#------------------------------------------------------------------------------
#$Date: 2016-03-26 12:56:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180217 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/03/7110323.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_7110323
loop_
_publ_author_name
'Baunemann, Arne'
'Thomas, Reji'
'Becker, Ralf'
'Winter, Manuela'
'Fischer, Roland A.'
'Ehrhart, Peter'
'Waser, Rainer'
'Devi, Anjana'
_publ_section_title
;
 Mononuclear precursor for MOCVD of HfO2 thin filmsElectronic
 supplementary information (ESI) available: TG/DTA, and isothermal
 studies, RBS and AFM data of HfO2 film. See
 http://www.rsc.org/suppdata/cc/b4/b405015k/
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1610
_journal_page_last               1611
_journal_paper_doi               10.1039/b405015k
_journal_year                    2004
_chemical_formula_sum            'C22 H40 Hf O8'
_chemical_formula_weight         611.03
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 97.548(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.872(3)
_cell_length_b                   15.312(4)
_cell_length_c                   18.599(4)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      10.0
_cell_volume                     2787.1(13)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruke axs CCD 1000'
_diffrn_measurement_method       ω-scans
_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  0.1274
_diffrn_reflns_av_sigmaI/netI    0.1312
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7901
_diffrn_reflns_theta_full        25.13
_diffrn_reflns_theta_max         25.13
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    3.780
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.449
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.38
_refine_diff_density_max         1.273
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.082
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                1751
_reflns_number_total             2471
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b405015ksup1.cif
_cod_data_source_block           raf40
_cod_original_cell_volume        2787.1(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7110323
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Hf1 Hf 0.5000 0.30020(3) 0.7500 0.03817(19) Uani 1 2 d S
O1 O 0.7000(6) 0.3260(3) 0.7951(3) 0.0477(14) Uani 1 1 d .
C2 C 0.7593(8) 0.3860(6) 0.8388(4) 0.043(2) Uani 1 1 d .
C3 C 0.6943(8) 0.4480(5) 0.8711(4) 0.042(2) Uani 1 1 d .
H3 H 0.7469 0.4864 0.9028 0.050 Uiso 1 1 calc R
C4 C 0.5509(9) 0.4596(5) 0.8605(4) 0.041(2) Uani 1 1 d .
O4 O 0.5063(5) 0.5275(3) 0.8958(3) 0.0448(14) Uani 1 1 d .
C41 C 0.3639(9) 0.5564(6) 0.8881(4) 0.053(2) Uani 1 1 d .
C411 C 0.3708(10) 0.6336(6) 0.9386(4) 0.065(3) Uani 1 1 d .
H41A H 0.4022 0.6145 0.9877 0.097 Uiso 1 1 calc R
H41B H 0.2807 0.6595 0.9368 0.097 Uiso 1 1 calc R
H41C H 0.4339 0.6766 0.9238 0.097 Uiso 1 1 calc R
C413 C 0.2785(9) 0.4834(6) 0.9159(5) 0.072(3) Uani 1 1 d .
H41D H 0.2689 0.4358 0.8811 0.108 Uiso 1 1 calc R
H41E H 0.1888 0.5057 0.9220 0.108 Uiso 1 1 calc R
H41F H 0.3235 0.4622 0.9621 0.108 Uiso 1 1 calc R
C412 C 0.3186(11) 0.5839(7) 0.8115(5) 0.088(4) Uani 1 1 d .
H41G H 0.3852 0.6237 0.7958 0.132 Uiso 1 1 calc R
H41H H 0.2307 0.6128 0.8087 0.132 Uiso 1 1 calc R
H41I H 0.3105 0.5328 0.7803 0.132 Uiso 1 1 calc R
C21 C 0.9148(8) 0.3783(7) 0.8513(5) 0.065(3) Uani 1 1 d .
