#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:11:17 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179680 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/02/7000242.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7000242
loop_
_publ_author_name
'Pothiraja, Ramasamy'
'Milanov, Andrian'
'Parala, Harish'
'Winter, Manuela'
'Fischer, Roland A.'
'Devi, Anjana'
_publ_section_title
;
 Monomeric malonate precursors for the MOCVD of HfO2 and ZrO2 thin
 films
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              654
_journal_paper_doi               10.1039/b810528f
_journal_year                    2009
_chemical_formula_sum            'C35 H52 Hf O16'
_chemical_formula_weight         907.26
_chemical_name_systematic
;
?
;
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.421(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3042(7)
_cell_length_b                   18.4262(8)
_cell_length_c                   15.8807(7)
_cell_measurement_reflns_used    2100
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      2.565
_cell_volume                     3975.2(3)
_computing_cell_refinement       'CrysAlis RED 1.171.13, Oxford Diffraction'
_computing_data_collection       'CrysAlis CCD 1.171.13, Oxford Diffraction'
_computing_data_reduction        'CrysAlis RED 1.171.13, Oxford Diffraction'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Sapphire2-CCD, Oxford Diffraction'
_diffrn_measurement_method       '560 images at 1.0 deg. in ω and 15 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32128
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    2.692
_exptl_absorpt_correction_T_max  0.430
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.31
_refine_diff_density_max         3.003
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0203P)²+13.2862P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                5379
_reflns_number_total             6982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b810528f.txt
_cod_data_source_block           cvd185
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7000242
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_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 0.254718(13) 0.890089(9) 0.746876(13) 0.02340(6) Uani 1 1 d . . .
O31 O 0.2310(2) 0.98481(16) 0.8160(2) 0.0272(7) Uani 1 1 d . . .
O15 O 0.2615(2) 0.98077(16) 0.6624(2) 0.0267(7) Uani 1 1 d . . .
O25 O 0.1798(2) 0.79342(16) 0.6683(2) 0.0267(7) Uani 1 1 d . . .
O41 O 0.3438(2) 0.80048(16) 0.8367(2) 0.0285(7) Uani 1 1 d . . .
O11 O 0.3418(2) 0.85008(15) 0.6802(2) 0.0262(7) Uani 1 1 d . . .
O35 O 0.1837(2) 0.84823(16) 0.8259(2) 0.0281(7) Uani 1 1 d . . .
O45 O 0.3955(2) 0.93846(16) 0.8368(2) 0.0260(7) Uani 1 1 d . . .
O44 O 0.5550(2) 0.96378(17) 0.9216(2) 0.0323(7) Uani 1 1 d . . .
O14 O 0.3203(2) 1.06692(16) 0.6020(2) 0.0340(8) Uani 1 1 d . . .
C14 C 0.3203(3) 0.9980(2) 0.6301(3) 0.0272(10) Uani 1 1 d . . .
O21 O 0.1058(2) 0.92596(16) 0.6542(2) 0.0291(7) Uani 1 1 d . . .
O32 O 0.1621(3) 1.06777(18) 0.8696(3) 0.0419(9) Uani 1 1 d . . .
O12 O 0.4601(2) 0.84065(17) 0.6340(2) 0.0337(7) Uani 1 1 d . . .
O42 O 0.4692(2) 0.72373(17) 0.9166(2) 0.0359(8) Uani 1 1 d . . .
C32 C 0.1754(3) 0.9981(2) 0.8526(3) 0.0295(10) Uani 1 1 d . . .
O34 O 0.0991(2) 0.82811(19) 0.9070(3) 0.0419(9) Uani 1 1 d . . .
C22 C 0.0243(3) 0.8944(3) 0.6112(3) 0.0331(11) Uani 1 1 d . . .
C13 C 0.3865(3) 0.9527(2) 0.6191(3) 0.0323(11) Uani 1 1 d . . .
H2A H 0.4272 0.9707 0.5932 0.039 Uiso 1 1 calc R . .
C44 C 0.4814(3) 0.9153(2) 0.8872(3) 0.0267(10) Uani 1 1 d . . .
C34 C 0.1383(3) 0.8745(3) 0.8680(3) 0.0313(11) Uani 1 1 d . . .
C33 C 0.1256(3) 0.9476(3) 0.8799(3) 0.0340(11) Uani 1 1 d . . .
H8A H 0.0840 0.9628 0.9061 0.041 Uiso 1 1 calc R . .
