12) 10 . ? O5 Hf2 Hf1 71.97(12) . . ? O2 Hf2 Hf1 88.7(3) 2_655 9_655 ? O2 Hf2 Hf1 35.8(3) 9_655 9_655 ? O1 Hf2 Hf1 35.3(3) 10 9_655 ? O1 Hf2 Hf1 89.0(3) . 9_655 ? O3 Hf2 Hf1 117.2(2) . 9_655 ? O4 Hf2 Hf1 118.1(2) . 9_655 ? O5 Hf2 Hf1 71.97(12) 10 9_655 ? O5 Hf2 Hf1 161.38(12) . 9_655 ? Hf1 Hf2 Hf1 89.412(18) . 9_655 ? O2 Hf2 Hf2 90.1(4) 2_655 3 ? O2 Hf2 Hf2 90.1(4) 9_655 3 ? O1 Hf2 Hf2 34.6(2) 10 3 ? O1 Hf2 Hf2 34.6(2) . 3 ? O3 Hf2 Hf2 84.9(4) . 3 ? O4 Hf2 Hf2 176.6(3) . 3 ? O5 Hf2 Hf2 108.20(14) 10 3 ? O5 Hf2 Hf2 108.20(14) . 3 ? Hf1 Hf2 Hf2 59.904(9) . 3 ? Hf1 Hf2 Hf2 59.904(9) 9_655 3 ? O2 Hf2 Hf2 34.1(2) 2_655 11_655 ? O2 Hf2 Hf2 34.1(2) 9_655 11_655 ? O1 Hf2 Hf2 89.5(4) 10 11_655 ? O1 Hf2 Hf2 89.5(4) . 11_655 ? O3 Hf2 Hf2 174.9(4) . 11_655 ? O4 Hf2 Hf2 86.6(3) . 11_655 ? O5 Hf2 Hf2 108.81(15) 10 11_655 ? O5 Hf2 Hf2 108.81(15) . 11_655 ? Hf1 Hf2 Hf2 59.758(8) . 11_655 ? Hf1 Hf2 Hf2 59.758(9) 9_655 11_655 ? Hf2 Hf2 Hf2 90.0 3 11_655 ? Hf2 O1 Hf2 110.8(4) . 3 ? Hf2 O1 Hf1 109.8(4) . . ? Hf2 O1 Hf1 109.8(4) 3 . ? Hf2 O2 Hf2 111.8(5) 3 9_655 ? Hf2 O2 Hf1 109.1(4) 3 . ? Hf2 O2 Hf1 109.1(4) 9_655 . ? C1 O5 Hf2 133.6(4) . . ? C1 O6 Hf1 131.3(4) . . ? O6 C1 O5 127.4(6) . . ? O6 C1 C2 116.5(6) . . ? O5 C1 C2 116.1(7) . . ? C4 C2 C3 119.6(7) . . ? C4 C2 C1 120.2(7) . . ? C3 C2 C1 120.1(7) . . ? C2 C3 C6 120.7(9) . 13 ? C2 C3 H3 119.6 . . ? C6 C3 H3 119.6 13 . ? C2 C4 C5 120.9(7) . . ? C2 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C5 119.8(10) . 13 ? C4 C5 C6 122.3(8) . . ? C5 C5 C6 117.9(9) 13 . ? C3 C6 C5 121.0(9) 13 . ? C3 C6 H6 119.5 13 . ? C5 C6 H6 119.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Hf1 Hf2 O2 -53.6(6) 2_655 . . 2_655 ? O1 Hf1 Hf2 O2 -177.7(8) . . . 2_655 ? O2 Hf1 Hf2 O2 -123.7(8) . . . 2_655 ? O6 Hf1 Hf2 O2 24.4(6) 11_655 . . 2_655 ? O6 Hf1 Hf2 O2 158.5(6) 12 . . 2_655 ? O6 Hf1 Hf2 O2 -89.9(9) 2_655 . . 2_655 ? O6 Hf1 Hf2 O2 91.1(6) . . . 2_655 ? Hf2 Hf1 Hf2 O2 -143.6(6) 3 . . 2_655 ? Hf2 Hf1 Hf2 O2 -88.6(6) 9_655 . . 2_655 ? Hf2 Hf1 Hf2 O2 -33.8(6) 11_655 . . 2_655 ? O1 Hf1 Hf2 O2 -0.8(3) 2_655 . . 9_655 ? O1 Hf1 Hf2 O2 -124.9(6) . . . 9_655 ? O2 Hf1 Hf2 O2 52.8(4) 2_655 . . 9_655 ? O2 Hf1 Hf2 O2 -70.9(4) . . . 9_655 ? O6 Hf1 Hf2 O2 77.2(3) 11_655 . . 9_655 ? O6 Hf1 Hf2 O2 -148.7(3) 12 . . 9_655 ? O6 Hf1 Hf2 O2 -37.1(8) 2_655 . . 9_655 ? O6 Hf1 Hf2 O2 143.9(3) . . . 9_655 ? Hf2 Hf1 Hf2 O2 -90.8(3) 3 . . 9_655 ? Hf2 Hf1 Hf2 O2 -35.8(3) 9_655 . . 9_655 ? Hf2 Hf1 Hf2 O2 18.9(3) 11_655 . . 9_655 ? O1 Hf1 Hf2 O1 70.2(4) 2_655 . . 10 ? O1 Hf1 Hf2 O1 -53.8(4) . . . 10 ? O2 Hf1 Hf2 O1 123.9(6) 2_655 . . 10 ? O2 Hf1 Hf2 O1 0.2(3) . . . 10 ? O6 Hf1 Hf2 O1 148.3(3) 11_655 . . 10 ? O6 Hf1 Hf2 O1 -77.6(3) 12 . . 10 ? O6 Hf1 Hf2 O1 34.0(8) 2_655 . . 10 ? O6 Hf1 Hf2 O1 -145.1(3) . . . 10 ? Hf2 Hf1 Hf2 O1 -19.7(3) 3 . . 10 ? Hf2 Hf1 Hf2 O1 35.3(3) 9_655 . . 10 ? Hf2 Hf1 Hf2 O1 90.0(3) 11_655 . . 10 ? O1 Hf1 Hf2 O1 124.0(7) 2_655 . . . ? O2 Hf1 Hf2 O1 177.7(8) 2_655 . . . ? O2 Hf1 Hf2 O1 54.0(6) . . . . ? O6 Hf1 Hf2 O1 -157.9(6) 11_655 . . . ? O6 Hf1 Hf2 O1 -23.8(6) 12 . . . ? O6 Hf1 Hf2 O1 87.8(9) 2_655 . . . ? O6 Hf1 Hf2 O1 -91.3(6) . . . . ? Hf2 Hf1 Hf2 O1 34.1(6) 3 . . . ? Hf2 Hf1 Hf2 O1 89.1(6) 9_655 . . . ? Hf2 Hf1 Hf2 O1 143.8(6) 11_655 . . . ? O1 Hf1 Hf2 O3 155.5(4) 2_655 . . . ? O1 Hf1 Hf2 O3 31.5(7) . . . . ? O2 Hf1 Hf2 O3 -150.9(7) 2_655 . . . ? O2 Hf1 Hf2 O3 85.5(4) . . . . ? O6 Hf1 Hf2 O3 -126.5(4) 11_655 . . . ? O6 Hf1 Hf2 O3 7.7(4) 12 . . . ? O6 Hf1 Hf2 O3 119.3(8) 2_655 . . . ? O6 Hf1 Hf2 O3 -59.8(4) . . . . ? Hf2 Hf1 Hf2 O3 65.5(3) 3 . . . ? Hf2 Hf1 Hf2 O3 120.5(3) 9_655 . . . ? Hf2 Hf1 Hf2 O3 175.3(3) 11_655 . . . ? O1 Hf1 Hf2 O4 -86.9(4) 2_655 . . . ? O1 Hf1 Hf2 O4 149.0(6) . . . . ? O2 Hf1 Hf2 O4 -33.3(7) 2_655 . . . ? O2 Hf1 Hf2 O4 -157.0(4) . . . . ? O6 Hf1 Hf2 O4 -8.9(3) 11_655 . . . ? O6 Hf1 Hf2 O4 125.2(3) 12 . . . ? O6 Hf1 Hf2 O4 -123.2(8) 2_655 . . . ? O6 Hf1 Hf2 O4 57.8(4) . . . . ? Hf2 Hf1 Hf2 O4 -176.9(3) 3 . . . ? Hf2 Hf1 Hf2 O4 -121.9(3) 9_655 . . . ? Hf2 Hf1 Hf2 O4 -67.1(3) 11_655 . . . ? O1 Hf1 Hf2 O5 36.1(5) 2_655 . . 