#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/75/2217593.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_2217593
loop_
_publ_author_name
'Wisniewska, Aleksandra'
'Baranowska, Katarzyna'
'Pikies, Jerzy'
_publ_section_title
Dichlorido-1κCl,3κCl-hexakis[1,1,2,2,3,3(η⁵)-methylcyclopentadienyl]di-μ₂-oxido-1:2κ²O:O;2:3κ²O:O-trihafnium(IV)
_journal_coeditor_code           NG2389
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m361
_journal_page_last               m361
_journal_paper_doi               10.1107/S1600536807061417
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Hf3 (C6 H7)6 Cl2 O2]'
_chemical_formula_moiety         'C36 H42 Cl2 Hf3 O2'
_chemical_formula_sum            'C36 H42 Cl2 Hf3 O2'
_chemical_formula_weight         1113.07
_chemical_name_systematic
;
Dichlorido-1\kCl,3\kCl-hexakis[1,1,2,2,3,3(η⁵)-methylcyclopentadienyl]di-
μ₂-oxido-1:2κ²O:O;2:3κ²O:O-trihafnium(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.466(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9598(10)
_cell_length_b                   12.9710(5)
_cell_length_c                   14.6178(6)
_cell_measurement_reflns_used    6065
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.4265
_cell_measurement_theta_min      1.9305
_cell_volume                     3409.8(3)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device       '4-axis κ geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction KM4 CCD'
_diffrn_measurement_method       'ω scans, 0.75 deg width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11353
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    9.298
_exptl_absorpt_correction_T_max  0.434
_exptl_absorpt_correction_T_min  0.283
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.413
_refine_diff_density_min         -2.698
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5801
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.061
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.1162P)²+4.6904P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1851
_reflns_number_gt                4052
_reflns_number_total             5801
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng2389.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2217593
_cod_database_fobs_code          2217593
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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 0.11659(4) 0.32908(5) 0.39912(5) 0.0309(2) Uani d . 1 . .
Hf Hf2 0.31749(4) 0.38207(5) 0.56434(5) 0.0279(2) Uani d . 1 . .
Hf Hf3 0.30910(4) 0.67984(5) 0.58248(5) 0.0331(2) Uani d . 1 A .
O O1 0.2183(6) 0.3553(8) 0.4746(9) 0.037(3) Uani d . 1 . .
O O2 0.3134(7) 0.5372(8) 0.5725(10) 0.049(4) Uani d . 1 A .
Cl Cl1 0.0620(3) 0.3676(3) 0.5261(4) 0.0450(11) Uani d . 1 . .
Cl Cl2 0.2938(12) 0.741(3) 0.4165(7) 0.056(7) Uani d P 0.61(7) A 1
Cl Cl2A 0.319(2) 0.693(3) 0.4198(12) 0.051(8) Uani d P 0.39(7) A 2
C C1 0.0637(13) 0.3899(16) 0.2276(16) 0.059(6) Uani d . 1 . .
H H1 0.0484 0.3399 0.1776 0.07 Uiso calc R 1 . .
C C2 0.1362(13) 0.4306(14) 0.2644(15) 0.052(5) Uani d . 1 . .
H H2 0.1777 0.411 0.2452 0.062 Uiso calc R 1 . .
C C3 0.1366(13) 0.5039(13) 0.3334(15) 0.049(5) Uani d . 1 . .
H H3 0.1774 0.5461 0.3676 0.059 Uiso calc R 1 . .
C C4 0.0661(11) 0.5041(13) 0.3434(15) 0.046(5) Uani d . 1 . .
H H4 0.0514 0.5446 0.3884 0.056 Uiso calc R 1 . .
C C5 0.0181(11) 0.4330(14) 0.2745(16) 0.050(5) Uani d . 1 . .
C C6 -0.0606(12) 0.4165(17) 0.261(2) 0.070(7) Uani d . 1 . .
H H6A -0.0777 0.3549 0.2211 0.105 Uiso calc R 1 . .
H H6B -0.0891 0.4765 0.2285 0.105 Uiso calc R 1 . .
H H6C -0.0679 0.4069 0.3237 0.105 Uiso calc R 1 . .
C C7 0.1181(10) 0.1447(13) 0.4586(17) 0.051(5) Uani d . 1 . .
H H7 0.1331 0.1332 0.5262 0.061 Uiso calc R 1 . .
