#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:42:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179124 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/86/4308688.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_4308688
loop_
_publ_author_name
'Timothy J. Boyle'
'Scott D. Bunge'
'Paul G. Clem'
'Jacob Richardson'
'Jeffrey T. Dawley'
'Leigh Anna M. Ottley'
'Mark A. Rodriguez'
'Bruce A. Tuttle'
'Gabriel R. Avilucea'
'Ralph G. Tissot'
_publ_section_title
;
Synthesis and Characterization of a Family of Structurally Characterized
Dysprosium Alkoxides for Improved Fatigue-Resistance Characteristics of
PDyZT Thin Films
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1588
_journal_page_last               1600
_journal_paper_doi               10.1021/ic048550b
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C67 H140 Dy4 O12'
_chemical_formula_weight         1787.79
_chemical_name_common            '(1) [Dy4(ONep)12]*(tol)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.324(5)
_cell_length_b                   20.324(5)
_cell_length_c                   11.976(4)
_cell_measurement_temperature    293(2)
_cell_volume                     4947(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            30539
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    3.026
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          .040
_exptl_crystal_size_mid          .106
_exptl_crystal_size_min          .167
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0417P)²+2.9024P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                3189
_reflns_number_total             3567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048550bsi20041015_025718_01.cif
_cod_data_source_block           tjb144ss
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4308688
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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
Dy1 Dy 0.098584(11) 0.923836(11) 0.50226(3) 0.03477(11) Uani 1 1 d . . .
O1 O 0.1216(2) 1.0163(3) 0.3980(4) 0.0401(14) Uani 1 1 d . . .
O2 O 0.0930(2) 1.0127(2) 0.6137(3) 0.0365(12) Uani 1 1 d . . .
O3 O 0.18286(16) 0.86854(16) 0.5030(6) 0.0440(8) Uani 1 1 d . . .
C1 C 0.1607(3) 0.9979(3) 0.3046(5) 0.0418(16) Uani 1 1 d . . .
H1A H 0.1353 1.0050 0.2371 0.050 Uiso 1 1 calc R . .
H1B H 0.1703 0.9513 0.3096 0.050 Uiso 1 1 calc R . .
C2 C 0.2253(3) 1.0354(3) 0.2949(5) 0.0442(16) Uani 1 1 d . . .
C3 C 0.2638(4) 1.0303(4) 0.4024(6) 0.061(2) Uani 1 1 d . . .
H3A H 0.2393 1.0505 0.4618 0.091 Uiso 1 1 calc R . .
H3B H 0.3052 1.0524 0.3939 0.091 Uiso 1 1 calc R . .
H3C H 0.2712 0.9848 0.4197 0.091 Uiso 1 1 calc R . .
C4 C 0.2652(4) 1.0016(4) 0.2013(6) 0.066(2) Uani 1 1 d . . .
H4A H 0.2698 0.9556 0.2179 0.100 Uiso 1 1 calc R . .
H4B H 0.3080 1.0214 0.1964 0.100 Uiso 1 1 calc R . .
H4C H 0.2427 1.0068 0.1314 0.100 Uiso 1 1 calc R . .
C5 C 0.2105(4) 1.1056(4) 0.2649(6) 0.059(2) Uani 1 1 d . . .
H5A H 0.1850 1.1068 0.1975 0.089 Uiso 1 1 calc R . .
H5B H 0.2510 1.1290 0.2538 0.089 Uiso 1 1 calc R . .
H5C H 0.1861 1.1258 0.3243 0.089 Uiso 1 1 calc R . .
C6 C 0.2451(3) 0.8454(3) 0.5309(5) 0.051(2) Uani 1 1 d . . .
H6A H 0.2453 0.8348 0.6099 0.062 Uiso 1 1 calc R . .
H6B H 0.2765 0.8806 0.5194 0.062 Uiso 1 1 calc R . .
C7 C 0.2684(3) 0.7853(3) 0.4666(5) 0.051(2) Uani 1 1 d . . .
C8 C 0.2215(4) 0.7291(3) 0.4892(10) 0.082(3) Uani 1 1 d . . .
H8A H 0.1771 0.7438 0.4785 0.123 Uiso 1 1 calc R . .
H8B H 0.2270 0.7142 0.5648 0.123 Uiso 1 1 calc R . .
H8C H 0.2307 0.6935 0.4388 0.123 Uiso 1 1 calc R . .
C9 C 0.3367(3) 0.7649(4) 0.5115(8) 0.071(2) Uani 1 1 d . . .
H9A H 0.3330 0.7534 0.5890 0.106 Uiso 1 1 calc R . .
H9B H 0.3669 0.8008 0.5033 0.106 Uiso 1 1 calc R . .
H9C H 0.3525 0.7276 0.4701 0.106 Uiso 1 1 calc R . .
C10 C 0.2695(4) 0.8008(4) 0.3419(5) 0.072(2) Uani 1 1 d . . .
H10A H 0.2855 0.7632 0.3016 0.108 Uiso 1 1 calc R . .
H10B H 0.2980 0.8376 0.3285 0.108 Uiso 1 1 calc R . .
H10C H 0.2258 0.8112 0.3172 0.108 Uiso 1 1 calc R . .
C11 C 0.0880(3) 1.0039(3) 0.7315(5) 0.0425(16) Uani 1 1 d . . .
H11A H 0.0732 0.9594 0.7461 0.051 Uiso 1 1 calc R . .