C12 C 0.3925(3) 0.8808(2) 0.6462(3) 0.0270(10) Uani 1 1 d . . .
C43 C 0.5070(3) 0.8435(2) 0.9119(3) 0.0306(10) Uani 1 1 d . . .
H5A H 0.5743 0.8305 0.9475 0.037 Uiso 1 1 calc R . .
C42 C 0.4348(3) 0.7906(2) 0.8849(3) 0.0271(10) Uani 1 1 d . . .
O24 O 0.0687(2) 0.70400(17) 0.6090(2) 0.0377(8) Uani 1 1 d . . .
O22 O -0.0579(2) 0.93535(19) 0.5737(3) 0.0531(10) Uani 1 1 d . . .
C141 C 0.2603(3) 1.1187(2) 0.6204(3) 0.0323(10) Uani 1 1 d . . .
H31A H 0.2823 1.1227 0.6894 0.039 Uiso 1 1 calc R . .
H31B H 0.1904 1.1036 0.5887 0.039 Uiso 1 1 calc R . .
C441 C 0.5300(3) 1.0391(3) 0.8934(4) 0.0344(11) Uani 1 1 d . . .
H71A H 0.4808 1.0569 0.9127 0.041 Uiso 1 1 calc R . .
H71B H 0.5023 1.0441 0.8237 0.041 Uiso 1 1 calc R . .
C23 C 0.0100(3) 0.8201(3) 0.5972(4) 0.0380(12) Uani 1 1 d . . .
H11A H -0.0548 0.8006 0.5670 0.046 Uiso 1 1 calc R . .
C24 C 0.0905(3) 0.7748(2) 0.6273(3) 0.0300(10) Uani 1 1 d . . .
C421 C 0.4016(4) 0.6634(3) 0.8865(4) 0.0369(11) Uani 1 1 d . . .
H81A H 0.3335 0.6813 0.8639 0.044 Uiso 1 1 calc R . .
H81B H 0.4172 0.6303 0.9407 0.044 Uiso 1 1 calc R . .
C121 C 0.4804(4) 0.7689(3) 0.6760(4) 0.0373(12) Uani 1 1 d . . .
H41A H 0.4213 0.7377 0.6451 0.045 Uiso 1 1 calc R . .
H41B H 0.4995 0.7719 0.7446 0.045 Uiso 1 1 calc R . .
C122 C 0.5630(4) 0.7379(3) 0.6616(4) 0.0415(12) Uani 1 1 d . . .
H42A H 0.5792 0.6893 0.6897 0.062 Uiso 1 1 calc R . .
H42B H 0.6209 0.7693 0.6922 0.062 Uiso 1 1 calc R . .
H42C H 0.5429 0.7347 0.5936 0.062 Uiso 1 1 calc R . .
C241 C 0.1483(4) 0.6525(3) 0.6454(4) 0.0400(12) Uani 1 1 d . . .
H15A H 0.1880 0.6582 0.7149 0.048 Uiso 1 1 calc R . .
H15B H 0.1918 0.6599 0.6154 0.048 Uiso 1 1 calc R . .
C341 C 0.1106(4) 0.7509(3) 0.8954(4) 0.0430(13) Uani 1 1 d . . .
H12A H 0.1004 0.7415 0.8302 0.052 Uiso 1 1 calc R . .
H12B H 0.0600 0.7235 0.9047 0.052 Uiso 1 1 calc R . .
C442 C 0.6239(4) 1.0812(3) 0.9426(4) 0.0402(12) Uani 1 1 d . . .
H72A H 0.6109 1.1326 0.9259 0.060 Uiso 1 1 calc R . .
H72B H 0.6717 1.0629 0.9229 0.060 Uiso 1 1 calc R . .
H72C H 0.6504 1.0755 1.0114 0.060 Uiso 1 1 calc R . .
C321 C 0.2096(5) 1.1222(3) 0.8393(5) 0.0547(16) Uani 1 1 d . . .
H11B H 0.1917 1.1152 0.7715 0.066 Uiso 1 1 calc R . .
H11C H 0.2820 1.1182 0.8768 0.066 Uiso 1 1 calc R . .
C342 C 0.2111(4) 0.7249(3) 0.9653(4) 0.0474(14) Uani 1 1 d . . .
H12C H 0.2169 0.6729 0.9560 0.071 Uiso 1 1 calc R . .
H12D H 0.2208 0.7334 1.0300 0.071 Uiso 1 1 calc R . .