C C8 0.1654(14) 0.1518(14) 0.398(3) 0.075(9) Uani d . 1 . .
H H8 0.2179 0.1437 0.4181 0.09 Uiso calc R 1 . .
C C9 0.1227(14) 0.1712(15) 0.3092(19) 0.059(6) Uani d . 1 . .
H H9 0.14 0.1812 0.2555 0.07 Uiso calc R 1 . .
C C10 0.0499(14) 0.1749(12) 0.3057(16) 0.051(5) Uani d . 1 . .
H H10 0.0084 0.1868 0.2498 0.062 Uiso calc R 1 . .
C C11 0.0472(13) 0.1584(14) 0.3974(19) 0.057(6) Uani d . 1 . .
C C12 -0.0240(13) 0.1464(17) 0.426(2) 0.068(7) Uani d . 1 . .
H H12A -0.038 0.0735 0.4228 0.102 Uiso calc R 1 . .
H H12B -0.0643 0.186 0.3809 0.102 Uiso calc R 1 . .
H H12C -0.0149 0.1722 0.4915 0.102 Uiso calc R 1 . .
C C13 0.3497(13) 0.3140(18) 0.4161(18) 0.066(3) Uani d D 1 . .
H H13 0.311 0.2875 0.3627 0.079 Uiso calc R 1 . .
C C14 0.3922(12) 0.2589(19) 0.4995(17) 0.066(3) Uani d D 1 . .
H H14 0.3862 0.1879 0.5112 0.079 Uiso calc R 1 . .
C C15 0.4404(13) 0.3201(17) 0.5573(19) 0.066(3) Uani d D 1 . .
H H15 0.4749 0.3 0.6174 0.079 Uiso calc R 1 . .
C C16 0.4349(13) 0.4140(19) 0.5209(17) 0.066(3) Uani d D 1 . .
H H16 0.4644 0.4717 0.5502 0.079 Uiso calc R 1 . .
C C17 0.3762(12) 0.4144(18) 0.4285(17) 0.066(3) Uani d D 1 . .
C C18 0.3580(13) 0.5119(17) 0.3697(18) 0.066(3) Uani d D 1 . .
H H18A 0.3902 0.5173 0.329 0.08 Uiso calc R 1 . .
H H18B 0.3662 0.5715 0.413 0.08 Uiso calc R 1 . .
H H18C 0.3059 0.5103 0.3289 0.08 Uiso calc R 1 . .
C C19 0.2593(18) 0.283(2) 0.6744(16) 0.081(3) Uani d D 1 . .
H H19 0.2137 0.2478 0.6448 0.097 Uiso calc R 1 . .
C C20 0.2703(18) 0.381(2) 0.7065(15) 0.081(3) Uani d D 1 . .
H H20 0.2309 0.4285 0.702 0.097 Uiso calc R 1 . .
C C21 0.3378(18) 0.404(2) 0.7429(15) 0.081(3) Uani d D 1 . .
H H21 0.3542 0.4707 0.7685 0.097 Uiso calc R 1 . .
C C22 0.3828(19) 0.330(2) 0.7422(16) 0.081(3) Uani d D 1 . .
H H22 0.4355 0.3331 0.7667 0.097 Uiso calc R 1 . .
C C23 0.3394(17) 0.242(2) 0.6982(13) 0.081(3) Uani d D 1 . .
C C24 0.3580(17) 0.1362(19) 0.6783(17) 0.081(3) Uani d D 1 . .
H H24A 0.3199 0.1103 0.6205 0.08 Uiso calc R 1 . .
H H24B 0.36 0.092 0.7334 0.08 Uiso calc R 1 . .
H H24C 0.4065 0.1358 0.6676 0.08 Uiso calc R 1 . .
C C25 0.3903(12) 0.8149(18) 0.6894(18) 0.064(3) Uani d . 1 A .
H H25 0.366 0.8746 0.7023 0.076 Uiso calc R 1 . .
C C26 0.3995(12) 0.7254(17) 0.7377(18) 0.064(3) Uani d . 1 A .
H H26 0.3831 0.7127 0.7918 0.076 Uiso calc R 1 . .
C C27 0.4380(12) 0.6501(18) 0.6960(18) 0.064(3) Uani d . 1 A .
H H27 0.4519 0.5816 0.7172 0.076 Uiso calc R 1 . .