10 ? O1 Hf1 Hf2 O5 -88.0(8) . . . 10 ? O2 Hf1 Hf2 O5 89.7(8) 2_655 . . 10 ? O2 Hf1 Hf2 O5 -34.0(5) . . . 10 ? O6 Hf1 Hf2 O5 114.1(5) 11_655 . . 10 ? O6 Hf1 Hf2 O5 -111.8(5) 12 . . 10 ? O6 Hf1 Hf2 O5 -0.2(9) 2_655 . . 10 ? O6 Hf1 Hf2 O5 -179.2(6) . . . 10 ? Hf2 Hf1 Hf2 O5 -53.9(5) 3 . . 10 ? Hf2 Hf1 Hf2 O5 1.1(5) 9_655 . . 10 ? Hf2 Hf1 Hf2 O5 55.9(5) 11_655 . . 10 ? O1 Hf1 Hf2 O5 -145.4(3) 2_655 . . . ? O1 Hf1 Hf2 O5 90.6(6) . . . . ? O2 Hf1 Hf2 O5 -91.8(6) 2_655 . . . ? O2 Hf1 Hf2 O5 144.6(3) . . . . ? O6 Hf1 Hf2 O5 -67.4(2) 11_655 . . . ? O6 Hf1 Hf2 O5 66.8(2) 12 . . . ? O6 Hf1 Hf2 O5 178.4(7) 2_655 . . . ? O6 Hf1 Hf2 O5 -0.7(2) . . . . ? Hf2 Hf1 Hf2 O5 124.64(17) 3 . . . ? Hf2 Hf1 Hf2 O5 179.63(17) 9_655 . . . ? Hf2 Hf1 Hf2 O5 -125.61(17) 11_655 . . . ? O1 Hf1 Hf2 Hf1 34.97(19) 2_655 . . 9_655 ? O1 Hf1 Hf2 Hf1 -89.1(6) . . . 9_655 ? O2 Hf1 Hf2 Hf1 88.6(6) 2_655 . . 9_655 ? O2 Hf1 Hf2 Hf1 -35.06(19) . . . 9_655 ? O6 Hf1 Hf2 Hf1 113.00(16) 11_655 . . 9_655 ? O6 Hf1 Hf2 Hf1 -112.87(16) 12 . . 9_655 ? O6 Hf1 Hf2 Hf1 -1.3(7) 2_655 . . 9_655 ? O6 Hf1 Hf2 Hf1 179.68(18) . . . 9_655 ? Hf2 Hf1 Hf2 Hf1 -54.993(12) 3 . . 9_655 ? Hf2 Hf1 Hf2 Hf1 0.0 9_655 . . 9_655 ? Hf2 Hf1 Hf2 Hf1 54.757(13) 11_655 . . 9_655 ? O1 Hf1 Hf2 Hf2 89.97(19) 2_655 . . 3 ? O1 Hf1 Hf2 Hf2 -34.1(6) . . . 3 ? O2 Hf1 Hf2 Hf2 143.6(6) 2_655 . . 3 ? O2 Hf1 Hf2 Hf2 19.94(19) . . . 3 ? O6 Hf1 Hf2 Hf2 167.99(16) 11_655 . . 3 ? O6 Hf1 Hf2 Hf2 -57.88(16) 12 . . 3 ? O6 Hf1 Hf2 Hf2 53.7(7) 2_655 . . 3 ? O6 Hf1 Hf2 Hf2 -125.33(18) . . . 3 ? Hf2 Hf1 Hf2 Hf2 54.993(12) 9_655 . . 3 ? Hf2 Hf1 Hf2 Hf2 109.751(8) 11_655 . . 3 ? O1 Hf1 Hf2 Hf2 -19.78(19) 2_655 . . 11_655 ? O1 Hf1 Hf2 Hf2 -143.8(6) . . . 11_655 ? O2 Hf1 Hf2 Hf2 33.8(6) 2_655 . . 11_655 ? O2 Hf1 Hf2 Hf2 -89.81(19) . . . 11_655 ? O6 Hf1 Hf2 Hf2 58.24(16) 11_655 . . 11_655 ? O6 Hf1 Hf2 Hf2 -167.63(16) 12 . . 11_655 ? O6 Hf1 Hf2 Hf2 -56.0(7) 2_655 . . 11_655 ? O6 Hf1 Hf2 Hf2 124.92(18) . . . 11_655 ? Hf2 Hf1 Hf2 Hf2 -109.751(8) 3 . . 11_655 ? Hf2 Hf1 Hf2 Hf2 -54.758(12) 9_655 . . 11_655 ? O2 Hf2 O1 Hf2 -119.9(7) 2_655 . . 3 ? O2 Hf2 O1 Hf2 -61.7(6) 9_655 . . 3 ? O1 Hf2 O1 Hf2 -1.1(8) 10 . . 3 ? O3 Hf2 O1 Hf2 86.4(6) . . . 3 ? O4 Hf2 O1 Hf2 -174.1(6) . . . 3 ? O5 Hf2 O1 Hf2 28.8(10) 10 . . 3 ? O5 Hf2 O1 Hf2 159.7(6) . . . 3 ? Hf1 Hf2 O1 Hf2 -121.4(10) . . . 3 ? Hf1 Hf2 O1 Hf2 -31.0(5) 9_655 . . 3 ? Hf2 Hf2 O1 Hf2 -90.7(5) 11_655 . . 3 ? O2 Hf2 O1 Hf1 1.4(5) 2_655 . . . ? O2 Hf2 O1 Hf1 59.7(5) 9_655 . . . ? O1 Hf2 O1 Hf1 120.3(3) 10 . . . ? O3 Hf2 O1 Hf1 -152.3(5) . . . . ? O4 Hf2 O1 Hf1 -52.7(11) . . . . ? O5 Hf2 O1 Hf1 150.2(2) 10 . . . ? O5 Hf2 O1 Hf1 -78.9(4) . . . . ? Hf1 Hf2 O1 Hf1 90.4(5) 9_655 . . . ? Hf2 Hf2 O1 Hf1 121.4(10) 3 . . . ? Hf2 Hf2 O1 Hf1 30.7(5) 11_655 . . . ? O1 Hf1 O1 Hf2 -61.0(5) 2_655 . . . ? O2 Hf1 O1 Hf2 -1.4(5) 2_655 . . . ? O2 Hf1 O1 Hf2 -120.6(7) . . . . ? O6 Hf1 O1 Hf2 34.9(10) 11_655 . . . ? O6 Hf1 O1 Hf2 157.4(5) 12 . . . ? O6 Hf1 O1 Hf2 -156.9(2) 2_655 . . . ? O6 Hf1 O1 Hf2 80.5(5) . . . . ? Hf2 Hf1 O1 Hf2 -122.0(9) 3 . . . ? Hf2 Hf1 O1 Hf2 -91.1(5) 9_655 . . . ? Hf2 Hf1 O1 Hf2 -30.9(5) 11_655 . . . ? O1 Hf1 O1 Hf2 61.0(5) 2_655 . . 3 ? O2 Hf1 O1 Hf2 120.6(7) 2_655 . . 3 ? O2 Hf1 O1 Hf2 1.4(5) . . . 3 ? O6 Hf1 O1 Hf2 156.9(2) 11_655 . . 3 ? O6 Hf1 O1 Hf2 -80.5(5) 12 . . 3 ? O6 Hf1 O1 Hf2 -34.9(10) 2_655 . . 3 ? O6 Hf1 O1 Hf2 -157.4(5) . . . 3 ? Hf2 Hf1 O1 Hf2 122.0(9) . . . 3 ? Hf2 Hf1 O1 Hf2 30.9(5) 9_655 . . 3 ? Hf2 Hf1 O1 Hf2 91.1(5) 11_655 . . 3 ? O1 Hf1 O2 Hf2 -121.1(7) 2_655 . . 3 ? O1 Hf1 O2 Hf2 -1.4(5) . . . 3 ? O2 Hf1 O2 Hf2 -61.2(5) 2_655 . . 3 ? O6 Hf1 O2 Hf2 -156.6(2) 11_655 . . 3 ? O6 Hf1 O2 Hf2 80.7(5) 12 . . 3 ? O6 Hf1 O2 Hf2 156.9(5) 2_655 . . 3 ? O6 Hf1 O2 Hf2 34.2(10) . . . 3 ? Hf2 Hf1 O2 Hf2 -31.0(5) . . . 3 ? Hf2 Hf1 O2 Hf2 -122.5(9) 9_655 . . 3 ? Hf2 Hf1 O2 Hf2 -91.5(5) 11_655 . . 3 ? O1 Hf1 O2 Hf2 1.4(5) 2_655 . . 9_655 ? O1 Hf1 O2 Hf2 121.1(7) . . . 