H12E H 0.2612 0.7515 0.9556 0.071 Uiso 1 1 calc R . .
C221 C -0.0489(4) 1.0139(3) 0.5856(5) 0.0607(18) Uani 1 1 d . . .
H16A H 0.0208 1.0285 0.6101 0.073 Uiso 1 1 calc R . .
H16B H -0.0879 1.0382 0.5238 0.073 Uiso 1 1 calc R . .
C142 C 0.2730(4) 1.1901(3) 0.5811(4) 0.0463(13) Uani 1 1 d . . .
H32A H 0.2333 1.2274 0.5916 0.069 Uiso 1 1 calc R . .
H32B H 0.2514 1.1852 0.5129 0.069 Uiso 1 1 calc R . .
H32C H 0.3425 1.2043 0.6132 0.069 Uiso 1 1 calc R . .
C242 C 0.1025(4) 0.5782(3) 0.6222(4) 0.0475(14) Uani 1 1 d . . .
H15C H 0.1544 0.5413 0.6460 0.071 Uiso 1 1 calc R . .
H15D H 0.0637 0.5732 0.5533 0.071 Uiso 1 1 calc R . .
H15E H 0.0596 0.5717 0.6521 0.071 Uiso 1 1 calc R . .
C422 C 0.4093(4) 0.6234(3) 0.8087(4) 0.0566(16) Uani 1 1 d . . .
H82A H 0.3637 0.5822 0.7888 0.085 Uiso 1 1 calc R . .
H82B H 0.4768 0.6056 0.8314 0.085 Uiso 1 1 calc R . .
H82C H 0.3926 0.6561 0.7548 0.085 Uiso 1 1 calc R . .
C222 C -0.0842(7) 1.0346(4) 0.6507(6) 0.091(3) Uani 1 1 d . . .
H16C H -0.0790 1.0874 0.6593 0.136 Uiso 1 1 calc R . .
H16D H -0.0448 1.0108 0.7119 0.136 Uiso 1 1 calc R . .
H16E H -0.1532 1.0200 0.6259 0.136 Uiso 1 1 calc R . .
C93 C 0.6814(4) 0.9225(3) 0.7812(4) 0.0414(12) Uani 1 1 d . . .
H99A H 0.6164 0.9402 0.7603 0.050 Uiso 1 1 calc R . .
C94 C 0.7379(4) 0.9083(3) 0.8756(4) 0.0449(13) Uani 1 1 d . . .
H99B H 0.7120 0.9162 0.9188 0.054 Uiso 1 1 calc R . .
C92 C 0.7152(4) 0.9122(3) 0.7150(5) 0.0510(15) Uani 1 1 d . . .
C91 C 0.6503(5) 0.9275(4) 0.6111(5) 0.074(2) Uani 1 1 d . . .
H99C H 0.5867 0.9463 0.6022 0.111 Uiso 1 1 calc R . .
H99D H 0.6401 0.8827 0.5747 0.111 Uiso 1 1 calc R . .
H99E H 0.6821 0.9637 0.5891 0.111 Uiso 1 1 calc R . .
C95 C 0.8324(4) 0.8824(3) 0.9080(5) 0.0544(15) Uani 1 1 d . . .
H99F H 0.8723 0.8730 0.9736 0.065 Uiso 1 1 calc R . .
C97 C 0.8104(5) 0.8851(3) 0.7488(6) 0.0639(19) Uani 1 1 d . . .
H99G H 0.8363 0.8766 0.7056 0.077 Uiso 1 1 calc R . .
C96 C 0.8678(4) 0.8704(3) 0.8442(6) 0.069(2) Uani 1 1 d . . .
H99H H 0.9325 0.8518 0.8656 0.083 Uiso 1 1 calc R . .
C322 C 0.1769(7) 1.1929(4) 0.8535(8) 0.114(4) Uani 1 1 d . . .
H11D H 0.2093 1.2308 0.8345 0.172 Uiso 1 1 calc R . .
H11E H 0.1941 1.1990 0.9206 0.172 Uiso 1 1 calc R . .
H11F H 0.1054 1.1967 0.8150 0.172 Uiso 1 1 calc R . .
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'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O35 Hf1 O45 112.44(11) . . ?
O35 Hf1 O21 81.34(11) . . ?
O45 Hf1 O21 137.81(11) . . ?
O35 Hf1 O25 76.47(11) . . ?