C C28 0.4500(12) 0.7013(17) 0.6182(18) 0.064(3) Uani d . 1 A .
H H28 0.4721 0.6717 0.5745 0.076 Uiso calc R 1 . .
C C29 0.4241(12) 0.8036(18) 0.6143(18) 0.064(3) Uani d . 1 . .
C C30 0.4338(12) 0.8816(17) 0.5436(17) 0.064(3) Uani d . 1 A .
H H30A 0.3889 0.924 0.5204 0.08 Uiso calc R 1 . .
H H30B 0.4424 0.8461 0.4889 0.08 Uiso calc R 1 . .
H H30C 0.4765 0.9258 0.5752 0.08 Uiso calc R 1 . .
C C31 0.2248(13) 0.7771(18) 0.658(2) 0.071(3) Uani d . 1 A .
H H31 0.244 0.8231 0.7109 0.086 Uiso calc R 1 . .
C C32 0.2150(13) 0.6754(18) 0.665(2) 0.071(3) Uani d . 1 A .
H H32 0.2312 0.6363 0.7229 0.086 Uiso calc R 1 . .
C C33 0.1776(13) 0.6357(19) 0.574(2) 0.071(3) Uani d . 1 A .
H H33 0.1589 0.5675 0.5608 0.086 Uiso calc R 1 . .
C C34 0.1724(13) 0.7119(17) 0.508(2) 0.071(3) Uani d . 1 A .
H H34 0.1526 0.7046 0.4403 0.086 Uiso calc R 1 . .
C C35 0.2015(14) 0.8040(18) 0.559(2) 0.071(3) Uani d . 1 A .
C C36 0.2008(13) 0.9084(16) 0.520(2) 0.071(3) Uani d . 1 . .
H H36A 0.1504 0.9368 0.5024 0.08 Uiso calc R 1 A .
H H36B 0.2166 0.9057 0.462 0.08 Uiso calc R 1 . .
H H36C 0.2349 0.9525 0.5683 0.08 Uiso calc R 1 . .
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.583 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
_geom_angle_publ_flag
O1 Hf1 Cl1 96.7(4) yes
O1 Hf1 C9 104.2(7) ?
Cl1 Hf1 C9 132.8(6) ?
O1 Hf1 C8 81.9(7) ?
Cl1 Hf1 C8 116.4(7) ?
C9 Hf1 C8 30.9(8) ?
O1 Hf1 C2 89.2(6) ?
Cl1 Hf1 C2 134.2(5) ?
C9 Hf1 C2 88.5(7) ?
C8 Hf1 C2 109.5(9) ?
O1 Hf1 C4 103.7(5) ?
Cl1 Hf1 C4 81.5(5) ?
C9 Hf1 C4 131.4(8) ?
C8 Hf1 C4 160.9(9) ?
C2 Hf1 C4 53.1(7) ?
O1 Hf1 C1 121.8(6) ?
Cl1 Hf1 C1 124.2(6) ?
C9 Hf1 C1 78.4(8) ?
C8 Hf1 C1 108.3(10) ?
C2 Hf1 C1 32.7(7) ?
C4 Hf1 C1 53.1(7) ?
O1 Hf1 C10 133.6(6) ?
Cl1 Hf1 C10 108.2(5) ?
C9 Hf1 C10 31.8(7) ?
C8 Hf1 C10 52.1(8) ?
C2 Hf1 C10 99.5(7) ?
C4 Hf1 C10 118.0(7) ?
C1 Hf1 C10 74.7(7) ?
O1 Hf1 C3 79.4(6) ?
Cl1 Hf1 C3 104.7(5) ?
C9 Hf1 C3 120.3(7) ?
C8 Hf1 C3 136.4(8) ?
C2 Hf1 C3 32.0(6) ?
C4 Hf1 C3 32.0(6) ?
C1 Hf1 C3 53.3(7) ?
C10 Hf1 C3 127.8(7) ?
O1 Hf1 C7 94.0(5) ?
Cl1 Hf1 C7 83.9(5) ?
C9 Hf1 C7 53.2(8) ?
C8 Hf1 C7 33.6(8) ?
C2 Hf1 C7 141.2(7) ?
C4 Hf1 C7 158.2(6) ?
C1 Hf1 C7 126.4(7) ?
C10 Hf1 C7 52.3(7) ?
C3 Hf1 C7 169.6(7) ?
