#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:25:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179140 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/01/4310151.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_4310151
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 H20 O13 Y2'
_chemical_formula_weight         550.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 115.94(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.857(3)
_cell_length_b                   16.469(3)
_cell_length_c                   8.3567(17)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10.5
_cell_volume                     1962.5(8)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  AED2
_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  0.0967
_diffrn_reflns_av_sigmaI/netI    0.0915
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6707
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '90 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.946
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .4
_refine_diff_density_max         1.404
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.203
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3436
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0832
_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)+(0.1560P)²+1.5600P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2119
_refine_ls_wR_factor_ref         0.2156
_reflns_number_gt                3294
_reflns_number_total             3436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0505192si20050826_111738_2.cif
_cod_data_source_block           Compound2
_cod_original_cell_volume        1962.4(7)
_cod_database_code               4310151
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'
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 -0.01169(7) -0.14630(5) -0.19625(12) 0.0136(3) Uani 1 1 d . . .
O1 O -0.0432(6) -0.0066(4) -0.2090(12) 0.0270(18) Uani 1 1 d . . .
H1A H -0.0016 0.0304 -0.2198 0.032 Uiso 1 1 calc R . .
H1B H -0.0973 0.0119 -0.2033 0.032 Uiso 1 1 calc R . .
Y2 Y -0.25956(4) -0.25796(6) -0.43411(7) 0.0165(3) Uani 1 1 d . . .
O21 O 0.0066(5) -0.1079(5) 0.1056(10) 0.0221(17) Uani 1 1 d . . .
C21 C 0.0826(7) -0.1429(6) 0.1819(14) 0.014(2) Uani 1 1 d . . .
C22 C 0.1245(9) -0.1623(9) 0.3798(18) 0.034(3) Uani 1 1 d . . .
H22A H 0.1872 -0.1412 0.4374 0.051 Uiso 1 1 calc R . .
H22B H 0.1259 -0.2201 0.3961 0.051 Uiso 1 1 calc R . .
H22C H 0.0870 -0.1378 0.4309 0.051 Uiso 1 1 calc R . .
O31 O 0.1085(5) -0.0757(5) -0.2229(11) 0.0218(17) Uani 1 1 d . . .
C31 C 0.1939(7) -0.0810(6) -0.1882(15) 0.020(2) Uani 1 1 d . . .
O32 O 0.2490(6) -0.1345(5) -0.0891(13) 0.0271(19) Uani 1 1 d . . .
C32 C 0.2351(11) -0.0185(9) -0.268(2) 0.037(3) Uani 1 1 d . . .
H32A H 0.2808 -0.0441 -0.2976 0.056 Uiso 1 1 calc R . .
H32B H 0.2646 0.0240 -0.1829 0.056 Uiso 1 1 calc R . .
H32C H 0.1860 0.0041 -0.3734 0.056 Uiso 1 1 calc R . .
O41 O 0.0894(6) -0.2471(5) -0.2197(11) 0.0232(18) Uani 1 1 d . . .
C41 C 0.1089(9) -0.3191(7) -0.2429(16) 0.025(3) Uani 1 1 d . . .
C42 C 0.0405(13) -0.3675(11) -0.394(3) 0.068(6) Uani 1 1 d . . .
H42A H 0.0735 -0.4000 -0.4439 0.102 Uiso 1 1 calc R . .
H42B H -0.0018 -0.3316 -0.4839 0.102 Uiso 1 1 calc R . .
H42C H 0.0056 -0.4023 -0.3527 0.102 Uiso 1 1 calc R . .
O42 O 0.1863(7) -0.3496(5) -0.1421(14) 0.034(2) Uani 1 1 d . . .
O51 O -0.1220(6) -0.2300(5) -0.4601(12) 0.0226(18) Uani 1 1 d . . .
C51 C -0.1107(8) -0.1798(7) -0.5655(15) 0.020(2) Uani 1 1 d . . .
O52 O -0.0652(6) -0.1171(5) -0.5074(11) 0.0247(17) Uani 1 1 d . . .
C52 C -0.1537(11) -0.1991(10) -0.7623(17) 0.041(4) Uani 1 1 d . . .
H52A H -0.2030 -0.1610 -0.8256 0.062 Uiso 1 1 calc R . .
H52B H -0.1790 -0.2531 -0.7815 0.062 Uiso 1 1 calc R . .
H52C H -0.1065 -0.1954 -0.8045 0.062 Uiso 1 1 calc R . .
O61 O -0.0309(6) -0.2647(5) -0.0595(13) 0.029(2) Uani 1 1 d . . .
C61 C -0.0852(7) -0.3210(7) -0.0694(13) 0.019(2) Uani 1 1 d . . .