O45 Hf1 O25 145.26(11) . . ?
O21 Hf1 O25 75.44(11) . . ?
O35 Hf1 O15 144.86(11) . . ?
O45 Hf1 O15 76.93(11) . . ?
O21 Hf1 O15 71.44(11) . . ?
O25 Hf1 O15 115.94(11) . . ?
O35 Hf1 O11 138.67(10) . . ?
O45 Hf1 O11 79.25(11) . . ?
O21 Hf1 O11 117.42(11) . . ?
O25 Hf1 O11 73.90(11) . . ?
O15 Hf1 O11 75.28(11) . . ?
O35 Hf1 O31 75.31(11) . . ?
O45 Hf1 O31 71.48(11) . . ?
O21 Hf1 O31 74.38(11) . . ?
O25 Hf1 O31 141.15(11) . . ?
O15 Hf1 O31 76.25(11) . . ?
O11 Hf1 O31 142.88(11) . . ?
O35 Hf1 O41 71.33(11) . . ?
O45 Hf1 O41 75.44(11) . . ?
O21 Hf1 O41 144.38(11) . . ?
O25 Hf1 O41 76.27(11) . . ?
O15 Hf1 O41 141.82(11) . . ?
O11 Hf1 O41 74.09(11) . . ?
O31 Hf1 O41 118.17(11) . . ?
C32 O31 Hf1 134.0(3) . . ?
C14 O15 Hf1 133.5(3) . . ?
C24 O25 Hf1 132.8(3) . . ?
C42 O41 Hf1 133.4(3) . . ?
C12 O11 Hf1 133.5(3) . . ?
C34 O35 Hf1 136.3(3) . . ?
C44 O45 Hf1 135.6(3) . . ?
C44 O44 C441 117.2(3) . . ?
C14 O14 C141 117.3(3) . . ?
O15 C14 O14 118.8(4) . . ?
O15 C14 C13 126.7(4) . . ?
O14 C14 C13 114.5(4) . . ?
C22 O21 Hf1 134.3(3) . . ?
C32 O32 C321 116.7(4) . . ?
C12 O12 C121 116.7(3) . . ?
C42 O42 C421 119.0(4) . . ?
O31 C32 O32 118.4(4) . . ?
O31 C32 C33 126.7(4) . . ?
O32 C32 C33 114.9(4) . . ?
C34 O34 C341 117.2(4) . . ?
O21 C22 O22 118.2(4) . . ?
O21 C22 C23 126.0(4) . . ?
O22 C22 C23 115.7(4) . . ?
C12 C13 C14 119.1(4) . . ?
C12 C13 H2A 120.5 . . ?
C14 C13 H2A 120.5 . . ?
O45 C44 O44 118.0(4) . . ?
O45 C44 C43 125.5(4) . . ?
O44 C44 C43 116.5(4) . . ?
O35 C34 O34 118.1(4) . . ?
O35 C34 C33 126.2(4) . . ?
O34 C34 C33 115.7(4) . . ?
C34 C33 C32 118.5(4) . . ?
C34 C33 H8A 120.8 . . ?
C32 C33 H8A 120.8 . . ?
O11 C12 O12 118.3(4) . . ?
O11 C12 C13 126.6(4) . . ?
O12 C12 C13 115.1(4) . . ?
C44 C43 C42 120.2(4) . . ?
C44 C43 H5A 119.9 . . ?
C42 C43 H5A 119.9 . . ?
O41 C42 O42 119.7(4) . . ?
O41 C42 C43 126.1(4) . . ?
O42 C42 C43 114.2(4) . . ?
C24 O24 C241 118.2(4) . . ?
C22 O22 C221 119.0(4) . . ?
O14 C141 C142 106.2(4) . . ?
O14 C141 H31A 110.5 . . ?
C142 C141 H31A 110.5 . . ?
O14 C141 H31B 110.5 . . ?
C142 C141 H31B 110.5 . . ?
H31A C141 H31B 108.7 . . ?
O44 C441 C442 106.3(4) . . ?
O44 C441 H71A 110.5 . . ?
C442 C441 H71A 110.5 . . ?
O44 C441 H71B 110.5 . . ?
C442 C441 H71B 110.5 . . ?
H71A C441 H71B 108.7 . . ?
C24 C23 C22 119.4(4) . . ?
C24 C23 H11A 120.3 . . ?
C22 C23 H11A 120.3 . . ?
O25 C24 O24 118.6(4) . . ?