O1 Hf1 C5 133.8(5) ?
Cl1 Hf1 C5 92.6(5) ?
C9 Hf1 C5 102.0(8) ?
C8 Hf1 C5 132.6(9) ?
C2 Hf1 C5 54.1(7) ?
C4 Hf1 C5 33.5(6) ?
C1 Hf1 C5 31.7(7) ?
C10 Hf1 C5 84.5(7) ?
C3 Hf1 C5 54.5(7) ?
C7 Hf1 C5 132.1(6) ?
O1 Hf1 C11 125.0(6) ?
Cl1 Hf1 C11 81.1(5) ?
C9 Hf1 C11 52.2(7) ?
C8 Hf1 C11 52.6(7) ?
C2 Hf1 C11 130.6(7) ?
C4 Hf1 C11 129.6(7) ?
C1 Hf1 C11 102.7(8) ?
C10 Hf1 C11 31.3(7) ?
C3 Hf1 C11 154.6(8) ?
C7 Hf1 C11 31.1(7) ?
C5 Hf1 C11 101.1(7) ?
O1 Hf2 O2 99.8(5) yes
O1 Hf2 C15 128.9(7) ?
O2 Hf2 C15 112.2(6) ?
O1 Hf2 C20 92.0(8) ?
O2 Hf2 C20 85.6(7) ?
C15 Hf2 C20 128.0(9) ?
O1 Hf2 C14 99.8(7) ?
O2 Hf2 C14 133.9(7) ?
C15 Hf2 C14 30.1(7) ?
C20 Hf2 C14 134.6(8) ?
O1 Hf2 C21 120.8(8) ?
O2 Hf2 C21 79.7(7) ?
C15 Hf2 C21 103.9(9) ?
C20 Hf2 C21 28.9(8) ?
C14 Hf2 C21 122.9(9) ?
O1 Hf2 C16 126.6(7) ?
O2 Hf2 C16 84.6(6) ?
C15 Hf2 C16 30.4(7) ?
C20 Hf2 C16 141.2(9) ?
C14 Hf2 C16 50.6(8) ?
C21 Hf2 C16 112.4(9) ?
O1 Hf2 C19 79.5(8) ?
O2 Hf2 C19 115.5(7) ?
C15 Hf2 C19 117.1(8) ?
C20 Hf2 C19 31.0(8) ?
C14 Hf2 C19 108.9(8) ?
C21 Hf2 C19 50.7(9) ?
C16 Hf2 C19 145.6(9) ?
O1 Hf2 C13 79.0(6) ?
O2 Hf2 C13 114.4(6) ?
C15 Hf2 C13 52.0(8) ?
C20 Hf2 C13 159.0(8) ?
C14 Hf2 C13 32.4(7) ?
C21 Hf2 C13 154.7(9) ?
C16 Hf2 C13 52.2(8) ?
C19 Hf2 C13 128.1(8) ?
O1 Hf2 C22 132.9(7) ?
O2 Hf2 C22 102.4(7) ?
C15 Hf2 C22 78.6(9) ?
C20 Hf2 C22 49.5(10) ?
C14 Hf2 C22 93.8(8) ?
C21 Hf2 C22 29.1(8) ?
C16 Hf2 C22 96.6(9) ?
C19 Hf2 C22 53.4(9) ?
C13 Hf2 C22 126.0(8) ?
O1 Hf2 C17 94.0(7) ?
O2 Hf2 C17 85.3(6) ?
C15 Hf2 C17 52.4(8) ?
C20 Hf2 C17 169.8(8) ?
C14 Hf2 C17 52.1(7) ?
C21 Hf2 C17 143.8(9) ?
C16 Hf2 C17 32.9(8) ?
C19 Hf2 C17 158.9(8) ?
C13 Hf2 C17 31.0(7) ?
C22 Hf2 C17 128.7(9) ?
O1 Hf2 C23 105.7(8) ?
O2 Hf2 C23 130.6(7) ?
C15 Hf2 C23 83.0(8) ?
C20 Hf2 C23 52.4(8) ?
C14 Hf2 C23 82.2(8) ?
C21 Hf2 C23 50.9(8) ?
C16 Hf2 C23 111.0(9) ?
C19 Hf2 C23 34.7(8) ?
C13 Hf2 C23 111.5(8) ?
C22 Hf2 C23 32.1(8) ?