O62 O -0.1689(6) -0.3268(5) -0.1817(12) 0.0272(18) Uani 1 1 d . . .
C62 C -0.0477(11) -0.3874(11) 0.067(2) 0.055(5) Uani 1 1 d . . .
H62A H -0.0766 -0.4380 0.0147 0.082 Uiso 1 1 calc R . .
H62B H -0.0614 -0.3750 0.1655 0.082 Uiso 1 1 calc R . .
H62C H 0.0190 -0.3915 0.1086 0.082 Uiso 1 1 calc R . .
O71 O -0.1712(6) -0.1417(4) -0.2474(12) 0.0211(17) Uani 1 1 d . . .
C71 C -0.2407(8) -0.1198(7) -0.2202(15) 0.021(2) Uani 1 1 d . . .
O72 O -0.3119(6) -0.1659(6) -0.2709(14) 0.033(2) Uani 1 1 d . . .
C72 C -0.2411(10) -0.0404(9) -0.136(2) 0.037(3) Uani 1 1 d . . .
H72A H -0.1847 -0.0350 -0.0276 0.055 Uiso 1 1 calc R . .
H72B H -0.2945 -0.0375 -0.1109 0.055 Uiso 1 1 calc R . .
H72C H -0.2444 0.0028 -0.2161 0.055 Uiso 1 1 calc R . .
O22 O 0.1262(5) -0.1646(5) 0.0919(11) 0.0189(16) Uani 1 1 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
O31 Y1 O61 138.5(3) . . ?
O31 Y1 O1 70.9(3) . . ?
O61 Y1 O1 140.0(3) . . ?
O31 Y1 O41 74.4(3) . . ?
O61 Y1 O41 72.3(3) . . ?
O1 Y1 O41 145.1(3) . . ?
O31 Y1 O71 145.1(3) . . ?
O61 Y1 O71 76.0(3) . . ?
O1 Y1 O71 76.8(3) . . ?
O41 Y1 O71 135.4(3) . . ?
O31 Y1 O52 73.3(3) . . ?
O61 Y1 O52 129.3(3) . . ?
O1 Y1 O52 77.7(3) . . ?
O41 Y1 O52 89.0(3) . . ?
O71 Y1 O52 87.4(3) . . ?
O31 Y1 O22 74.9(3) . . ?
O61 Y1 O22 70.8(3) . . ?
O1 Y1 O22 104.2(3) . . ?
O41 Y1 O22 69.7(3) . . ?
O71 Y1 O22 126.9(3) . . ?
O52 Y1 O22 145.5(3) . . ?
O31 Y1 O21 103.5(3) . . ?
O61 Y1 O21 72.6(3) . . ?
O1 Y1 O21 74.0(3) . . ?
O41 Y1 O21 118.5(3) . . ?
O71 Y1 O21 79.5(3) . . ?
O52 Y1 O21 150.9(3) . . ?
O22 Y1 O21 51.7(2) . . ?
O31 Y1 O51 118.1(3) . . ?
O61 Y1 O51 77.6(3) . . ?
O1 Y1 O51 116.2(3) . . ?
O41 Y1 O51 77.4(3) . . ?
O71 Y1 O51 65.6(3) . . ?
O52 Y1 O51 52.2(3) . . ?
O22 Y1 O51 139.7(3) . . ?
O21 Y1 O51 138.4(3) . . ?
O31 Y1 C51 94.6(3) . . ?
O61 Y1 C51 103.9(3) . . ?
O1 Y1 C51 97.8(3) . . ?
O41 Y1 C51 81.2(3) . . ?
O71 Y1 C51 76.8(3) . . ?
O52 Y1 C51 25.5(3) . . ?
O22 Y1 C51 150.7(3) . . ?
O21 Y1 C51 156.1(3) . . ?
O51 Y1 C51 26.7(3) . . ?
O31 Y1 C21 92.4(3) . . ?
O61 Y1 C21 65.9(3) . . ?
O1 Y1 C21 91.7(3) . . ?
O41 Y1 C21 93.4(3) . . ?
O71 Y1 C21 101.5(3) . . ?
O52 Y1 C21 164.3(3) . . ?
O22 Y1 C21 26.6(3) . . ?
O21 Y1 C21 25.6(3) . . ?
O51 Y1 C21 143.4(3) . . ?
C51 Y1 C21 169.6(3) . . ?
O31 Y1 Y2 65.14(19) . 4_545 ?
O61 Y1 Y2 73.4(2) . 4_545 ?
O1 Y1 Y2 124.1(2) . 4_545 ?
O41 Y1 Y2 37.9(2) . 4_545 ?