9_655 ? O2 Hf1 O2 Hf2 61.2(5) 2_655 . . 9_655 ? O6 Hf1 O2 Hf2 -34.2(10) 11_655 . . 9_655 ? O6 Hf1 O2 Hf2 -156.9(5) 12 . . 9_655 ? O6 Hf1 O2 Hf2 -80.7(5) 2_655 . . 9_655 ? O6 Hf1 O2 Hf2 156.6(2) . . . 9_655 ? Hf2 Hf1 O2 Hf2 91.5(5) . . . 9_655 ? Hf2 Hf1 O2 Hf2 122.5(9) 3 . . 9_655 ? Hf2 Hf1 O2 Hf2 31.0(5) 11_655 . . 9_655 ? O2 Hf2 O5 C1 -33.1(9) 2_655 . . . ? O2 Hf2 O5 C1 -60.9(11) 9_655 . . . ? O1 Hf2 O5 C1 69.1(11) 10 . . . ? O1 Hf2 O5 C1 40.4(9) . . . . ? O3 Hf2 O5 C1 130.9(9) . . . . ? O4 Hf2 O5 C1 -124.3(9) . . . . ? O5 Hf2 O5 C1 -176.7(6) 10 . . . ? Hf1 Hf2 O5 C1 3.9(8) . . . . ? Hf1 Hf2 O5 C1 5.0(12) 9_655 . . . ? Hf2 Hf2 O5 C1 52.4(9) 3 . . . ? Hf2 Hf2 O5 C1 -44.0(9) 11_655 . . . ? O1 Hf1 O6 C1 68.6(11) 2_655 . . . ? O1 Hf1 O6 C1 -37.6(9) . . . . ? O2 Hf1 O6 C1 34.0(9) 2_655 . . . ? O2 Hf1 O6 C1 -71.5(11) . . . . ? O6 Hf1 O6 C1 115.3(8) 11_655 . . . ? O6 Hf1 O6 C1 -118.8(8) 12 . . . ? O6 Hf1 O6 C1 178.4(9) 2_655 . . . ? Hf2 Hf1 O6 C1 -1.8(8) . . . . ? Hf2 Hf1 O6 C1 -51.2(9) 3 . . . ? Hf2 Hf1 O6 C1 -0.5(14) 9_655 . . . ? Hf2 Hf1 O6 C1 48.0(9) 11_655 . . . ? Hf1 O6 C1 O5 5.4(16) . . . . ? Hf1 O6 C1 C2 -176.0(6) . . . . ? Hf2 O5 C1 O6 -6.9(16) . . . . ? Hf2 O5 C1 C2 174.4(6) . . . . ? O6 C1 C2 C4 -177.2(11) . . . . ? O5 C1 C2 C4 1.6(16) . . . . ? O6 C1 C2 C3 2.6(17) . . . . ? O5 C1 C2 C3 -178.6(12) . . . . ? C4 C2 C3 C6 -1(3) . . . 13 ? C1 C2 C3 C6 179.4(15) . . . 13 ? C3 C2 C4 C5 0(2) . . . . ? C1 C2 C4 C5 -179.8(12) . . . . ? C2 C4 C5 C5 1(2) . . . 13 ? C2 C4 C5 C6 178.9(15) . . . . ? C4 C5 C6 C3 -179.6(16) . . . 13 ? C5 C5 C6 C3 -2(3) 13 . . 13 ? _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 36.99 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 3.602 _refine_diff_density_min -2.906 _refine_diff_density_rms 0.298 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 -0.024 -0.024 -0.006 4950 1471 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 937878' ####################################################################### # # 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_DUT-53(Hf)_i4mmm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H24 Hf6 O32' _chemical_formula_weight 1091.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0060 0.0030 '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' Hf Hf -1.6680 8.8820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4/mmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x, -y, -z' 'y, x, -z' '-x, y, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x, y, z' '-y, -x, z' 'x, -y, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 17.600(2) _cell_length_b 17.600(2) _cell_length_c 22.600(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7000.6(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2534 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 32.85 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 7.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8590 _exptl_absorpt_correction_T_max 0.8590 _exptl_absorpt_process_details Scala _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.88561 _diffrn_source synchrotron _diffrn_source_type 'BESSY BL MX-14.2' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'MX-225 CCD' _diffrn_measurement_method '\D\f scans' _diffrn_reflns_number 3131 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.1165 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 1 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 4.56 _diffrn_reflns_theta_max 34.18 _reflns_number_total 1830 _reflns_number_gt 1708 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marCCD 1994-2002' _computing_cell_refinement 'mosflm 1.0.5' _computing_data_reduction scala _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material WinGX _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^)+(0.0378P)^2^+49.4719P] 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 1830 _refine_ls_number_parameters 60 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1642 _refine_ls_wR_factor_gt 