H11B H 0.0547 1.0337 0.7599 0.051 Uiso 1 1 calc R . .
C12 C 0.1510(3) 1.0155(3) 0.7953(6) 0.0488(18) Uani 1 1 d . . .
C13 C 0.1698(4) 1.0874(4) 0.7844(8) 0.077(3) Uani 1 1 d . . .
H13A H 0.1656 1.1009 0.7079 0.115 Uiso 1 1 calc R . .
H13B H 0.2146 1.0933 0.8083 0.115 Uiso 1 1 calc R . .
H13C H 0.1413 1.1136 0.8303 0.115 Uiso 1 1 calc R . .
C14 C 0.1385(5) 1.0009(5) 0.9170(6) 0.081(3) Uani 1 1 d . . .
H14A H 0.1006 1.0252 0.9417 0.121 Uiso 1 1 calc R . .
H14B H 0.1761 1.0136 0.9602 0.121 Uiso 1 1 calc R . .
H14C H 0.1306 0.9547 0.9263 0.121 Uiso 1 1 calc R . .
C15 C 0.2045(3) 0.9694(4) 0.7501(6) 0.0551(19) Uani 1 1 d . . .
H15A H 0.1899 0.9246 0.7561 0.083 Uiso 1 1 calc R . .
H15B H 0.2441 0.9750 0.7927 0.083 Uiso 1 1 calc R . .
H15C H 0.2130 0.9796 0.6732 0.083 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'
Dy Dy -0.1892 4.4098 '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
O3 Dy1 O2 118.7(2) . . ?
O3 Dy1 O1 113.2(2) . 3_466 ?
O2 Dy1 O1 88.70(19) . 3_466 ?
O3 Dy1 O2 124.5(2) . 3_466 ?
O2 Dy1 O2 116.6(2) . 3_466 ?
O1 Dy1 O2 71.92(15) 3_466 3_466 ?
O3 Dy1 O1 106.26(19) . . ?
O2 Dy1 O1 71.14(14) . . ?
O1 Dy1 O1 140.5(2) 3_466 . ?
O2 Dy1 O1 86.98(19) 3_466 . ?
O3 Dy1 Dy1 139.41(10) . 3_466 ?
O2 Dy1 Dy1 93.51(12) . 3_466 ?
O1 Dy1 Dy1 38.69(12) 3_466 3_466 ?
O2 Dy1 Dy1 37.29(11) 3_466 3_466 ?
O1 Dy1 Dy1 107.28(13) . 3_466 ?
O3 Dy1 Dy1 130.58(10) . 4_666 ?
O2 Dy1 Dy1 37.44(11) . 4_666 ?
O1 Dy1 Dy1 108.66(12) 3_466 4_666 ?
O2 Dy1 Dy1 92.46(12) 3_466 4_666 ?
O1 Dy1 Dy1 37.71(12) . 4_666 ?
Dy1 Dy1 Dy1 89.987(1) 3_466 4_666 ?
C1 O1 Dy1 147.2(4) . 4_666 ?
C1 O1 Dy1 109.0(4) . . ?
Dy1 O1 Dy1 103.61(17) 4_666 . ?
C11 O2 Dy1 119.3(4) . . ?
C11 O2 Dy1 134.1(4) . 4_666 ?
Dy1 O2 Dy1 105.27(17) . 4_666 ?
C6 O3 Dy1 161.3(5) . . ?
O1 C1 C2 114.2(5) . . ?
C5 C2 C3 111.9(6) . . ?
C5 C2 C1 108.8(6) . . ?
C3 C2 C1 110.3(5) . . ?
C5 C2 C4 110.7(6) . . ?
C3 C2 C4 108.4(6) . . ?
C1 C2 C4 106.6(6) . . ?
O3 C6 C7 115.7(6) . . ?
C8 C7 C6 108.6(5) . . ?
C8 C7 C10 109.9(7) . . ?
C6 C7 C10 109.7(6) . . ?
C8 C7 C9 107.4(6) . . ?
C6 C7 C9 108.7(6) . . ?
C10 C7 C9 112.5(6) . . ?
O2 C11 C12 114.9(5) . . ?
C14 C12 C11 108.3(6) . . ?
C14 C12 C13 108.3(7) . . ?
C11 C12 C13 108.7(6) . . ?
C14 C12 C15 109.9(6) . . ?
C11 C12 C15 109.1(5) . . ?
C13 C12 C15 112.3(7) . . ?
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
Dy1 O3 2.049(3) . ?
Dy1 O2 2.249(4) . ?
Dy1 O1 2.253(5) 3_466 ?
Dy1 O2 2.257(5) 3_466 ?
Dy1 O1 2.303(5) . ?
Dy1 Dy1 3.5812(8) 3_466 ?
Dy1 Dy1 3.5812(9) 4_666 ?
O1 C1 1.422(7) . ?
O1 Dy1 2.253(5) 4_666 ?
O2 C11 1.426(7) . ?
O2 Dy1 2.257(5) 4_666 ?
O3 C6 1.390(7) . ?
C1 C2 1.522(9) . ?
C2 C5 1.500(9) . ?
C2 C3 1.510(9) . ?
C2 C4 1.546(9) . ?
C6 C7 1.519(9) . ?
C7 C8 1.513(9) . ?
C7 C10 1.525(9) . ?
C7 C9 1.545(9) . ?
C11 C12 1.509(9) . ?
C12 C14 1.509(10) . ?
C12 C13 1.517(10) . ?
C12 C15 1.533(10) . ?