O25 C24 C23 126.7(4) . . ?
O24 C24 C23 114.8(4) . . ?
O42 C421 C422 109.7(4) . . ?
O42 C421 H81A 109.7 . . ?
C422 C421 H81A 109.7 . . ?
O42 C421 H81B 109.7 . . ?
C422 C421 H81B 109.7 . . ?
H81A C421 H81B 108.2 . . ?
O12 C121 C122 107.2(4) . . ?
O12 C121 H41A 110.3 . . ?
C122 C121 H41A 110.3 . . ?
O12 C121 H41B 110.3 . . ?
C122 C121 H41B 110.3 . . ?
H41A C121 H41B 108.5 . . ?
C121 C122 H42A 109.5 . . ?
C121 C122 H42B 109.5 . . ?
H42A C122 H42B 109.5 . . ?
C121 C122 H42C 109.5 . . ?
H42A C122 H42C 109.5 . . ?
H42B C122 H42C 109.5 . . ?
O24 C241 C242 106.8(4) . . ?
O24 C241 H15A 110.4 . . ?
C242 C241 H15A 110.4 . . ?
O24 C241 H15B 110.4 . . ?
C242 C241 H15B 110.4 . . ?
H15A C241 H15B 108.6 . . ?
O34 C341 C342 111.1(4) . . ?
O34 C341 H12A 109.4 . . ?
C342 C341 H12A 109.4 . . ?
O34 C341 H12B 109.4 . . ?
C342 C341 H12B 109.4 . . ?
H12A C341 H12B 108.0 . . ?
C441 C442 H72A 109.5 . . ?
C441 C442 H72B 109.5 . . ?
H72A C442 H72B 109.5 . . ?
C441 C442 H72C 109.5 . . ?
H72A C442 H72C 109.5 . . ?
H72B C442 H72C 109.5 . . ?
O32 C321 C322 108.1(5) . . ?
O32 C321 H11B 110.1 . . ?
C322 C321 H11B 110.1 . . ?
O32 C321 H11C 110.1 . . ?
C322 C321 H11C 110.1 . . ?
H11B C321 H11C 108.4 . . ?
C341 C342 H12C 109.5 . . ?
C341 C342 H12D 109.5 . . ?
H12C C342 H12D 109.5 . . ?
C341 C342 H12E 109.5 . . ?
H12C C342 H12E 109.5 . . ?
H12D C342 H12E 109.5 . . ?
C222 C221 O22 108.4(5) . . ?
C222 C221 H16A 110.0 . . ?
O22 C221 H16A 110.0 . . ?
C222 C221 H16B 110.0 . . ?
O22 C221 H16B 110.0 . . ?
H16A C221 H16B 108.4 . . ?
C141 C142 H32A 109.5 . . ?
C141 C142 H32B 109.5 . . ?
H32A C142 H32B 109.5 . . ?
C141 C142 H32C 109.5 . . ?
H32A C142 H32C 109.5 . . ?
H32B C142 H32C 109.5 . . ?
C241 C242 H15C 109.5 . . ?
C241 C242 H15D 109.5 . . ?
H15C C242 H15D 109.5 . . ?
C241 C242 H15E 109.5 . . ?
H15C C242 H15E 109.5 . . ?
H15D C242 H15E 109.5 . . ?
C421 C422 H82A 109.5 . . ?
C421 C422 H82B 109.5 . . ?
H82A C422 H82B 109.5 . . ?
C421 C422 H82C 109.5 . . ?
H82A C422 H82C 109.5 . . ?
H82B C422 H82C 109.5 . . ?
C221 C222 H16C 109.5 . . ?
C221 C222 H16D 109.5 . . ?
H16C C222 H16D 109.5 . . ?
C221 C222 H16E 109.5 . . ?
H16C C222 H16E 109.5 . . ?
H16D C222 H16E 109.5 . . ?
C94 C93 C92 122.6(5) . . ?
C94 C93 H99A 118.7 . . ?
C92 C93 H99A 118.7 . . ?
C93 C94 C95 120.1(6) . . ?
C93 C94 H99B 120.0 . . ?
C95 C94 H99B 120.0 . . ?
C93 C92 C97 116.6(6) . . ?
C93 C92 C91 121.2(5) . . ?
C97 C92 C91 122.2(6) . . ?
C92 C91 H99C 109.5 . . ?
C92 C91 H99D 109.5 . . ?
H99C C91 H99D 109.5 . . ?