0.1624 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _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 0.0000 0.39173(3) 0.0180(3) Uani 1 8 d S . . Hf2 Hf 0.099763(19) 0.099763(19) 0.5000 0.0323(3) Uani 1 4 d S . . O1 O 0.0753(2) 0.0753(2) 0.3424(3) 0.0327(11) Uani 1 2 d S . . O2 O 0.1390(3) 0.1390(3) 0.4114(3) 0.064(3) Uani 1 2 d S . . O3 O 0.0000 0.1004(6) 0.4476(3) 0.069(4) Uani 1 2 d S . . O4 O 0.2237(4) 0.0955(6) 0.5000 0.073(3) Uani 1 2 d S . . C1 C 0.1225(3) 0.1225(3) 0.3576(4) 0.0327(11) Uani 1 2 d S . . C2 C 0.1649(4) 0.1649(4) 0.3105(5) 0.065(3) Uani 1 2 d S . . C3 C 0.1505(5) 0.1505(5) 0.2514(6) 0.112(9) Uani 1 2 d S . . H3 H 0.1142 0.1142 0.2416 0.135 Uiso 1 2 calc SR . . C4 C 0.1881(6) 0.1881(6) 0.2064(6) 0.138(12) Uani 1 2 d S . . H4 H 0.1769 0.1769 0.1672 0.165 Uiso 1 2 calc SR . . C5 C 0.2428(4) 0.2428(4) 0.2197(5) 0.079(5) Uani 1 2 d S . . C6 C 0.2194(4) 0.2194(4) 0.3240(5) 0.065(3) Uani 1 2 d S . . H6 H 0.2302 0.2302 0.3634 0.078 Uiso 1 2 calc SR . . 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 0.0207(3) 0.0207(3) 0.0126(4) 0.000 0.000 0.000 Hf2 0.0401(3) 0.0401(3) 0.0168(4) 0.000 0.000 -0.0214(2) O1 0.0416(17) 0.0416(17) 0.015(3) 0.0075(13) 0.0075(13) -0.020(2) O2 0.081(4) 0.081(4) 0.029(4) 0.007(2) 0.007(2) -0.059(5) O3 0.043(4) 0.131(9) 0.034(6) -0.048(5) 0.000 0.000 O4 0.022(3) 0.141(9) 0.056(6) 0.000 0.000 -0.040(4) C1 0.0416(17) 0.0416(17) 0.015(3) 0.0075(13) 0.0075(13) -0.020(2) C2 0.089(4) 0.089(4) 0.017(4) 0.0068(19) 0.0068(19) -0.064(5) C3 0.157(14) 0.157(14) 0.024(7) 0.000(3) 0.000(3) -0.138(15) C4 0.193(19) 0.193(19) 0.027(8) -0.003(4) -0.003(4) -0.16(2) C5 0.101(8) 0.101(8) 0.034(6) -0.004(3) -0.004(3) -0.091(9) C6 0.089(4) 0.089(4) 0.017(4) 0.0068(19) 0.0068(19) -0.064(5) _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 O3 2.172(8) . ? Hf1 O3 2.172(8) 4 ? Hf1 O3 2.172(8) 2 ? Hf1 O3 2.172(8) 3 ? Hf1 O1 2.181(5) . ? Hf1 O1 2.181(5) 3 ? Hf1 O1 2.181(5) 4 ? Hf1 O1 2.181(5) 2 ? Hf2 O3 2.118(4) . ? Hf2 O3 2.118(4) 4 ? Hf2 O3 2.118(4) 18_556 ? Hf2 O3 2.118(4) 19_556 ? Hf2 O4 2.182(7) . ? Hf2 O4 2.182(7) 6_556 ? Hf2 O2 2.229(7) 19_556 ? Hf2 O2 2.229(7) . ? Hf2 Hf1 3.4861(6) 17_556 ? O1 C1 1.224(12) . ? O2 C1 1.283(12) . ? O3 Hf2 2.118(4) 2 ? C1 C2 1.499(12) . ? C2 C3 1.383(17) . ? C2 C6 1.389(15) . ? C3 C4 1.382(19) . ? C3 H3 0.9300 . ? C4 C5 1.395(17) . ? C4 H4 0.9300 . ? C5 C6 1.364(15) 25 ? C5 C5 1.41(2) 25 ? C6 C5 1.364(15) 25 ? C6 H6 0.9300 . ? 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 O3 Hf1 O3 70.3(3) . 4 ? O3 Hf1 O3 70.3(3) . 2 ? O3 Hf1 O3 109.0(5) 4 2 ? O3 Hf1 O3 109.0(5) . 3 ? O3 Hf1 O3 70.3(3) 4 3 ? O3 Hf1 O3 70.3(3) 2 3 ? O3 Hf1 O1 78.6(2) . . ? O3 Hf1 O1 78.6(2) 4 . ? O3 Hf1 O1 142.34(6) 2 . ? O3 Hf1 O1 142.34(6) 3 . ? O3 Hf1 O1 142.34(6) . 3 ? O3 Hf1 O1 142.34(6) 4 3 ? O3 Hf1 O1 78.6(2) 2 3 ? O3 Hf1 O1 78.6(2) 3 3 ? O1 Hf1 O1 118.5(3) . 3 ? O3 Hf1 O1 142.34(6) . 4 ? O3 Hf1 O1 78.6(2) 4 4 ? O3 Hf1 O1 142.34(6) 2 4 ? O3 Hf1 O1 78.6(2) 3 4 ? O1 Hf1 O1 74.86(15) . 4 ? O1 Hf1 O1 74.86(15) 3 4 ? O3 Hf1 O1 78.6(2) . 2 ? O3 Hf1 O1 142.34(6) 4 2 ? O3 Hf1 O1 78.6(2) 2 2 ? O3 Hf1 O1 142.34(6) 3 2 ? O1 Hf1 O1 74.86(15) . 2 ? O1 Hf1 O1 74.86(15) 3 2 ? O1 Hf1 O1 118.5(3) 4 2 ? O3 Hf2 O3 72.3(5) . 4 ? O3 Hf2 O3 108.8(6) . 18_556 ? O3 Hf2 O3 68.0(3) 4 18_556 ? O3 Hf2 O3 68.0(3) . 19_556 ? O3 Hf2 O3 108.8(6) 4 19_556 ? O3 Hf2 O3 72.3(5) 18_556 19_556 ? O3 Hf2 O4 145.95(16) . . ? O3 Hf2 O4 88.1(4) 4 . ? O3 Hf2 O4 88.1(4) 18_556 . ? O3 Hf2 O4 145.95(16) 19_556 . ? O3 Hf2 O4 88.1(4) . 6_556 ? O3 Hf2 O4 145.95(16) 4 6_556 ? O3 Hf2 O4 145.95(16) 18_556 6_556 ? O3 Hf2 O4 88.1(4) 19_556 6_556 ? O4 Hf2 O4 93.9(6) . 6_556 ? O3 Hf2 O2 139.29(18) . 19_556 ? O3 Hf2 O2 139.29(18) 4 19_556 ? O3 Hf2 O2 75.7(3) 18_556 19_556 ? O3 Hf2 O2 75.7(3) 19_556 19_556 ? O4 Hf2 O2 72.59(16) . 19_556 ? O4 Hf2 O2 72.59(16) 6_556 19_556 ? O3 Hf2 O2 75.7(3) . . ? O3 Hf2 O2 75.7(3) 4 . ? O3 Hf2 O2 139.29(18) 18_556 . ? O3 Hf2 O2 139.29(18) 19_556 . ? O4 Hf2 O2 72.59(16) . . ? O4 Hf2 O2 72.59(16) 6_556 . ? O2 Hf2 O2 128.0(4) 19_556 . ? O3 Hf2 Hf1 88.7(2) . 