C17 Hf2 C23 132.9(8) ?
O2 Hf3 C26 106.2(7) ?
O2 Hf3 Cl2A 88.4(10) ?
C26 Hf3 Cl2A 129.8(8) ?
O2 Hf3 C32 94.1(7) ?
C26 Hf3 C32 87.4(8) ?
Cl2A Hf3 C32 140.3(12) ?
O2 Hf3 Cl2 103.5(10) yes
C26 Hf3 Cl2 131.5(6) ?
Cl2A Hf3 Cl2 18.0(4) ?
C32 Hf3 Cl2 127.7(9) ?
O2 Hf3 C34 101.3(7) ?
C26 Hf3 C34 133.3(8) ?
Cl2A Hf3 C34 87.3(13) ?
C32 Hf3 C34 53.3(9) ?
Cl2 Hf3 C34 74.9(9) ?
O2 Hf3 C27 80.9(7) ?
C26 Hf3 C27 34.3(7) ?
Cl2A Hf3 C27 107.3(12) ?
C32 Hf3 C27 112.3(9) ?
Cl2 Hf3 C27 118.9(8) ?
C34 Hf3 C27 165.4(9) ?
O2 Hf3 C25 135.0(7) ?
C26 Hf3 C25 31.3(7) ?
Cl2A Hf3 C25 109.7(7) ?
C32 Hf3 C25 96.2(8) ?
Cl2 Hf3 C25 104.2(8) ?
C34 Hf3 C25 119.8(8) ?
C27 Hf3 C25 54.7(8) ?
O2 Hf3 C33 80.7(6) ?
C26 Hf3 C33 119.3(8) ?
Cl2A Hf3 C33 110.2(10) ?
C32 Hf3 C33 32.4(8) ?
Cl2 Hf3 C33 102.6(8) ?
C34 Hf3 C33 31.4(8) ?
C27 Hf3 C33 137.4(8) ?
C25 Hf3 C33 125.9(8) ?
O2 Hf3 C35 132.4(7) ?
C26 Hf3 C35 105.7(8) ?
Cl2A Hf3 C35 97.3(14) ?
C32 Hf3 C35 53.3(9) ?
Cl2 Hf3 C35 79.9(11) ?
C34 Hf3 C35 32.7(7) ?
C27 Hf3 C35 139.5(8) ?
C25 Hf3 C35 87.2(8) ?
C33 Hf3 C35 53.0(8) ?
O2 Hf3 C31 125.1(7) ?
C26 Hf3 C31 80.1(8) ?
Cl2A Hf3 C31 129.7(14) ?
C32 Hf3 C31 31.0(7) ?
Cl2 Hf3 C31 111.9(11) ?
C34 Hf3 C31 53.2(9) ?
C27 Hf3 C31 113.7(8) ?
C25 Hf3 C31 74.3(8) ?
C33 Hf3 C31 52.2(8) ?
C35 Hf3 C31 32.6(8) ?
O2 Hf3 C28 93.2(6) ?
C26 Hf3 C28 53.6(8) ?
Cl2A Hf3 C28 78.4(10) ?
C32 Hf3 C28 140.8(9) ?
Cl2 Hf3 C28 87.5(7) ?
C34 Hf3 C28 159.4(8) ?
C27 Hf3 C28 31.9(8) ?
C25 Hf3 C28 53.7(8) ?
C33 Hf3 C28 169.1(8) ?
C35 Hf3 C28 134.3(8) ?
C31 Hf3 C28 127.8(8) ?
Hf1 O1 Hf2 173.3(7) yes
Hf3 O2 Hf2 178.7(8) yes
C5 C1 C2 110.2(19) ?
C5 C1 Hf1 75.3(12) ?
C2 C1 Hf1 72.8(11) ?
C5 C1 H1 124.9 ?
C2 C1 H1 124.9 ?
Hf1 C1 H1 118.7 ?
C3 C2 C1 108(2) ?
C3 C2 Hf1 75.8(11) ?
C1 C2 Hf1 74.5(12) ?
C3 C2 H2 125.8 ?
C1 C2 H2 125.8 ?
Hf1 C2 H2 116 ?
C2 C3 C4 107.1(19) ?
C2 C3 Hf1 72.2(10) ?
C4 C3 Hf1 72.4(10) ?
C2 C3 H3 126.5 ?
C4 C3 H3 126.5 ?