C92 C91 H99E 109.5 . . ?
H99C C91 H99E 109.5 . . ?
H99D C91 H99E 109.5 . . ?
C96 C95 C94 118.9(6) . . ?
C96 C95 H99F 120.5 . . ?
C94 C95 H99F 120.5 . . ?
C96 C97 C92 121.0(6) . . ?
C96 C97 H99G 119.5 . . ?
C92 C97 H99G 119.5 . . ?
C95 C96 C97 120.7(5) . . ?
C95 C96 H99H 119.6 . . ?
C97 C96 H99H 119.6 . . ?
C321 C322 H11D 109.5 . . ?
C321 C322 H11E 109.5 . . ?
H11D C322 H11E 109.5 . . ?
C321 C322 H11F 109.5 . . ?
H11D C322 H11F 109.5 . . ?
H11E C322 H11F 109.5 . . ?
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 O35 2.146(3) . ?
Hf1 O45 2.154(3) . ?
Hf1 O21 2.170(3) . ?
Hf1 O25 2.174(3) . ?
Hf1 O15 2.176(3) . ?
Hf1 O11 2.178(3) . ?
Hf1 O31 2.180(3) . ?
Hf1 O41 2.197(3) . ?
O31 C32 1.256(5) . ?
O15 C14 1.264(5) . ?
O25 C24 1.260(5) . ?
O41 C42 1.256(5) . ?
O11 C12 1.265(5) . ?
O35 C34 1.262(5) . ?
O45 C44 1.258(5) . ?
O44 C44 1.342(5) . ?
O44 C441 1.455(5) . ?
O14 C14 1.346(5) . ?
O14 C141 1.444(5) . ?
C14 C13 1.386(6) . ?
O21 C22 1.255(5) . ?
O32 C32 1.346(5) . ?
O32 C321 1.445(6) . ?
O12 C12 1.356(5) . ?
O12 C121 1.450(5) . ?
O42 C42 1.343(5) . ?
O42 C421 1.443(6) . ?
C32 C33 1.393(6) . ?
O34 C34 1.347(5) . ?
O34 C341 1.456(6) . ?
C22 O22 1.348(5) . ?
C22 C23 1.388(7) . ?
C13 C12 1.382(6) . ?
C13 H2A 0.9500 . ?
C44 C43 1.384(6) . ?
C34 C33 1.386(7) . ?
C33 H8A 0.9500 . ?
C43 C42 1.386(6) . ?
C43 H5A 0.9500 . ?
O24 C24 1.345(5) . ?
O24 C241 1.440(6) . ?
O22 C221 1.458(7) . ?
C141 C142 1.507(6) . ?
C141 H31A 0.9900 . ?
C141 H31B 0.9900 . ?
C441 C442 1.497(6) . ?
C441 H71A 0.9900 . ?
C441 H71B 0.9900 . ?
C23 C24 1.379(7) . ?
C23 H11A 0.9500 . ?
C421 C422 1.488(7) . ?
C421 H81A 0.9900 . ?
C421 H81B 0.9900 . ?
C121 C122 1.497(6) . ?
C121 H41A 0.9900 . ?
C121 H41B 0.9900 . ?
C122 H42A 0.9800 . ?
C122 H42B 0.9800 . ?
C122 H42C 0.9800 . ?
C241 C242 1.504(7) . ?
C241 H15A 0.9900 . ?
C241 H15B 0.9900 . ?
C341 C342 1.501(7) . ?
C341 H12A 0.9900 . ?
C341 H12B 0.9900 . ?
C442 H72A 0.9800 . ?
C442 H72B 0.9800 . ?
C442 H72C 0.9800 . ?
C321 C322 1.449(8) . ?
C321 H11B 0.9900 . ?
C321 H11C 0.9900 . ?
C342 H12C 0.9800 . ?
C342 H12D 0.9800 . ?
C342 H12E 0.9800 . ?
C221 C222 1.423(9) . ?
C221 H16A 0.9900 . ?
C221 H16B 0.9900 . ?
C142 H32A 0.9800 . ?
C142 H32B 0.9800 . ?
C142 H32C 0.9800 . ?
C242 H15C 0.9800 . ?
C242 H15D 0.9800 . ?
C242 H15E 0.9800 . ?
C422 H82A 0.9800 . ?
C422 H82B 0.9800 . ?
C422 H82C 0.9800 . ?
C222 H16C 0.9800 . ?
C222 H16D 0.9800 . ?
