#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:44:50 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179672 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/25/4512539.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_4512539
loop_
_publ_author_name
'King, Nacole'
'Sommer, Roger D.'
'Watkins-Curry, Pilanda'
'Chan, Julia Y.'
'Maggard, Paul A.'
_publ_section_title
;
 Synthesis, Structure, and Thermal Instability of the Cu2Ta4O11Phase
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              552
_journal_paper_doi               10.1021/cg500987c
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         '0.17(Cu12 O66 Ta24)'
_chemical_formula_sum            'Cu2 O11 Ta4'
_chemical_formula_weight         1027.52
_chemical_name_common            'Copper (I) Tantalum (V) Oxide (2/4/11)'
_chemical_properties_physical    semiconductor
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_primary     direct
_audit_creation_date             2014-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   6.2190(2)
_cell_length_b                   6.2190(2)
_cell_length_c                   37.1067(11)
_cell_measurement_reflns_used    78
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      6.5427
_cell_measurement_theta_min      31.8702
_cell_volume                     1242.87(7)
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'ShelXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker-Nonius X8 Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            3079
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         3.294
_diffrn_source_type              'Bruker-Nonius X8 Apex2'
_exptl_absorpt_coefficient_mu    57.723
_exptl_absorpt_correction_T_max  0.25
_exptl_absorpt_correction_T_min  0.07
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    8.237
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2630
_exptl_crystal_size_max          0.069
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.033
_refine_diff_density_max         1.278
_refine_diff_density_min         -3.174
_refine_diff_density_rms         0.807
_refine_ls_extinction_coef       Fsqd
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.377
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.377
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0330P)²+66.6320P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                287
_reflns_number_total             287
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg500987c_si_002.cif
_cod_data_source_block           rds173
_cod_depositor_comments          'Adding full bibliography for 4512539.cif.'
_cod_original_cell_volume        1242.86(9)
_cod_database_code               4512539
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           2013-4
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.252
_shelx_estimated_absorpt_t_min   0.109
_olex2_refinement_description
;
Fixed Sof: Cu1(0.335)
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ta1 Ta 0.30407(10) 0.3333 0.5833 0.0155(3) Uani 1 2 d S T P
Ta2 Ta 0.0000 0.0000 0.5000 0.0276(4) Uani 1 6 d S T P
Cu1 Cu 0.5000 0.5000 0.5000 0.0279(7) Uani 0.67 2 d S T P
O1 O 0.3333 0.6667 0.5736(4) 0.019(3) Uani 1 3 d S T P
O2 O 0.2402(16) 0.2770(15) 0.5311(2) 0.0198(15) Uani 1 1 d . . .
O3 O 0.6667 0.5791(19) 0.5833 0.018(2) Uani 1 2 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 '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'
Ta Ta -0.7052 6.5227 '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
O1 Ta1 O1 129.97(7) 16_445 .
O1 Ta1 O3 64.98(4) 16_445 3_565
O1 Ta1 O3 64.98(4) . 3_565
O2 Ta1 O1 89.5(5) . 16_445
O2 Ta1 O1 89.5(4) 17 .
O2 Ta1 O1 85.1(4) 17 16_445
O2 Ta1 O1 85.1(4) . .
O2 Ta1 O2 167.1(5) . 17
O2 Ta1 O3 100.7(2) 17 2_655
O2 Ta1 O3 89.0(3) 17 .
O2 Ta1 O3 83.5(2) . 3_565
O2 Ta1 O3 89.0(2) . 2_655
O2 Ta1 O3 83.5(2) 17 3_565
O2 Ta1 O3 100.7(3) . .
O3 Ta1 O1 74.1(3) . .
O3 Ta1 O1 74.1(3) 2_655 16_445
O3 Ta1 O1 155.0(4) 2_655 .
O3 Ta1 O1 155.0(3) . 16_445
O3 Ta1 O3 83.2(7) 2_655 .