Hf1 C3 H3 120.7 ?
C3 C4 C5 109.8(19) ?
C3 C4 Hf1 75.6(11) ?
C5 C4 Hf1 75.0(10) ?
C3 C4 H4 125.1 ?
C5 C4 H4 125.1 ?
Hf1 C4 H4 116.2 ?
C1 C5 C4 104.4(19) ?
C1 C5 C6 130(2) ?
C4 C5 C6 125(2) ?
C1 C5 Hf1 73.0(12) ?
C4 C5 Hf1 71.6(11) ?
C6 C5 Hf1 120.5(13) ?
C5 C6 H6A 109.5 ?
C5 C6 H6B 109.5 ?
H6A C6 H6B 109.5 ?
C5 C6 H6C 109.5 ?
H6A C6 H6C 109.5 ?
H6B C6 H6C 109.5 ?
C11 C7 C8 105(2) ?
C11 C7 Hf1 75.7(11) ?
C8 C7 Hf1 71.0(12) ?
C11 C7 H7 127.5 ?
C8 C7 H7 127.5 ?
Hf1 C7 H7 118.1 ?
C9 C8 C7 108(2) ?
C9 C8 Hf1 73.5(13) ?
C7 C8 Hf1 75.4(11) ?
C9 C8 H8 126.1 ?
C7 C8 H8 126.1 ?
Hf1 C8 H8 117.1 ?
C8 C9 C10 110(2) ?
C8 C9 Hf1 75.7(14) ?
C10 C9 Hf1 76.8(11) ?
C8 C9 H9 124.9 ?
C10 C9 H9 124.9 ?
Hf1 C9 H9 114.5 ?
C9 C10 C11 108(2) ?
C9 C10 Hf1 71.4(12) ?
C11 C10 Hf1 76.3(11) ?
C9 C10 H10 126.1 ?
C11 C10 H10 126.1 ?
Hf1 C10 H10 118.2 ?
C7 C11 C10 109(2) ?
C7 C11 C12 125(2) ?
C10 C11 C12 126(2) ?
C7 C11 Hf1 73.3(11) ?
C10 C11 Hf1 72.5(11) ?
C12 C11 Hf1 125.0(14) ?
C11 C12 H12A 109.5 ?
C11 C12 H12B 109.5 ?
H12A C12 H12B 109.5 ?
C11 C12 H12C 109.5 ?
H12A C12 H12C 109.5 ?
H12B C12 H12C 109.5 ?
C17 C13 C14 106(2) ?
C17 C13 Hf2 75.0(10) ?
C14 C13 Hf2 70.9(9) ?
C17 C13 H13 127 ?
C14 C13 H13 127 ?
Hf2 C13 H13 119.1 ?
C15 C14 C13 110(2) ?
C15 C14 Hf2 74.4(10) ?
C13 C14 Hf2 76.7(9) ?
C15 C14 H14 125 ?
C13 C14 H14 125 ?
Hf2 C14 H14 115.8 ?
C14 C15 C16 111(3) ?
C14 C15 Hf2 75.5(10) ?
C16 C15 Hf2 76.3(9) ?
C14 C15 H15 124.7 ?
C16 C15 H15 124.7 ?
Hf2 C15 H15 115.3 ?
C15 C16 C17 108(2) ?
C15 C16 Hf2 73.2(9) ?
C17 C16 Hf2 76.0(10) ?
C15 C16 H16 125.8 ?
C17 C16 H16 125.8 ?
Hf2 C16 H16 117 ?
C13 C17 C16 105(2) ?
C13 C17 C18 135(2) ?
C16 C17 C18 120(2) ?
C13 C17 Hf2 74.0(9) ?
C16 C17 Hf2 71.2(9) ?
C18 C17 Hf2 119.7(7) ?
C17 C18 H18A 109.5 ?
C17 C18 H18B 109.5 ?
H18A C18 H18B 109.5 ?
C17 C18 H18C 109.5 ?
H18A C18 H18C 109.5 ?
H18B C18 H18C 109.5 ?
C20 C19 C23 102(3) ?
C20 C19 Hf2 72.2(10) ?
C23 C19 Hf2 74.1(10) ?
C20 C19 H19 128.8 ?
C23 C19 H19 128.8 ?
Hf2 C19 H19 117.6 ?
C21 C20 C19 113(3) ?
C21 C20 Hf2 76.5(12) ?