O71 Y1 Y2 148.5(2) . 4_545 ?
O52 Y1 Y2 118.2(2) . 4_545 ?
O22 Y1 Y2 32.71(18) . 4_545 ?
O21 Y1 Y2 84.18(18) . 4_545 ?
O51 Y1 Y2 114.2(2) . 4_545 ?
C51 Y1 Y2 118.0(2) . 4_545 ?
C21 Y1 Y2 58.6(2) . 4_545 ?
O32 Y2 O62 88.2(3) 4_444 . ?
O32 Y2 O22 82.2(3) 4_444 4_444 ?
O62 Y2 O22 80.8(3) . 4_444 ?
O32 Y2 O51 78.8(3) 4_444 . ?
O62 Y2 O51 87.0(3) . . ?
O22 Y2 O51 157.7(3) 4_444 . ?
O32 Y2 O42 105.2(4) 4_444 4_444 ?
O62 Y2 O42 159.4(3) . 4_444 ?
O22 Y2 O42 115.9(3) 4_444 4_444 ?
O51 Y2 O42 80.6(4) . 4_444 ?
O32 Y2 O72 161.5(3) 4_444 . ?
O62 Y2 O72 91.3(3) . . ?
O22 Y2 O72 79.4(3) 4_444 . ?
O51 Y2 O72 119.7(3) . . ?
O42 Y2 O72 80.9(4) 4_444 . ?
O32 Y2 O71 144.7(3) 4_444 . ?
O62 Y2 O71 81.2(3) . . ?
O22 Y2 O71 128.3(3) 4_444 . ?
O51 Y2 O71 67.2(3) . . ?
O42 Y2 O71 78.9(3) 4_444 . ?
O72 Y2 O71 53.1(3) . . ?
O32 Y2 O41 75.7(3) 4_444 4_444 ?
O62 Y2 O41 147.6(3) . 4_444 ?
O22 Y2 O41 69.5(3) 4_444 4_444 ?
O51 Y2 O41 116.3(3) . 4_444 ?
O42 Y2 O41 52.7(3) 4_444 4_444 ?
O72 Y2 O41 95.4(3) . 4_444 ?
O71 Y2 O41 127.4(3) . 4_444 ?
O32 Y2 C41 92.0(3) 4_444 4_444 ?
O62 Y2 C41 172.9(3) . 4_444 ?
O22 Y2 C41 92.2(3) 4_444 4_444 ?
O51 Y2 C41 100.0(3) . 4_444 ?
O42 Y2 C41 26.2(3) 4_444 4_444 ?
O72 Y2 C41 86.3(4) . 4_444 ?
O71 Y2 C41 102.5(3) . 4_444 ?
O41 Y2 C41 26.6(3) 4_444 4_444 ?
O32 Y2 C71 171.3(3) 4_444 . ?
O62 Y2 C71 88.0(3) . . ?
O22 Y2 C71 104.8(3) 4_444 . ?
O51 Y2 C71 93.2(3) . . ?
O42 Y2 C71 76.5(3) 4_444 . ?
O72 Y2 C71 26.6(3) . . ?
O71 Y2 C71 26.7(3) . . ?
O41 Y2 C71 111.3(3) 4_444 . ?
C41 Y2 C71 92.7(3) 4_444 . ?
O32 Y2 Y1 70.4(2) 4_444 4_444 ?
O62 Y2 Y1 113.1(2) . 4_444 ?
O22 Y2 Y1 35.3(2) 4_444 4_444 ?
O51 Y2 Y1 142.1(2) . 4_444 ?
O42 Y2 Y1 86.4(2) 4_444 4_444 ?
O72 Y2 Y1 92.8(2) . 4_444 ?
O71 Y2 Y1 144.39(18) . 4_444 ?
O41 Y2 Y1 35.09(17) 4_444 4_444 ?
C41 Y2 Y1 60.5(3) 4_444 4_444 ?
C71 Y2 Y1 118.2(2) . 4_444 ?
O32 Y2 Y1 111.0(2) 4_444 . ?
O62 Y2 Y1 71.4(2) . . ?
O22 Y2 Y1 148.4(2) 4_444 . ?
O51 Y2 Y1 36.7(2) . . ?
O42 Y2 Y1 89.0(2) 4_444 . ?
O72 Y2 Y1 86.4(2) . . ?
O71 Y2 Y1 33.83(18) . . ?
O41 Y2 Y1 140.49(18) 4_444 . ?
C41 Y2 Y1 115.0(3) 4_444 . ?
C71 Y2 Y1 60.4(2) . . ?
Y1 Y2 Y1 175.42(3) 4_444 . ?
C21 O21 Y1 93.4(6) . . ?