17_556 ? O3 Hf2 Hf1 88.7(2) 4 17_556 ? O3 Hf2 Hf1 36.2(2) 18_556 17_556 ? O3 Hf2 Hf1 36.2(2) 19_556 17_556 ? O4 Hf2 Hf1 119.09(18) . 17_556 ? O4 Hf2 Hf1 119.09(18) 6_556 17_556 ? O2 Hf2 Hf1 71.42(19) 19_556 17_556 ? O2 Hf2 Hf1 160.58(19) . 17_556 ? C1 O1 Hf1 133.0(6) . . ? C1 O2 Hf2 135.3(6) . . ? Hf2 O3 Hf2 112.0(3) . 2 ? Hf2 O3 Hf1 108.7(3) . . ? Hf2 O3 Hf1 108.7(3) 2 . ? O1 C1 O2 124.9(7) . . ? O1 C1 C2 118.5(8) . . ? O2 C1 C2 116.5(8) . . ? C3 C2 C6 117.7(9) . . ? C3 C2 C1 120.1(10) . . ? C6 C2 C1 122.1(9) . . ? C2 C3 C4 122.3(11) . . ? C2 C3 H3 118.9 . . ? C4 C3 H3 118.9 . . ? C3 C4 C5 120.2(12) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 121.2(12) 25 . ? C6 C5 C5 121.8(12) 25 25 ? C4 C5 C5 117.1(14) . 25 ? C5 C6 C2 120.9(10) 25 . ? C5 C6 H6 119.5 25 . ? C2 C6 H6 119.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Hf1 O1 C1 35.95(17) . . . . ? O3 Hf1 O1 C1 -35.95(17) 4 . . . ? O3 Hf1 O1 C1 70.4(5) 2 . . . ? O3 Hf1 O1 C1 -70.4(5) 3 . . . ? O1 Hf1 O1 C1 180.0 3 . . . ? O1 Hf1 O1 C1 -117.07(11) 4 . . . ? O1 Hf1 O1 C1 117.07(11) 2 . . . ? O3 Hf2 O2 C1 -37.5(3) . . . . ? O3 Hf2 O2 C1 37.5(3) 4 . . . ? O3 Hf2 O2 C1 64.8(5) 18_556 . . . ? O3 Hf2 O2 C1 -64.8(5) 19_556 . . . ? O4 Hf2 O2 C1 130.0(3) . . . . ? O4 Hf2 O2 C1 -130.0(3) 6_556 . . . ? O2 Hf2 O2 C1 180.0 19_556 . . . ? Hf1 Hf2 O2 C1 0.0 17_556 . . . ? O3 Hf2 O3 Hf2 118.9(3) 4 . . 2 ? O3 Hf2 O3 Hf2 60.4(4) 18_556 . . 2 ? O3 Hf2 O3 Hf2 -0.7(6) 19_556 . . 2 ? O4 Hf2 O3 Hf2 176.5(5) . . . 2 ? O4 Hf2 O3 Hf2 -89.4(5) 6_556 . . 2 ? O2 Hf2 O3 Hf2 -29.3(8) 19_556 . . 2 ? O2 Hf2 O3 Hf2 -161.9(5) . . . 2 ? Hf1 Hf2 O3 Hf2 29.8(4) 17_556 . . 2 ? O3 Hf2 O3 Hf1 -1.2(5) 4 . . . ? O3 Hf2 O3 Hf1 -59.7(3) 18_556 . . . ? O3 Hf2 O3 Hf1 -120.8(2) 19_556 . . . ? O4 Hf2 O3 Hf1 56.4(9) . . . . ? O4 Hf2 O3 Hf1 150.5(4) 6_556 . . . ? O2 Hf2 O3 Hf1 -149.4(3) 19_556 . . . ? O2 Hf2 O3 Hf1 78.0(3) . . . . ? Hf1 Hf2 O3 Hf1 -90.3(3) 17_556 . . . ? O3 Hf1 O3 Hf2 1.2(5) 4 . . . ? O3 Hf1 O3 Hf2 120.89(17) 2 . . . ? O3 Hf1 O3 Hf2 61.0(3) 3 . . . ? O1 Hf1 O3 Hf2 -80.6(3) . . . . ? O1 Hf1 O3 Hf2 157.0(3) 3 . . . ? O1 Hf1 O3 Hf2 -34.9(7) 4 . . . ? O1 Hf1 O3 Hf2 -157.3(4) 2 . . . ? O3 Hf1 O3 Hf2 -120.89(17) 4 . . 2 ? O3 Hf1 O3 Hf2 -1.2(5) 2 . . 2 ? O3 Hf1 O3 Hf2 -61.0(3) 3 . . 2 ? O1 Hf1 O3 Hf2 157.3(4) . . . 2 ? O1 Hf1 O3 Hf2 34.9(7) 3 . . 2 ? O1 Hf1 O3 Hf2 -157.0(3) 4 . . 2 ? O1 Hf1 O3 Hf2 80.6(3) 2 . . 2 ? Hf1 O1 C1 O2 0.0 . . . . ? Hf1 O1 C1 C2 180.0 . . . . ? Hf2 O2 C1 O1 0.0 . . . . ? Hf2 O2 C1 C2 180.0 . . . . ? O1 C1 C2 C3 0.0 . . . . ? O2 C1 C2 C3 180.0 . . . . ? O1 C1 C2 C6 180.0 . . . . ? O2 C1 C2 C6 0.0 . . . . ? C6 C2 C3 C4 0.0 . . . . ? C1 C2 C3 C4 180.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 180.0 . . . 25 ? C3 C4 C5 C5 0.0 . . . 25 ? C3 C2 C6 C5 0.0 . . . 25 ? C1 C2 C6 C5 180.0 . . . 25 ? _diffrn_measured_fraction_theta_max 0.850 _diffrn_reflns_theta_full 34.18 _diffrn_measured_fraction_theta_full 0.850 _refine_diff_density_max 1.662 _refine_diff_density_min -2.606 _refine_diff_density_rms 0.157 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 -0.026 -0.014 -0.005 4874 664 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 937879' ####################################################################### # # 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_cmma-sr _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H24 O32 Zr6' _chemical_formula_weight 1563.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0060 0.0030 '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' O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -1.2060 0.8400 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 22.530(5) _cell_length_b 25.380(5) _cell_length_c 16.900(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9664(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 624 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 25.45 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 1.