C222 H16E 0.9800 . ?
C93 C94 1.368(8) . ?
C93 C92 1.380(7) . ?
C93 H99A 0.9500 . ?
C94 C95 1.377(7) . ?
C94 H99B 0.9500 . ?
C92 C97 1.393(9) . ?
C92 C91 1.510(9) . ?
C91 H99C 0.9800 . ?
C91 H99D 0.9800 . ?
C91 H99E 0.9800 . ?
C95 C96 1.370(9) . ?
C95 H99F 0.9500 . ?
C97 C96 1.384(10) . ?
C97 H99G 0.9500 . ?
C96 H99H 0.9500 . ?
C322 H11D 0.9800 . ?
C322 H11E 0.9800 . ?
C322 H11F 0.9800 . ?
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
O35 Hf1 O31 C32 -19.0(4) . . . . ?
O45 Hf1 O31 C32 -139.3(4) . . . . ?
O21 Hf1 O31 C32 65.9(4) . . . . ?
O25 Hf1 O31 C32 25.7(5) . . . . ?
O15 Hf1 O31 C32 140.1(4) . . . . ?
O11 Hf1 O31 C32 -179.1(4) . . . . ?
O41 Hf1 O31 C32 -78.0(4) . . . . ?
O35 Hf1 O15 C14 169.9(3) . . . . ?
O45 Hf1 O15 C14 59.3(4) . . . . ?
O21 Hf1 O15 C14 -149.0(4) . . . . ?
O25 Hf1 O15 C14 -86.3(4) . . . . ?
O11 Hf1 O15 C14 -22.8(4) . . . . ?
O31 Hf1 O15 C14 133.1(4) . . . . ?
O41 Hf1 O15 C14 14.8(5) . . . . ?
O35 Hf1 O25 C24 59.9(4) . . . . ?
O45 Hf1 O25 C24 169.9(4) . . . . ?
O21 Hf1 O25 C24 -24.5(4) . . . . ?
O15 Hf1 O25 C24 -85.0(4) . . . . ?
O11 Hf1 O25 C24 -149.2(4) . . . . ?
O31 Hf1 O25 C24 15.5(5) . . . . ?
O41 Hf1 O25 C24 133.7(4) . . . . ?
O35 Hf1 O41 C42 -140.3(4) . . . . ?
O45 Hf1 O41 C42 -20.0(4) . . . . ?
O21 Hf1 O41 C42 177.9(3) . . . . ?
O25 Hf1 O41 C42 139.6(4) . . . . ?
O15 Hf1 O41 C42 24.9(5) . . . . ?
O11 Hf1 O41 C42 62.7(4) . . . . ?
O31 Hf1 O41 C42 -79.2(4) . . . . ?
O35 Hf1 O11 C12 -168.1(3) . . . . ?
O45 Hf1 O11 C12 -56.2(4) . . . . ?
O21 Hf1 O11 C12 82.5(4) . . . . ?
O25 Hf1 O11 C12 146.1(4) . . . . ?
O15 Hf1 O11 C12 23.0(4) . . . . ?
O31 Hf1 O11 C12 -18.1(5) . . . . ?
O41 Hf1 O11 C12 -134.0(4) . . . . ?
O45 Hf1 O35 C34 75.6(4) . . . . ?
O21 Hf1 O35 C34 -62.9(4) . . . . ?
O25 Hf1 O35 C34 -139.9(4) . . . . ?
O15 Hf1 O35 C34 -23.8(5) . . . . ?
O11 Hf1 O35 C34 175.0(4) . . . . ?
O31 Hf1 O35 C34 13.2(4) . . . . ?
O41 Hf1 O35 C34 140.3(4) . . . . ?
O35 Hf1 O45 C44 80.7(4) . . . . ?
O21 Hf1 O45 C44 -177.0(4) . . . . ?
O25 Hf1 O45 C44 -18.0(5) . . . . ?
O15 Hf1 O45 C44 -134.9(4) . . . . ?
O11 Hf1 O45 C44 -57.7(4) . . . . ?
O31 Hf1 O45 C44 145.4(4) . . . . ?
O41 Hf1 O45 C44 18.4(4) . . . . ?
Hf1 O15 C14 O14 -162.3(3) . . . . ?
Hf1 O15 C14 C13 18.3(7) . . . . ?
C141 O14 C14 O15 6.6(6) . . . . ?
C141 O14 C14 C13 -173.9(4) . . . . ?
