#------------------------------------------------------------------------------ #$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $ #$Revision: 176798 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/23/00/2230093.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2230093 loop_ _publ_author_name 'Burlakov, Vladimir V.' 'Arndt, Perdita' 'Spannenberg, Anke' 'Rosenthal, Uwe' _publ_section_title ; Tris(\h^5^-cyclopentadienyl)hafnium(III) ; _journal_coeditor_code NG5148 _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m629 _journal_paper_doi 10.1107/S1600536811014516 _journal_volume 67 _journal_year 2011 _chemical_formula_iupac '[Hf (C5 H5)3]' _chemical_formula_moiety 'C15 H15 Hf' _chemical_formula_sum 'C15 H15 Hf' _chemical_formula_weight 373.76 _chemical_name_systematic ; Tris(\h^5^-cyclopentadienyl)hafnium(III) ; _space_group_IT_number 176 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-P 6c' _symmetry_space_group_name_H-M 'P 63/m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 2 _cell_length_a 7.9772(4) _cell_length_b 7.9772 _cell_length_c 10.2975(6) _cell_measurement_reflns_used 4609 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.42 _cell_measurement_theta_min 1.93 _cell_volume 567.50(4) _computing_cell_refinement 'X-AREA (Stoe & Cie, 2005)' _computing_data_collection 'X-AREA (Stoe & Cie, 2005)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2005)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0970 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 7314 _diffrn_reflns_theta_full 24.99 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_min 2.95 _exptl_absorpt_coefficient_mu 9.157 _exptl_absorpt_correction_T_max 0.3462 _exptl_absorpt_correction_T_min 0.1499 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(X-SHAPE and X-RED32; Stoe & Cie, 2005)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 354 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.946 _refine_diff_density_min -3.400 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 27 _refine_ls_number_reflns 362 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.217 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0336 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+5.6136P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.0759 _reflns_number_gt 333 _reflns_number_total 362 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ng5148.cif _cod_data_source_block I _cod_original_cell_volume 567.50(5) _cod_database_code 2230093 _cod_database_fobs_code 2230093 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Hf Hf1 0.3333 0.6667 0.2500 0.0342(3) Uani d S 1 . . C C1 0.4331(9) 0.4179(9) 0.1824(6) 0.0236(13) Uani d . 1 . . H H1 0.5434 0.4592 0.1283 0.028 Uiso calc R 1 . . C C2 0.2408(10) 0.3460(10) 0.1393(7) 0.0300(15) Uani d . 1 . . H H2 0.1992 0.3347 0.0517 0.036 Uiso calc R 1 . . C C3 0.1229(14) 0.2944(13) 0.2500 0.026(2) Uani d S 1 . . H H3 -0.0143 0.2344 0.2500 0.032 Uiso calc SR 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Hf1 0.0126(3) 0.0126(3) 0.0772(6) 0.00632(15) 0.000 0.000 C1 0.022(3) 0.019(3) 0.031(3) 0.011(3) 0.003(3) -0.002(3) C2 0.024(3) 0.027(4) 0.035(4) 0.010(3) -0.004(3) -0.001(3) C3 0.017(4) 0.014(4) 0.048(6) 0.008(4) 0.000 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 Hf1 C2 12_566 10_556 101.55(19) ? C2 Hf1 C2 12_566 3_565 53.1(3) ? C2 Hf1 C2 10_556 3_565 126.86(8) ? C2 Hf1 C2 12_566 11_666 101.55(19) ? C2 Hf1 C2 10_556 11_666 101.55(19) ? C2 Hf1 C2 3_565 11_666 126.86(8) ? C2 Hf1 C2 12_566 . 