#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:25:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179140 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/01/4310150.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_4310150
loop_
_publ_author_name
'Peter Lobinger'
'Harald Jarzina'
'Herbert W. Roesky'
'Sanjay Singh'
'S. Shravan Kumar'
'Hans-Georg Schmidt'
'Matthias Noltemeyer'
'Herbert C. Freyhardt'
_publ_section_title
;
New Synthetic Approach to Yttrium Hydroxoacetates, Structural
Characterization, and Use as a Precursor for Coated Conductors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9192
_journal_page_last               9196
_journal_paper_doi               10.1021/ic0505192
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C12 H34 O20 Y2'
_chemical_formula_weight         676.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.86(3)
_cell_angle_beta                 113.97(3)
_cell_angle_gamma                117.91(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8125(18)
_cell_length_b                   9.1769(18)
_cell_length_c                   10.346(2)
_cell_measurement_temperature    200(2)
_cell_volume                     649.4(4)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe AED2'
_diffrn_measurement_method       'profile fit'
_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  0.1139
_diffrn_reflns_av_sigmaI/netI    0.0890
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7564
_diffrn_reflns_theta_full        29.48
_diffrn_reflns_theta_max         29.48
_diffrn_reflns_theta_min         3.88
_diffrn_standards_interval_time  '90 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.528
_exptl_absorpt_correction_T_max  0.2105
_exptl_absorpt_correction_T_min  0.1720
_exptl_absorpt_correction_type   'azimuthal scans'
_exptl_absorpt_process_details   semiempiric
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         2.417
_refine_diff_density_min         -2.682
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3617
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0542
_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)+(0.0840P)²+0.1200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1454
_reflns_number_gt                3142
_reflns_number_total             3617
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0505192si20050826_111738_1.cif
_cod_data_source_block           Compound1
_cod_original_cell_volume        649.4(2)
_cod_database_code               4310150
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Y1 Y 0.17855(5) -0.09556(4) 0.08948(4) 0.01457(13) Uani 1 1 d . . .
O1 O 0.1428(5) -0.2951(4) -0.0804(4) 0.0261(7) Uani 1 1 d D . .
O2 O 0.2796(5) 0.0582(4) -0.0630(4) 0.0232(6) Uani 1 1 d D . .
O11 O 0.1173(4) 0.1481(3) 0.0983(3) 0.0183(5) Uani 1 1 d . . .
C11 C 0.2787(5) 0.2407(5) 0.2137(4) 0.0174(7) Uani 1 1 d . . .
O12 O 0.3857(4) 0.1823(4) 0.2683(3) 0.0247(6) Uani 1 1 d . . .
C12 C 0.3389(6) 0.4159(5) 0.2837(5) 0.0291(10) Uani 1 1 d . . .
H12A H 0.3137 0.4753 0.2080 0.044 Uiso 1 1 calc R . .
H12B H 0.4786 0.4800 0.3546 0.044 Uiso 1 1 calc R . .
H12C H 0.2641 0.4080 0.3348 0.044 Uiso 1 1 calc R . .
O21 O -0.0172(4) -0.1523(4) 0.2109(3) 0.0207(6) Uani 1 1 d . . .
C21 C -0.0984(6) -0.3126(5) 0.1686(5) 0.0209(7) Uani 1 1 d . . .
O22 O -0.0510(5) -0.3769(4) 0.0936(3) 0.0241(6) Uani 1 1 d . . .
C22 C -0.2538(8) -0.4252(7) 0.2061(6) 0.0377(11) Uani 1 1 d . . .
H22A H -0.2974 -0.5453 0.1705 0.057 Uiso 1 1 calc R . .
H22B H -0.3646 -0.4095 0.1594 0.057 Uiso 1 1 calc R . .
H22C H -0.2014 -0.3947 0.3131 0.057 Uiso 1 1 calc R . .
O31 O 0.3551(5) -0.1507(4) 0.3047(4) 0.0299(7) Uani 1 1 d . . .