H21A H 0.9403 0.3193 0.8666 0.098 Uiso 1 1 calc R
H21B H 0.9516 0.4193 0.8886 0.098 Uiso 1 1 calc R
H21C H 0.9513 0.3914 0.8065 0.098 Uiso 1 1 calc R
O5 O 0.4680(5) 0.4112(4) 0.8210(3) 0.0420(13) Uani 1 1 d .
O6 O 0.5538(5) 0.2218(3) 0.6784(3) 0.0499(15) Uani 1 1 d .
C61 C 0.6281(10) 0.1817(9) 0.6296(6) 0.098(4) Uani 1 1 d .
H61 H 0.6460 0.1230 0.6510 0.118 Uiso 1 1 calc R
C611 C 0.5499(11) 0.1625(8) 0.5609(5) 0.089(4) Uani 1 1 d .
H61A H 0.4799 0.1199 0.5676 0.134 Uiso 1 1 calc R
H61B H 0.6097 0.1391 0.5282 0.134 Uiso 1 1 calc R
H61C H 0.5072 0.2156 0.5405 0.134 Uiso 1 1 calc R
C612 C 0.7632(10) 0.2171(7) 0.6306(6) 0.091(4) Uani 1 1 d .
H61D H 0.7589 0.2696 0.6012 0.136 Uiso 1 1 calc R
H61E H 0.8212 0.1743 0.6111 0.136 Uiso 1 1 calc R
H61F H 0.8007 0.2311 0.6800 0.136 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
O6 Hf1 O6 102.6(3) . 2_656
O6 Hf1 O1 100.0(2) . 2_656
O6 Hf1 O1 93.7(2) 2_656 2_656
O6 Hf1 O1 93.7(2) . .
O6 Hf1 O1 100.0(2) 2_656 .
O1 Hf1 O1 158.1(3) 2_656 .
O6 Hf1 O5 89.5(2) . 2_656
O6 Hf1 O5 166.97(19) 2_656 2_656
O1 Hf1 O5 79.31(18) 2_656 2_656
O1 Hf1 O5 83.81(19) . 2_656
O6 Hf1 O5 167.0(2) . .
O6 Hf1 O5 89.5(2) 2_656 .
O1 Hf1 O5 83.81(19) 2_656 .
O1 Hf1 O5 79.31(18) . .
O5 Hf1 O5 78.9(3) 2_656 .
C2 O1 Hf1 134.9(5) . .
O1 C2 C3 125.1(8) . .
O1 C2 C21 113.5(7) . .
C3 C2 C21 121.4(8) . .
C2 C3 C4 124.0(8) . .
C2 C3 H3 118.0 . .
C4 C3 H3 118.0 . .
O5 C4 O4 120.8(7) . .
O5 C4 C3 124.5(7) . .
O4 C4 C3 114.7(7) . .
C4 O4 C41 124.3(6) . .
O4 C41 C412 109.9(6) . .
O4 C41 C411 102.3(7) . .
C412 C41 C411 110.9(8) . .
O4 C41 C413 108.1(7) . .
C412 C41 C413 114.6(8) . .
C411 C41 C413 110.2(6) . .
C41 C411 H41A 109.5 . .
C41 C411 H41B 109.5 . .
H41A C411 H41B 109.5 . .
C41 C411 H41C 109.5 . .
H41A C411 H41C 109.5 . .
H41B C411 H41C 109.5 . .
C41 C413 H41D 109.5 . .
C41 C413 H41E 109.5 . .
H41D C413 H41E 109.5 . .
C41 C413 H41F 109.5 . .
H41D C413 H41F 109.5 . .
H41E C413 H41F 109.5 . .
C41 C412 H41G 109.5 . .
C41 C412 H41H 109.5 . .
H41G C412 H41H 109.5 . .
C41 C412 H41I 109.5 . .
H41G C412 H41I 109.5 . .
H41H C412 H41I 109.5 . .
C2 C21 H21A 109.5 . .
C2 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C2 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C4 O5 Hf1 132.0(5) . .