C19 C20 Hf2 76.8(10) ?
C21 C20 H20 123.4 ?
C19 C20 H20 123.4 ?
Hf2 C20 H20 114.8 ?
C20 C21 C22 114(3) ?
C20 C21 Hf2 74.6(12) ?
C22 C21 Hf2 78.0(11) ?
C20 C21 H21 123 ?
C22 C21 H21 123 ?
Hf2 C21 H21 115.7 ?
C21 C22 C23 108(3) ?
C21 C22 Hf2 72.9(12) ?
C23 C22 Hf2 74.5(11) ?
C21 C22 H22 125.9 ?
C23 C22 H22 125.9 ?
Hf2 C22 H22 118.6 ?
C22 C23 C24 134(3) ?
C22 C23 C19 102(2) ?
C24 C23 C19 124(3) ?
C22 C23 Hf2 73.3(11) ?
C24 C23 Hf2 119.6(8) ?
C19 C23 Hf2 71.3(10) ?
C23 C24 H24A 109.5 ?
C23 C24 H24B 109.5 ?
H24A C24 H24B 109.5 ?
C23 C24 H24C 109.5 ?
H24A C24 H24C 109.5 ?
H24B C24 H24C 109.5 ?
C26 C25 C29 107(2) ?
C26 C25 Hf3 71.2(12) ?
C29 C25 Hf3 77.8(12) ?
C26 C25 H25 126.3 ?
C29 C25 H25 126.3 ?
Hf3 C25 H25 116.8 ?
C25 C26 C27 111(2) ?
C25 C26 Hf3 77.6(14) ?
C27 C26 Hf3 75.4(13) ?
C25 C26 H26 124.5 ?
C27 C26 H26 124.5 ?
Hf3 C26 H26 114.4 ?
C28 C27 C26 105(2) ?
C28 C27 Hf3 76.3(14) ?
C26 C27 Hf3 70.3(13) ?
C28 C27 H27 127.7 ?
C26 C27 H27 127.7 ?
Hf3 C27 H27 118 ?
C27 C28 C29 110(2) ?
C27 C28 Hf3 71.8(13) ?
C29 C28 Hf3 76.6(13) ?
C27 C28 H28 125.2 ?
C29 C28 H28 125.2 ?
Hf3 C28 H28 118.2 ?
C28 C29 C25 107(2) ?
C28 C29 C30 123(2) ?
C25 C29 C30 130(2) ?
C28 C29 Hf3 72.0(11) ?
C25 C29 Hf3 69.7(11) ?
C30 C29 Hf3 124.5(15) ?
C29 C30 H30A 109.5 ?
C29 C30 H30B 109.5 ?
H30A C30 H30B 109.5 ?
C29 C30 H30C 109.5 ?
H30A C30 H30C 109.5 ?
H30B C30 H30C 109.5 ?
C32 C31 C35 108(2) ?
C32 C31 Hf3 70.4(14) ?
C35 C31 Hf3 73.2(14) ?
C32 C31 H31 126 ?
C35 C31 H31 126 ?
Hf3 C31 H31 122 ?
C31 C32 C33 110(3) ?
C31 C32 Hf3 78.6(16) ?
C33 C32 Hf3 76.8(16) ?
C31 C32 H32 125.1 ?
C33 C32 H32 125.1 ?
Hf3 C32 H32 111.8 ?
C34 C33 C32 108(2) ?
C34 C33 Hf3 73.6(14) ?
C32 C33 Hf3 70.9(14) ?
C34 C33 H33 126 ?
C32 C33 H33 126 ?
Hf3 C33 H33 121.2 ?
C33 C34 C35 108(3) ?
C33 C34 Hf3 74.9(14) ?
C35 C34 Hf3 74.7(14) ?
C33 C34 H34 125.9 ?
C35 C34 H34 125.9 ?
Hf3 C34 H34 116.5 ?
C34 C35 C31 106(2) ?
C34 C35 C36 128(3) ?
C31 C35 C36 126(2) ?
C34 C35 Hf3 72.6(13) ?
C31 C35 Hf3 74.2(13) ?
C36 C35 Hf3 123.1(17) ?
C35 C36 H36A 109.5 ?
C35 C36 H36B 109.5 ?
H36A C36 H36B 109.5 ?
C35 C36 H36C 109.5 ?
H36A C36 H36C 109.5 ?