C31 C 0.5089(6) -0.0900(5) 0.2928(5) 0.0215(8) Uani 1 1 d . . .
O32 O 0.5110(4) -0.0354(4) 0.1835(3) 0.0250(6) Uani 1 1 d . . .
C32 C 0.6844(7) -0.0850(6) 0.4079(5) 0.0298(9) Uani 1 1 d . . .
H32A H 0.7926 -0.0285 0.3852 0.045 Uiso 1 1 calc R . .
H32B H 0.6527 -0.2023 0.4094 0.045 Uiso 1 1 calc R . .
H32C H 0.7226 -0.0209 0.5044 0.045 Uiso 1 1 calc R . .
O42 O 0.7452(5) 0.3195(4) 0.5035(4) 0.0287(7) Uani 1 1 d D . .
O41 O 0.0233(5) -0.3292(5) -0.3726(4) 0.0352(8) Uani 1 1 d D . .
H1A H 0.099(10) -0.380(5) -0.078(7) 0.050(7) Uiso 1 1 d D . .
H1B H 0.127(10) -0.284(9) -0.151(4) 0.050(7) Uiso 1 1 d D . .
H2A H 0.318(9) 0.033(9) -0.101(7) 0.050(7) Uiso 1 1 d D . .
H2B H 0.219(9) 0.084(8) -0.109(6) 0.050(7) Uiso 1 1 d D . .
H4A H 0.701(9) 0.263(8) 0.558(4) 0.050(7) Uiso 1 1 d D . .
H4B H 0.769(11) 0.375(8) 0.519(5) 0.050(7) Uiso 1 1 d D . .
H4C H -0.026(9) -0.425(7) -0.372(5) 0.050(7) Uiso 1 1 d D . .
H4D H 0.093(9) -0.302(7) -0.416(4) 0.050(7) Uiso 1 1 d D . .
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'
Y Y -2.7962 3.5667 '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
O1 Y1 O2 75.97(11) . . ?
O1 Y1 O11 84.05(12) . 2 ?
O2 Y1 O11 78.49(11) . 2 ?
O1 Y1 O31 97.53(12) . . ?
O2 Y1 O31 130.76(11) . . ?
O11 Y1 O31 150.36(10) 2 . ?
O1 Y1 O21 126.31(11) . . ?
O2 Y1 O21 144.43(10) . . ?
O11 Y1 O21 77.24(10) 2 . ?
O31 Y1 O21 78.16(10) . . ?
O1 Y1 O12 148.37(11) . . ?
O2 Y1 O12 84.04(12) . . ?
O11 Y1 O12 115.94(10) 2 . ?
O31 Y1 O12 77.21(12) . . ?
O21 Y1 O12 83.65(11) . . ?
O1 Y1 O22 73.58(11) . . ?
O2 Y1 O22 143.44(11) . . ?
O11 Y1 O22 78.70(11) 2 . ?
O31 Y1 O22 73.49(12) . . ?
O21 Y1 O22 53.67(10) . . ?
O12 Y1 O22 131.88(11) . . ?
O1 Y1 O32 77.17(13) . . ?
O2 Y1 O32 77.81(11) . . ?
O11 Y1 O32 152.66(10) 2 . ?
O31 Y1 O32 53.50(10) . . ?
O21 Y1 O32 130.01(10) . . ?
O12 Y1 O32 74.79(11) . . ?
O22 Y1 O32 113.93(11) . . ?
O1 Y1 O11 139.40(10) . . ?
O2 Y1 O11 73.37(10) . . ?
O11 Y1 O11 64.32(11) 2 . ?
O31 Y1 O11 122.66(11) . . ?
O21 Y1 O11 72.82(9) . . ?
O12 Y1 O11 51.62(9) . . ?
O22 Y1 O11 120.29(9) . . ?
O32 Y1 O11 120.51(10) . . ?