C61 O6 Hf1 162.2(6) . .
O6 C61 C611 114.0(9) . .
O6 C61 C612 113.3(8) . .
C611 C61 C612 118.6(10) . .
O6 C61 H61 102.7 . .
C611 C61 H61 102.7 . .
C612 C61 H61 102.7 . .
C61 C611 H61A 109.4 . .
C61 C611 H61B 109.5 . .
H61A C611 H61B 109.5 . .
C61 C611 H61C 109.5 . .
H61A C611 H61C 109.5 . .
H61B C611 H61C 109.5 . .
C61 C612 H61D 109.5 . .
C61 C612 H61E 109.4 . .
H61D C612 H61E 109.5 . .
C61 C612 H61F 109.5 . .
H61D C612 H61F 109.5 . .
H61E C612 H61F 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Hf1 O6 1.919(5) .
Hf1 O6 1.919(5) 2_656
Hf1 O1 2.079(6) 2_656
Hf1 O1 2.079(6) .
Hf1 O5 2.200(5) 2_656
Hf1 O5 2.200(5) .
O1 C2 1.312(9) .
C2 C3 1.333(10) .
C2 C21 1.526(11) .
C3 C4 1.414(10) .
C3 H3 0.9400 .
C4 O5 1.266(9) .
C4 O4 1.335(9) .
O4 C41 1.462(9) .
C41 C412 1.497(11) .
C41 C411 1.505(11) .
C41 C413 1.531(12) .
C411 H41A 0.9700 .
C411 H41B 0.9700 .
C411 H41C 0.9700 .
C413 H41D 0.9700 .
C413 H41E 0.9700 .
C413 H41F 0.9700 .
C412 H41G 0.9700 .
C412 H41H 0.9700 .
C412 H41I 0.9700 .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C21 H21C 0.9700 .
O6 C61 1.384(10) .
C61 C611 1.433(13) .
C61 C612 1.438(13) .
C61 H61 0.9900 .
C611 H61A 0.9700 .
C611 H61B 0.9700 .
C611 H61C 0.9700 .
C612 H61D 0.9700 .
C612 H61E 0.9700 .
C612 H61F 0.9700 .
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
O6 Hf1 O1 C2 164.2(6) .
O6 Hf1 O1 C2 -92.3(7) 2_656
O1 Hf1 O1 C2 35.5(6) 2_656
O5 Hf1 O1 C2 75.1(6) 2_656
O5 Hf1 O1 C2 -4.7(6) .
Hf1 O1 C2 C3 5.0(12) .
Hf1 O1 C2 C21 -175.9(5) .
O1 C2 C3 C4 -2.4(12) .
C21 C2 C3 C4 178.6(7) .
C2 C3 C4 O5 2.1(12) .
C2 C3 C4 O4 -177.7(7) .
O5 C4 O4 C41 -5.2(10) .
C3 C4 O4 C41 174.6(6) .
C4 O4 C41 C412 -61.9(9) .
C4 O4 C41 C411 -179.8(6) .
C4 O4 C41 C413 63.9(9) .
O4 C4 O5 Hf1 175.7(4) .
C3 C4 O5 Hf1 -4.0(11) .
O6 Hf1 O5 C4 -54.0(12) .
O6 Hf1 O5 C4 104.5(6) 2_656
O1 Hf1 O5 C4 -161.8(6) 2_656
O1 Hf1 O5 C4 4.2(6) .
O5 Hf1 O5 C4 -81.5(6) 2_656
O6 Hf1 O6 C61 -130(2) 2_656
O1 Hf1 O6 C61 134(2) 2_656
O1 Hf1 O6 C61 -28(2) .
O5 Hf1 O6 C61 55(2) 2_656
O5 Hf1 O6 C61 28(3) .
Hf1 O6 C61 C611 -133.9(18) .
Hf1 O6 C61 C612 6(3) .