H36B C36 H36C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Hf1 O1 1.925(12) yes
Hf1 Cl1 2.446(4) yes
Hf1 C9 2.46(2) ?
Hf1 C8 2.482(19) ?
Hf1 C2 2.493(18) ?
Hf1 C4 2.498(18) ?
Hf1 C1 2.51(2) ?
Hf1 C10 2.524(18) ?
Hf1 C3 2.538(18) ?
Hf1 C7 2.541(19) ?
Hf1 C5 2.543(19) ?
Hf1 C11 2.571(18) ?
Hf2 O1 1.953(12) yes
Hf2 O2 2.019(11) yes
Hf2 C15 2.498(18) ?
Hf2 C20 2.510(19) ?
Hf2 C14 2.511(17) ?
Hf2 C21 2.53(2) ?
Hf2 C16 2.536(18) ?
Hf2 C19 2.57(2) ?
Hf2 C13 2.586(19) ?
Hf2 C22 2.59(2) ?
Hf2 C17 2.599(15) ?
Hf2 C23 2.606(17) ?
Hf3 O2 1.859(11) yes
Hf3 C26 2.44(2) ?
Hf3 Cl2A 2.447(17) ?
Hf3 C32 2.45(3) ?
Hf3 Cl2 2.479(13) yes
Hf3 C34 2.51(2) ?
Hf3 C27 2.51(2) ?
Hf3 C25 2.52(2) ?
Hf3 C33 2.52(2) ?
Hf3 C35 2.54(2) ?
Hf3 C31 2.55(2) ?
Hf3 C28 2.57(2) ?
C1 C5 1.38(3) ?
C1 C2 1.41(3) ?
C1 H1 0.95 ?
C2 C3 1.39(3) ?
C2 H2 0.95 ?
C3 C4 1.39(3) ?
C3 H3 0.95 ?
C4 C5 1.45(3) ?
C4 H4 0.95 ?
C5 C6 1.46(3) ?
C6 H6A 0.98 ?
C6 H6B 0.98 ?
C6 H6C 0.98 ?
C7 C11 1.37(3) ?
C7 C8 1.45(3) ?
C7 H7 0.95 ?
C8 C9 1.31(4) ?
C8 H8 0.95 ?
C9 C10 1.37(3) ?
C9 H9 0.95 ?
C10 C11 1.37(3) ?
C10 H10 0.95 ?
C11 C12 1.54(3) ?
C12 H12A 0.98 ?
C12 H12B 0.98 ?
C12 H12C 0.98 ?
C13 C17 1.39(3) ?
C13 C14 1.42(3) ?
C13 H13 0.95 ?
C14 C15 1.30(3) ?
C14 H14 0.95 ?
C15 C16 1.32(3) ?
C15 H15 0.95 ?
C16 C17 1.45(4) ?
C16 H16 0.95 ?
C17 C18 1.51(3) ?
C18 H18A 0.98 ?
C18 H18B 0.98 ?
C18 H18C 0.98 ?
C19 C20 1.36(4) ?
C19 C23 1.54(4) ?
C19 H19 0.95 ?
C20 C21 1.26(4) ?
C20 H20 0.95 ?
C21 C22 1.29(4) ?
C21 H21 0.95 ?
C22 C23 1.44(4) ?
C22 H22 0.95 ?
C23 C24 1.47(3) ?
C24 H24A 0.98 ?
C24 H24B 0.98 ?
C24 H24C 0.98 ?
C25 C26 1.34(3) ?
C25 C29 1.44(3) ?
C25 H25 0.95 ?
C26 C27 1.46(3) ?
C26 H26 0.95 ?
C27 C28 1.40(3) ?
C27 H27 0.95 ?
C28 C29 1.41(3) ?
C28 H28 0.95 ?
C29 C30 1.50(3) ?
C30 H30A 0.98 ?
C30 H30B 0.98 ?
C30 H30C 0.98 ?
C31 C32 1.34(3) ?
C31 C35 1.43(4) ?
C31 H31 0.95 ?
C32 C33 1.39(4) ?
C32 H32 0.95 ?
C33 C34 1.36(4) ?
C33 H33 0.95 ?
C34 C35 1.42(3) ?
C34 H34 0.95 ?
C35 C36 1.47(3) ?
C36 H36A 0.98 ?
C36 H36B 0.98 ?
C36 H36C 0.98 ?