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9421 _exptl_absorpt_correction_T_max 0.9880 _exptl_absorpt_process_details XDS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.88561 _diffrn_source synchrotron _diffrn_source_type 'BESSY BL MX-14.2' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'MX-225 CCD' _diffrn_measurement_method '\D\f scans' _diffrn_reflns_number 12363 _diffrn_reflns_av_R_equivalents 0.1478 _diffrn_reflns_av_sigmaI/netI 0.1426 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 30.14 _reflns_number_total 2979 _reflns_number_gt 1749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marCCD 1994-2002' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3.1' _computing_publication_material WinGX _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2979 _refine_ls_number_parameters 223 _refine_ls_number_restraints 94 _refine_ls_R_factor_all 0.1512 _refine_ls_R_factor_gt 0.1230 _refine_ls_wR_factor_ref 0.3232 _refine_ls_wR_factor_gt 0.3064 _refine_ls_goodness_of_fit_ref 1.527 _refine_ls_restrained_S_all 1.525 _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 Zr1 Zr 0.0000 0.34822(13) 0.12318(13) 0.0275(8) Uani 0.72 2 d SP . . Zr2 Zr 0.0000 0.2500 -0.02406(13) 0.0242(9) Uani 0.72 4 d SP . . Zr3 Zr 0.11012(7) 0.2500 0.12415(10) 0.0243(7) Uani 0.72 2 d SP . . Zr4 Zr 0.0000 0.2500 0.27235(14) 0.0328(11) Uani 0.72 4 d SP . . O1 O 0.0547(5) 0.2993(7) 0.1981(6) 0.128(7) Uani 1 1 d . . . O2 O 0.0516(5) 0.2985(6) 0.0509(6) 0.120(6) Uani 1 1 d . . . O3 O 0.1601(5) 0.2500 0.2380(6) 0.076(5) Uani 1 2 d S . . O4 O 0.0932(6) 0.2500 0.3284(7) 0.078(5) Uani 1 2 d S . . O5 O 0.1578(4) 0.3269(5) 0.1252(4) 0.070(3) Uani 1 1 d . . . O6 O 0.0906(4) 0.3892(5) 0.1228(5) 0.083(3) Uani 1 1 d . . . O7 O 0.1610(4) 0.2500 0.0155(6) 0.063(4) Uani 1 2 d S . . O8 O 0.0000 0.4038(10) 0.0190(8) 0.129(9) Uani 1 2 d S . . O9 O 0.0000 0.3118(8) 0.3543(6) 0.088(6) Uani 1 2 d S . . O10 O 0.0000 0.4079(8) 0.2224(6) 0.099(7) Uani 1 2 d S . . O11 O -0.0917(6) 0.2500 -0.0822(8) 0.196(15) Uani 1 2 d S . . O12 O 0.0000 0.3077(11) -0.1143(7) 0.131(9) Uani 1 2 d S . . C1 C 0.1464(8) 0.2500 0.3063(9) 0.083(6) Uani 1 2 d SU . . C2 C 0.1915(8) 0.2500 0.3708(9) 0.086(5) Uani 1 2 d SU . . C3 C 0.2522(8) 0.2500 0.3491(11) 0.096(5) Uani 1 2 d SU . . H3 H 0.2634 0.2500 0.2961 0.115 Uiso 1 2 calc SR . . C4 C 0.2935(8) 0.2500 0.4071(11) 0.096(6) Uani 1 2 d SU . . H4 H 0.3332 0.2500 0.3921 0.115 Uiso 1 2 calc SR . . C5 C 0.1759(8) 0.2500 0.4524(10) 0.096(5) Uani 1 2 d SU . . H5 H 0.1361 0.2500 0.4668 0.115 Uiso 1 2 calc SR . . C6 C 0.2193(7) 0.2500 0.5108(10) 0.095(6) Uani 1 2 d SU . . C7 C 0.1427(6) 0.3758(7) 0.1229(8) 0.065(3) Uani 1 1 d U . . C8 C 0.1897(7) 0.4148(8) 0.1186(9) 0.083(3) Uani 1 1 d U . . C9 C 0.1745(7) 0.4683(8) 0.1144(9) 0.089(3) Uani 1 1 d U . . H9 H 0.1348 0.4782 0.1115 0.106 Uiso 1 1 calc R . . C10 C 0.2204(7) 0.5081(8) 0.1147(10) 0.087(4) Uani 1 1 d U . . C11 C 0.2488(7) 0.3991(10) 0.1141(9) 0.111(4) Uani 1 1 d U . . H11 H 0.2582 0.3635 0.1155 0.133 Uiso 1 1 calc R . . C12 C 0.2952(8) 0.4376(11) 0.1074(12) 0.122(5) Uani 1 1 d U . . H12 H 0.3344 0.4274 0.0986 0.146 Uiso 1 1 calc R . . C13 C 0.1433(8) 0.2500 -0.0581(10) 0.101(9) Uani 1 2 d SU . . C14 C 0.1931(10) 0.2500 -0.1217(11) 0.112(9) Uani 1 2 d SU . . H14A H 0.1833 0.2253 -0.1627 0.168 Uiso 0.50 1 calc PR . . H14B H 0.2301 0.2401 -0.0976 0.168 Uiso 0.50 1 calc PR . . H14C H 0.1967 0.2846 -0.1440 0.168 Uiso 0.50 1 calc PR . . Zr2B Zr 0.0000 0.2795(5) -0.0248(5) 0.0242(9) Uani 0.14 2 d SP . . Zr4B Zr 0.0000 0.2802(6) 0.2750(5) 0.0328(11) Uani 0.14 2 d SP . . Zr3B Zr 0.1103(3) 0.2792(3) 0.1260(4) 0.0243(7) Uani 0.14 1 d P . . Zr1A Zr 0.0000 0.3187(5) 0.1231(8) 0.0275(8) Uani 0.14 2 d SPU . . Zr1B Zr 0.0000 0.3761(6) 0.1276(9) 0.027(2) Uani 0.14 2 d SPU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0095(11) 0.028(2) 0.0455(11) -0.006(2) 0.000 0.000 Zr2 0.0107(15) 0.026(2) 0.0357(12) 