O35 Hf1 O21 C22 -56.9(4) . . . . ?
O45 Hf1 O21 C22 -170.9(4) . . . . ?
O25 Hf1 O21 C22 21.3(4) . . . . ?
O15 Hf1 O21 C22 145.6(4) . . . . ?
O11 Hf1 O21 C22 84.0(4) . . . . ?
O31 Hf1 O21 C22 -134.0(4) . . . . ?
O41 Hf1 O21 C22 -17.1(5) . . . . ?
Hf1 O31 C32 O32 -164.5(3) . . . . ?
Hf1 O31 C32 C33 16.7(7) . . . . ?
C321 O32 C32 O31 3.2(7) . . . . ?
C321 O32 C32 C33 -177.9(5) . . . . ?
Hf1 O21 C22 O22 167.4(3) . . . . ?
Hf1 O21 C22 C23 -13.4(8) . . . . ?
O15 C14 C13 C12 -0.8(8) . . . . ?
O14 C14 C13 C12 179.8(4) . . . . ?
Hf1 O45 C44 O44 168.9(3) . . . . ?
Hf1 O45 C44 C43 -12.1(7) . . . . ?
C441 O44 C44 O45 -3.3(6) . . . . ?
C441 O44 C44 C43 177.6(4) . . . . ?
Hf1 O35 C34 O34 176.8(3) . . . . ?
Hf1 O35 C34 C33 -4.4(7) . . . . ?
C341 O34 C34 O35 -1.4(6) . . . . ?
C341 O34 C34 C33 179.7(4) . . . . ?
O35 C34 C33 C32 -7.3(8) . . . . ?
O34 C34 C33 C32 171.5(4) . . . . ?
O31 C32 C33 C34 1.2(8) . . . . ?
O32 C32 C33 C34 -177.7(4) . . . . ?
Hf1 O11 C12 O12 161.5(3) . . . . ?
Hf1 O11 C12 C13 -18.6(7) . . . . ?
C121 O12 C12 O11 -10.3(6) . . . . ?
C121 O12 C12 C13 169.9(4) . . . . ?
C14 C13 C12 O11 1.0(7) . . . . ?
C14 C13 C12 O12 -179.2(4) . . . . ?
O45 C44 C43 C42 -3.4(7) . . . . ?
O44 C44 C43 C42 175.6(4) . . . . ?
Hf1 O41 C42 O42 -165.6(3) . . . . ?
Hf1 O41 C42 C43 15.9(7) . . . . ?
C421 O42 C42 O41 6.3(6) . . . . ?
C421 O42 C42 C43 -175.0(4) . . . . ?
C44 C43 C42 O41 1.2(7) . . . . ?
C44 C43 C42 O42 -177.4(4) . . . . ?
O21 C22 O22 C221 -0.8(7) . . . . ?
C23 C22 O22 C221 179.9(5) . . . . ?
C14 O14 C141 C142 -179.3(4) . . . . ?
C44 O44 C441 C442 178.8(4) . . . . ?
O21 C22 C23 C24 -3.9(8) . . . . ?
O22 C22 C23 C24 175.3(5) . . . . ?
Hf1 O25 C24 O24 -160.3(3) . . . . ?
Hf1 O25 C24 C23 20.5(7) . . . . ?
C241 O24 C24 O25 6.0(6) . . . . ?
C241 O24 C24 C23 -174.7(4) . . . . ?
C22 C23 C24 O25 0.3(8) . . . . ?
C22 C23 C24 O24 -179.0(4) . . . . ?
C42 O42 C421 C422 100.2(5) . . . . ?
C12 O12 C121 C122 -174.7(4) . . . . ?
C24 O24 C241 C242 175.0(4) . . . . ?
C34 O34 C341 C342 80.0(5) . . . . ?
C32 O32 C321 C322 173.3(6) . . . . ?
C22 O22 C221 C222 -108.6(6) . . . . ?
C92 C93 C94 C95 -0.2(8) . . . . ?
C94 C93 C92 C97 1.0(8) . . . . ?
C94 C93 C92 C91 179.2(5) . . . . ?
C93 C94 C95 C96 -0.8(8) . . . . ?
C93 C92 C97 C96 -0.8(8) . . . . ?
C91 C92 C97 C96 -179.0(6) . . . . ?
C94 C95 C96 C97 1.0(9) . . . . ?
C92 C97 C96 C95 -0.2(9) . . . . ?