126.86(8) ? C2 Hf1 C2 10_556 . 53.1(3) ? C2 Hf1 C2 3_565 . 101.55(19) ? C2 Hf1 C2 11_666 . 126.86(8) ? C2 Hf1 C2 12_566 2_665 126.86(8) ? C2 Hf1 C2 10_556 2_665 126.86(8) ? C2 Hf1 C2 3_565 2_665 101.55(19) ? C2 Hf1 C2 11_666 2_665 53.1(3) ? C2 Hf1 C2 . 2_665 101.55(19) ? C2 Hf1 C1 12_566 12_566 32.0(2) ? C2 Hf1 C1 10_556 12_566 81.0(2) ? C2 Hf1 C1 3_565 12_566 52.7(2) ? C2 Hf1 C1 11_666 12_566 130.0(2) ? C2 Hf1 C1 . 12_566 94.8(2) ? C2 Hf1 C1 2_665 12_566 152.2(2) ? C2 Hf1 C1 12_566 3_565 52.7(2) ? C2 Hf1 C1 10_556 3_565 94.8(2) ? C2 Hf1 C1 3_565 3_565 32.0(2) ? C2 Hf1 C1 11_666 3_565 152.2(2) ? C2 Hf1 C1 . 3_565 81.0(2) ? C2 Hf1 C1 2_665 3_565 130.0(2) ? C1 Hf1 C1 12_566 3_565 31.4(3) ? C2 Hf1 C1 12_566 11_666 81.0(2) ? C2 Hf1 C1 10_556 11_666 130.0(2) ? C2 Hf1 C1 3_565 11_666 94.8(2) ? C2 Hf1 C1 11_666 11_666 32.0(2) ? C2 Hf1 C1 . 11_666 152.2(2) ? C2 Hf1 C1 2_665 11_666 52.7(2) ? C1 Hf1 C1 12_566 11_666 112.98(12) ? C1 Hf1 C1 3_565 11_666 122.45(4) ? C2 Hf1 C1 12_566 2_665 94.8(2) ? C2 Hf1 C1 10_556 2_665 152.2(2) ? C2 Hf1 C1 3_565 2_665 81.0(2) ? C2 Hf1 C1 11_666 2_665 52.7(2) ? C2 Hf1 C1 . 2_665 130.0(2) ? C2 Hf1 C1 2_665 2_665 32.0(2) ? C1 Hf1 C1 12_566 2_665 122.45(4) ? C1 Hf1 C1 3_565 2_665 112.98(12) ? C1 Hf1 C1 11_666 2_665 31.4(3) ? C2 Hf1 C1 12_566 . 152.1(2) ? C2 Hf1 C1 10_556 . 52.7(2) ? C2 Hf1 C1 3_565 . 130.0(2) ? C2 Hf1 C1 11_666 . 94.8(2) ? C2 Hf1 C1 . . 32.0(2) ? C2 Hf1 C1 2_665 . 81.0(2) ? C1 Hf1 C1 12_566 . 122.45(4) ? C1 Hf1 C1 3_565 . 112.98(12) ? C1 Hf1 C1 11_666 . 122.45(4) ? C1 Hf1 C1 2_665 . 112.98(12) ? C2 Hf1 C1 12_566 10_556 130.0(2) ? C2 Hf1 C1 10_556 10_556 32.0(2) ? C2 Hf1 C1 3_565 10_556 152.1(2) ? C2 Hf1 C1 11_666 10_556 81.0(2) ? C2 Hf1 C1 . 10_556 52.7(2) ? C2 Hf1 C1 2_665 10_556 94.8(2) ? C1 Hf1 C1 12_566 10_556 112.98(12) ? C1 Hf1 C1 3_565 10_556 122.45(4) ? C1 Hf1 C1 11_666 10_556 112.98(12) ? C1 Hf1 C1 2_665 10_556 122.45(4) ? C1 Hf1 C1 . 10_556 31.4(3) ? C1 C1 C2 10_556 . 108.3(4) ? C1 C1 Hf1 10_556 . 74.32(14) ? C2 C1 Hf1 . . 72.9(4) ? C1 C1 H1 10_556 . 125.9 ? C2 C1 H1 . . 125.9 ? Hf1 C1 H1 . . 118.7 ? C3 C2 C1 . . 107.3(6) ? C3 C2 Hf1 . . 75.3(5) ? C1 C2 Hf1 . . 75.0(4) ? C3 C2 H2 . . 126.4 ? C1 C2 H2 . . 126.4 ? Hf1 C2 H2 . . 115.6 ? C2 C3 C2 . 10_556 108.7(8) ? C2 C3 Hf1 . . 73.0(5) ? C2 C3 Hf1 10_556 . 73.0(5) ? C2 C3 H3 . . 125.6 ? C2 C3 H3 10_556 . 125.6 ? Hf1 C3 H3 . . 120.2 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Hf1 C2 12_566 2.549(7) ? Hf1 C2 10_556 2.549(7) ? Hf1 C2 3_565 2.549(7) ? Hf1 C2 11_666 2.549(7) ? Hf1 C2 . 2.549(7) ? Hf1 C2 2_665 2.549(7) ? Hf1 C1 12_566 2.576(6) ? Hf1 C1 3_565 2.576(6) ? Hf1 C1 11_666 2.576(6) ? Hf1 C1 2_665 2.576(6) ? Hf1 C1 . 2.576(6) ? Hf1 C1 10_556 2.576(6) ? C1 C1 10_556 1.392(12) ? C1 C2 . 1.414(9) ? C1 H1 . 0.9500 ? C2 C3 . 1.402(9) ? C2 H2 . 0.9500 ? C3 C2 10_556 1.402(9) ? C3 H3 . 0.9500 ?