0.000 0.000 0.000 Zr3 0.0058(11) 0.0265(16) 0.0405(10) 0.000 -0.0006(5) 0.000 Zr4 0.0126(15) 0.056(3) 0.0300(12) 0.000 0.000 0.000 O1 0.065(9) 0.23(2) 0.090(8) 0.053(8) 0.024(5) 0.039(9) O2 0.059(8) 0.218(19) 0.083(7) -0.052(8) -0.030(5) 0.056(8) O3 0.020(7) 0.175(18) 0.035(6) 0.000 0.001(4) 0.000 O4 0.060(10) 0.111(16) 0.062(8) 0.000 -0.023(6) 0.000 O5 0.027(5) 0.131(12) 0.051(5) 0.005(5) 0.004(3) -0.021(6) O6 0.019(6) 0.090(11) 0.139(9) -0.005(6) -0.013(4) 0.001(5) O7 0.010(6) 0.116(15) 0.065(7) 0.000 0.003(5) 0.000 O8 0.020(9) 0.29(3) 0.079(9) -0.030(11) 0.000 0.000 O9 0.061(9) 0.17(2) 0.030(6) -0.007(7) 0.000 0.000 O10 0.033(8) 0.21(2) 0.053(7) 0.024(9) 0.000 0.000 O11 0.007(9) 0.53(5) 0.050(8) 0.000 -0.009(6) 0.000 O12 0.115(15) 0.22(3) 0.053(9) -0.021(10) 0.000 0.000 C1 0.017(7) 0.195(18) 0.038(7) 0.000 0.000(6) 0.000 C2 0.012(6) 0.200(16) 0.047(5) 0.000 -0.009(4) 0.000 C3 0.019(6) 0.209(17) 0.060(7) 0.000 -0.002(5) 0.000 C4 0.007(7) 0.216(19) 0.063(8) 0.000 0.002(6) 0.000 C5 0.031(7) 0.207(17) 0.049(6) 0.000 -0.010(5) 0.000 C6 0.036(8) 0.204(19) 0.046(7) 0.000 -0.013(6) 0.000 C7 0.023(7) 0.048(8) 0.124(9) -0.005(7) 0.009(6) 0.009(5) C8 0.028(5) 0.065(7) 0.157(8) -0.007(6) 0.004(5) -0.008(5) C9 0.035(6) 0.066(8) 0.165(9) -0.007(7) 0.004(6) -0.011(5) C10 0.041(7) 0.063(9) 0.158(10) -0.002(8) 0.007(6) -0.010(6) C11 0.039(6) 0.089(10) 0.204(10) -0.002(8) -0.004(7) -0.001(6) C12 0.038(8) 0.100(12) 0.226(12) -0.006(10) -0.004(8) -0.006(7) C13 0.019(12) 0.23(3) 0.051(10) 0.000 0.023(7) 0.000 C14 0.035(12) 0.24(3) 0.062(11) 0.000 0.028(7) 0.000 Zr2B 0.0107(15) 0.026(2) 0.0357(12) 0.000 0.000 0.000 Zr4B 0.0126(15) 0.056(3) 0.0300(12) 0.000 0.000 0.000 Zr3B 0.0058(11) 0.0265(16) 0.0405(10) 0.000 -0.0006(5) 0.000 Zr1A 0.0095(11) 0.028(2) 0.0455(11) -0.006(2) 0.000 0.000 Zr1B 0.013(4) 0.033(4) 0.034(4) -0.017(5) 0.000 0.000 _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 Zr1 O2 2.106(10) 12 ? Zr1 O2 2.106(10) . ? Zr1 O1 2.160(11) 12 ? Zr1 O1 2.160(11) . ? Zr1 O8 2.26(2) . ? Zr1 O10 2.259(18) . ? Zr1 O6 2.291(11) . ? Zr1 O6 2.291(11) 12 ? Zr2 O12 2.11(2) . ? Zr2 O12 2.11(2) 2 ? Zr2 O2 2.115(12) . ? Zr2 O2 2.115(12) 12 ? Zr2 O2 2.115(12) 2 ? Zr2 O2 2.115(12) 11_565 ? Zr2 O11 2.287(13) 2 ? Zr2 O11 2.287(13) . ? Zr3 O1 2.164(12) . ? Zr3 O1 2.164(12) 11_565 ? Zr3 O7 2.164(10) . ? Zr3 O2 2.188(11) 11_565 ? Zr3 O2 2.188(11) . ? Zr3 O5 2.229(12) 11_565 ? Zr3 O5 2.229(12) . ? Zr3 O3 2.230(10) . ? Zr4 O9 2.092(16) 2 ? Zr4 O9 2.092(16) . ? Zr4 O1 2.159(12) 2 ? Zr4 O1 2.159(12) 12 ? Zr4 O1 2.159(12) 11_565 ? Zr4 O1 2.159(12) . ? Zr4 O4 2.304(12) 2 ? Zr4 O4 2.304(12) . ? O3 C1 1.195(18) . ? O4 C1 1.255(19) . ? O5 C7 1.287(19) . ? O6 C7 1.221(17) . ? O7 C13 1.31(2) . ? O11 C13 1.23(2) 2 ? C1 C2 1.49(2) . ? C2 C3 1.42(3) . ? C2 C5 1.42(2) . ? C3 C4 1.35(2) . ? C3 H3 0.9300 . ? C4 C6 1.42(2) 13_556 ? C4 H4 0.9300 . ? C5 C6 1.39(2) . ? C5 H5 0.9300 . ? C6 C4 1.42(2) 13_556 ? C6 C6 1.43(3) 13_556 ? C7 C8 1.45(2) . ? C8 C11 1.39(2) . ? C8 C9 1.40(3) . ? C9 C10 1.45(2) . ? C9 H9 0.9300 . ? C10 C10 1.39(3) 6 ? C10 C12 1.43(3) 6 ? C11 C12 1.44(3) . ? C11 H11 0.9300 . ? C12 C10 1.43(3) 6 ? C12 H12 0.9300 . ? C13 O11 1.23(2) 2 ? C13 C14 1.55(2) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? 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 O2 Zr1 O2 67.0(6) 12 . ? O2 Zr1 O1 71.3(5) 12 12 ? O2 Zr1 O1 108.1(7) . 12 ? O2 Zr1 O1 108.1(7) 12 . ? O2 Zr1 O1 71.3(5) . . ? O1 Zr1 O1 69.6(6) 12 . ? O2 Zr1 O8 85.5(6) 12 . ? O2 Zr1 O8 85.5(6) . . ? O1 Zr1 O8 144.8(3) 12 . ? O1 Zr1 O8 144.8(3) . . ? O2 Zr1 O10 146.3(3) 12 . ? O2 Zr1 O10 146.3(3) . . ? O1 Zr1 O10 87.2(5) 12 . ? O1 Zr1 O10 87.2(5) . . ? O8 Zr1 O10 99.3(7) . . ? O2 Zr1 O6 139.7(4) 12 . ? O2 Zr1 O6 77.2(5) . . ? O1 Zr1 O6 140.5(4) 12 . ? O1 Zr1 O6 75.8(5) . . ? O8 Zr1 O6 73.4(3) . . ? O10 Zr1 O6 72.4(3) . . ? O2 Zr1 O6 77.2(5) 12 12 ? O2 Zr1 O6 139.7(4) . 12 ? O1 Zr1 O6 75.8(5) 12 12 ? O1 Zr1 O6 140.5(4) . 12 ? O8 Zr1 O6 73.4(3) . 12 ? O10 Zr1 O6 72.4(3) . 