O1 Y1 C21 99.94(12) . . ?
O2 Y1 C21 154.40(12) . . ?
O11 Y1 C21 75.95(11) 2 . ?
O31 Y1 C21 74.63(12) . . ?
O21 Y1 C21 26.79(11) . . ?
O12 Y1 C21 108.36(12) . . ?
O22 Y1 C21 26.89(11) . . ?
O32 Y1 C21 126.51(11) . . ?
O11 Y1 C21 96.43(10) . . ?
O1 Y1 C31 87.58(13) . . ?
O2 Y1 C31 104.19(12) . . ?
O11 Y1 C31 170.32(10) 2 . ?
O31 Y1 C31 26.81(11) . . ?
O21 Y1 C31 104.10(11) . . ?
O12 Y1 C31 73.71(11) . . ?
O22 Y1 C31 94.30(12) . . ?
O32 Y1 C31 26.71(11) . . ?
O11 Y1 C31 125.33(11) . . ?
C21 Y1 C31 100.83(12) . . ?
O1 Y1 C11 153.44(11) . . ?
O2 Y1 C11 77.47(11) . . ?
O11 Y1 C11 90.42(11) 2 . ?
O31 Y1 C11 99.96(12) . . ?
O21 Y1 C11 77.11(10) . . ?
O12 Y1 C11 25.52(10) . . ?
O22 Y1 C11 130.76(10) . . ?
O32 Y1 C11 97.54(12) . . ?
O11 Y1 C11 26.10(10) . . ?
C21 Y1 C11 103.87(11) . . ?
C31 Y1 C11 99.23(12) . . ?
C11 O11 Y1 152.7(3) . 2 ?
C11 O11 Y1 91.6(2) . . ?
Y1 O11 Y1 115.68(11) 2 . ?
O12 C11 O11 119.0(3) . . ?
O12 C11 C12 120.7(4) . . ?
O11 C11 C12 120.3(4) . . ?
O12 C11 Y1 56.7(2) . . ?
O11 C11 Y1 62.3(2) . . ?
C12 C11 Y1 177.3(3) . . ?
C11 O12 Y1 97.8(2) . . ?
C21 O21 Y1 93.8(2) . . ?
O21 C21 O22 120.3(4) . . ?
O21 C21 C22 119.1(4) . . ?
O22 C21 C22 120.5(4) . . ?
O21 C21 Y1 59.4(2) . . ?
O22 C21 Y1 60.9(2) . . ?
C22 C21 Y1 176.8(3) . . ?
C21 O22 Y1 92.2(2) . . ?
C31 O31 Y1 95.3(3) . . ?
O32 C31 O31 118.9(4) . . ?
O32 C31 C32 121.2(4) . . ?
O31 C31 C32 119.9(4) . . ?
O32 C31 Y1 61.1(2) . . ?
O31 C31 Y1 57.9(2) . . ?
C32 C31 Y1 177.2(3) . . ?
C31 O32 Y1 92.2(2) . . ?
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
Y1 O1 2.312(3) . ?
Y1 O2 2.320(3) . ?
Y1 O11 2.335(3) 2 ?
Y1 O31 2.373(3) . ?
Y1 O21 2.405(3) . ?
Y1 O12 2.419(3) . ?
Y1 O22 2.439(3) . ?
Y1 O32 2.444(3) . ?
Y1 O11 2.541(3) . ?
Y1 C21 2.788(4) . ?
Y1 C31 2.789(4) . ?
Y1 C11 2.868(4) . ?
O11 C11 1.262(5) . ?
O11 Y1 2.335(3) 2 ?
C11 O12 1.247(5) . ?
C11 C12 1.484(5) . ?
O21 C21 1.259(5) . ?
C21 O22 1.262(5) . ?
C21 C22 1.492(6) . ?
O31 C31 1.263(5) . ?
C31 O32 1.254(5) . ?
C31 C32 1.499(6) . ?