O21 C21 O22 119.0(9) . . ?
O21 C21 C22 121.6(9) . . ?
O22 C21 C22 119.3(9) . . ?
O21 C21 Y1 61.0(5) . . ?
O22 C21 Y1 59.8(5) . . ?
C22 C21 Y1 166.1(8) . . ?
C31 O31 Y1 142.0(7) . . ?
O31 C31 O32 124.5(10) . . ?
O31 C31 C32 118.5(10) . . ?
O32 C31 C32 116.9(10) . . ?
C31 O32 Y2 137.2(7) . 4_545 ?
C41 O41 Y1 152.9(8) . . ?
C41 O41 Y2 88.9(7) . 4_545 ?
Y1 O41 Y2 107.0(3) . 4_545 ?
O42 C41 O41 120.6(11) . . ?
O42 C41 C42 119.6(12) . . ?
O41 C41 C42 119.8(12) . . ?
O42 C41 Y2 56.5(6) . 4_545 ?
O41 C41 Y2 64.4(7) . 4_545 ?
C42 C41 Y2 173.9(12) . 4_545 ?
C41 O42 Y2 97.3(7) . 4_545 ?
C51 O51 Y2 127.7(7) . . ?
C51 O51 Y1 89.8(7) . . ?
Y2 O51 Y1 110.1(3) . . ?
O52 C51 O51 120.4(10) . . ?
O52 C51 C52 120.8(10) . . ?
O51 C51 C52 118.8(10) . . ?
O52 C51 Y1 57.2(5) . . ?
O51 C51 Y1 63.5(6) . . ?
C52 C51 Y1 174.1(8) . . ?
C51 O52 Y1 97.3(6) . . ?
C61 O61 Y1 145.2(7) . . ?
O61 C61 O62 125.8(10) . . ?
O61 C61 C62 117.3(10) . . ?
O62 C61 C62 116.9(11) . . ?
C61 O62 Y2 133.9(8) . . ?
C71 O71 Y1 156.3(8) . . ?
C71 O71 Y2 92.1(7) . . ?
Y1 O71 Y2 110.6(3) . . ?
O72 C71 O71 119.0(10) . . ?
O72 C71 C72 119.8(11) . . ?
O71 C71 C72 121.1(11) . . ?
O72 C71 Y2 58.4(6) . . ?
O71 C71 Y2 61.2(6) . . ?
C72 C71 Y2 170.4(9) . . ?
C71 O72 Y2 95.1(7) . . ?
C21 O22 Y2 149.6(7) . 4_545 ?
C21 O22 Y1 93.6(6) . . ?
Y2 O22 Y1 112.0(3) 4_545 . ?
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 O31 2.326(8) . ?
Y1 O61 2.347(8) . ?
Y1 O1 2.348(7) . ?
Y1 O41 2.375(8) . ?
Y1 O71 2.376(8) . ?
Y1 O52 2.405(8) . ?
Y1 O22 2.462(8) . ?
Y1 O21 2.492(8) . ?
Y1 O51 2.539(9) . ?
Y1 C51 2.838(11) . ?
Y1 C21 2.845(11) . ?
Y1 Y2 3.9503(17) 4_545 ?
Y2 O32 2.233(8) 4_444 ?
Y2 O62 2.269(8) . ?
Y2 O22 2.302(8) 4_444 ?
Y2 O51 2.331(8) . ?
Y2 O42 2.364(9) 4_444 ?
Y2 O72 2.417(9) . ?
Y2 O71 2.480(8) . ?
Y2 O41 2.537(8) 4_444 ?
Y2 C41 2.812(12) 4_444 ?
Y2 C71 2.827(12) . ?
Y2 Y1 3.9503(17) 4_444 ?
O21 C21 1.232(14) . ?
C21 O22 1.276(13) . ?
C21 C22 1.522(17) . ?
O31 C31 1.257(13) . ?
C31 O32 1.262(13) . ?
C31 C32 1.520(17) . ?
O32 Y2 2.233(8) 4_545 ?
O41 C41 1.261(15) . ?
O41 Y2 2.537(8) 4_545 ?
C41 O42 1.250(15) . ?
C41 C42 1.488(19) . ?
C41 Y2 2.812(12) 4_545 ?
O42 Y2 2.364(9) 4_545 ?
O51 C51 1.276(14) . ?
C51 O52 1.232(14) . ?
C51 C52 1.513(16) . ?
O61 C61 1.242(14) . ?
C61 O62 1.250(13) . ?
C61 C62 1.503(18) . ?
O71 C71 1.271(14) . ?
C71 O72 1.269(15) . ?
C71 C72 1.486(17) . ?
O22 Y2 2.302(8) 4_545 ?