12 ? O6 Zr1 O6 126.0(6) . 12 ? O12 Zr2 O12 87.7(11) . 2 ? O12 Zr2 O2 91.6(6) . . ? O12 Zr2 O2 146.7(3) 2 . ? O12 Zr2 O2 91.6(6) . 12 ? O12 Zr2 O2 146.7(3) 2 12 ? O2 Zr2 O2 66.7(5) . 12 ? O12 Zr2 O2 146.7(3) . 2 ? O12 Zr2 O2 91.6(6) 2 2 ? O2 Zr2 O2 106.4(8) . 2 ? O2 Zr2 O2 71.2(7) 12 2 ? O12 Zr2 O2 146.7(3) . 11_565 ? O12 Zr2 O2 91.6(6) 2 11_565 ? O2 Zr2 O2 71.2(7) . 11_565 ? O2 Zr2 O2 106.4(8) 12 11_565 ? O2 Zr2 O2 66.7(5) 2 11_565 ? O12 Zr2 O11 72.0(3) . 2 ? O12 Zr2 O11 72.0(3) 2 2 ? O2 Zr2 O11 76.2(4) . 2 ? O2 Zr2 O11 138.9(3) 12 2 ? O2 Zr2 O11 138.9(3) 2 2 ? O2 Zr2 O11 76.2(4) 11_565 2 ? O12 Zr2 O11 72.0(3) . . ? O12 Zr2 O11 72.0(3) 2 . ? O2 Zr2 O11 138.9(3) . . ? O2 Zr2 O11 76.2(4) 12 . ? O2 Zr2 O11 76.2(4) 2 . ? O2 Zr2 O11 138.9(3) 11_565 . ? O11 Zr2 O11 129.1(7) 2 . ? O1 Zr3 O1 70.6(8) . 11_565 ? O1 Zr3 O7 142.7(3) . . ? O1 Zr3 O7 142.7(3) 11_565 . ? O1 Zr3 O2 107.7(6) . 11_565 ? O1 Zr3 O2 69.7(4) 11_565 11_565 ? O7 Zr3 O2 80.8(4) . 11_565 ? O1 Zr3 O2 69.7(4) . . ? O1 Zr3 O2 107.7(6) 11_565 . ? O7 Zr3 O2 80.8(4) . . ? O2 Zr3 O2 68.5(7) 11_565 . ? O1 Zr3 O5 141.3(4) . 11_565 ? O1 Zr3 O5 76.6(5) 11_565 11_565 ? O7 Zr3 O5 75.6(2) . 11_565 ? O2 Zr3 O5 78.6(5) 11_565 11_565 ? O2 Zr3 O5 142.0(4) . 11_565 ? O1 Zr3 O5 76.6(5) . . ? O1 Zr3 O5 141.3(4) 11_565 . ? O7 Zr3 O5 75.6(2) . . ? O2 Zr3 O5 142.0(4) 11_565 . ? O2 Zr3 O5 78.6(5) . . ? O5 Zr3 O5 122.3(5) 11_565 . ? O1 Zr3 O3 78.1(4) . . ? O1 Zr3 O3 78.1(4) 11_565 . ? O7 Zr3 O3 117.7(4) . . ? O2 Zr3 O3 142.4(3) 11_565 . ? O2 Zr3 O3 142.4(3) . . ? O5 Zr3 O3 75.5(2) 11_565 . ? O5 Zr3 O3 75.5(2) . . ? O9 Zr4 O9 97.1(8) 2 . ? O9 Zr4 O1 87.2(5) 2 2 ? O9 Zr4 O1 145.0(3) . 2 ? O9 Zr4 O1 145.0(3) 2 12 ? O9 Zr4 O1 87.2(5) . 12 ? O1 Zr4 O1 70.8(8) 2 12 ? O9 Zr4 O1 87.2(5) 2 11_565 ? O9 Zr4 O1 145.0(3) . 11_565 ? O1 Zr4 O1 69.7(6) 2 11_565 ? O1 Zr4 O1 108.9(7) 12 11_565 ? O9 Zr4 O1 145.0(3) 2 . ? O9 Zr4 O1 87.2(5) . . ? O1 Zr4 O1 108.9(7) 2 . ? O1 Zr4 O1 69.7(6) 12 . ? O1 Zr4 O1 70.8(8) 11_565 . ? O9 Zr4 O4 74.2(3) 2 2 ? O9 Zr4 O4 74.2(3) . 2 ? O1 Zr4 O4 73.7(4) 2 2 ? O1 Zr4 O4 73.7(4) 12 2 ? O1 Zr4 O4 139.4(4) 11_565 2 ? O1 Zr4 O4 139.4(4) . 2 ? O9 Zr4 O4 74.2(3) 2 . ? O9 Zr4 O4 74.2(3) . . ? O1 Zr4 O4 139.4(4) 2 . ? O1 Zr4 O4 139.4(4) 12 . ? O1 Zr4 O4 73.7(4) 11_565 . ? O1 Zr4 O4 73.7(4) . . ? O4 Zr4 O4 131.4(7) 2 . ? Zr4 O1 Zr1 110.4(5) . . ? Zr4 O1 Zr3 109.3(7) . . ? Zr1 O1 Zr3 108.9(4) . . ? Zr1 O2 Zr2 113.1(5) . . ? Zr1 O2 Zr3 110.0(4) . . ? Zr2 O2 Zr3 110.0(7) . . ? C1 O3 Zr3 134.6(11) . . ? C1 O4 Zr4 138.4(10) . . ? C7 O5 Zr3 135.7(9) . . ? C7 O6 Zr1 136.9(12) . . ? C13 O7 Zr3 130.3(10) . . ? C13 O11 Zr2 135.3(11) 2 . ? O3 C1 O4 122.4(15) . . ? O3 C1 C2 122.0(16) . . ? O4 C1 C2 115.6(14) . . ? C3 C2 C5 119.4(15) . . ? C3 C2 C1 117.9(15) . . ? C5 C2 C1 122.7(16) . . ? C4 C3 C2 118.4(17) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C6 124.7(16) . 13_556 ? C3 C4 H4 117.6 . . ? C6 C4 H4 117.6 13_556 . ? C6 C5 C2 120.9(17) . . ? C6 C5 H5 119.5 . . ? C2 C5 H5 119.5 . . ? C5 C6 C4 123.5(16) . 13_556 ? C5 C6 C6 120(2) . 13_556 ? C4 C6 C6 116.5(17) 13_556 13_556 ? O6 C7 O5 121.5(15) . . ? O6 C7 C8 120.8(16) . . ? O5 C7 C8 117.7(13) . . ? C11 C8 C9 120.6(16) . . ? C11 C8 C7 120.3(19) . . ? C9 C8 C7 118.9(14) . . ? C8 C9 C10 120.1(16) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C10 C10 C12 121(2) 6 6 ? C10 C10 C9 118(2) 6 . ? C12 C10 C9 119.8(17) 6 . ? C8 C11 C12 120(2) . . ? C8 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C10 C12 C11 118.0(18) 6 . ? C10 C12 H12 121.0 6 . ? C11 C12 H12 121.0 . . ? O11 C13 O7 127.0(14) 2 . ? O11 C13 C14 116.9(17) 2 . ? O7 C13 C14 116.0(17) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.765 _diffrn_reflns_theta_full 30.14 _diffrn_measured_fraction_theta_full 0.765 _refine_diff_density_max 1.831 _refine_diff_density_min -2.795 _refine_diff_density_rms 0.196 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.015 0.005 -0.031 5177 1774 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 937880'