O3 Ta1 O3 138.4(3) . 3_565
O3 Ta1 O3 138.4(3) 2_655 3_565
Cu1 Ta2 Cu1 60.0 3 2_655
Cu1 Ta2 Cu1 60.0 . 2_655
Cu1 Ta2 Cu1 180.0 2_655 2
Cu1 Ta2 Cu1 120.0 . 2
Cu1 Ta2 Cu1 60.0 . 3_565
Cu1 Ta2 Cu1 120.0 1_445 2_655
Cu1 Ta2 Cu1 120.0 1_445 3_565
Cu1 Ta2 Cu1 60.0 1_445 2
Cu1 Ta2 Cu1 120.0 . 3
Cu1 Ta2 Cu1 60.0 3_565 2
Cu1 Ta2 Cu1 60.0 1_445 3
Cu1 Ta2 Cu1 120.0 3_565 2_655
Cu1 Ta2 Cu1 180.0 1_445 .
Cu1 Ta2 Cu1 180.0 3_565 3
Cu1 Ta2 Cu1 120.0 3 2
O2 Ta2 Cu1 143.9(2) 3 3_565
O2 Ta2 Cu1 36.1(2) 3 3
O2 Ta2 Cu1 60.7(2) 21_556 2
O2 Ta2 Cu1 60.7(2) . 3_565
O2 Ta2 Cu1 60.7(2) 20_556 .
O2 Ta2 Cu1 36.1(2) . .
O2 Ta2 Cu1 143.9(2) 21_556 3
O2 Ta2 Cu1 108.5(2) 21_556 1_445
O2 Ta2 Cu1 119.3(2) 20_556 1_445
O2 Ta2 Cu1 108.5(2) 2 3
O2 Ta2 Cu1 119.3(2) . 3
O2 Ta2 Cu1 108.5(2) . 2
O2 Ta2 Cu1 60.7(2) 19_556 3
O2 Ta2 Cu1 71.5(2) . 2_655
O2 Ta2 Cu1 60.7(2) 3 2_655
O2 Ta2 Cu1 108.5(2) 20_556 3_565
O2 Ta2 Cu1 143.9(2) . 1_445
O2 Ta2 Cu1 71.5(2) 20_556 3
O2 Ta2 Cu1 119.3(2) 2 .
O2 Ta2 Cu1 71.5(2) 21_556 .
O2 Ta2 Cu1 71.5(2) 19_556 2
O2 Ta2 Cu1 60.7(2) 2 1_445
O2 Ta2 Cu1 119.3(2) 3 2
O2 Ta2 Cu1 71.5(2) 2 3_565
O2 Ta2 Cu1 36.1(2) 2 2
O2 Ta2 Cu1 143.9(2) 19_556 .
O2 Ta2 Cu1 36.1(2) 19_556 1_445
O2 Ta2 Cu1 143.9(2) 20_556 2
O2 Ta2 Cu1 119.3(2) 21_556 2_655
O2 Ta2 Cu1 71.5(2) 3 1_445
O2 Ta2 Cu1 36.1(2) 21_556 3_565
O2 Ta2 Cu1 119.3(2) 19_556 3_565
O2 Ta2 Cu1 143.9(2) 2 2_655
O2 Ta2 Cu1 36.1(2) 20_556 2_655
O2 Ta2 Cu1 108.5(2) 3 .
O2 Ta2 Cu1 108.5(2) 19_556 2_655
O2 Ta2 O2 90.3(3) 19_556 3
O2 Ta2 O2 89.7(3) 21_556 20_556
O2 Ta2 O2 89.7(3) . 2
O2 Ta2 O2 89.7(3) 3 2
O2 Ta2 O2 90.3(3) 3 20_556
O2 Ta2 O2 89.7(3) . 3
O2 Ta2 O2 180.0(4) 21_556 3
O2 Ta2 O2 90.3(3) 21_556 2
O2 Ta2 O2 180.0 20_556 2
O2 Ta2 O2 180.0 . 19_556
O2 Ta2 O2 90.3(3) . 20_556
O2 Ta2 O2 90.3(3) . 21_556
O2 Ta2 O2 90.3(3) 19_556 2
O2 Ta2 O2 89.7(3) 19_556 20_556
O2 Ta2 O2 89.7(3) 19_556 21_556
Ta2 Cu1 Ta2 180.0 . 1_665
O2 Cu1 Ta2 142.0(2) . 1_665
O2 Cu1 Ta2 142.0(2) 19_666 .
O2 Cu1 Ta2 38.0(2) . .
O2 Cu1 Ta2 38.0(2) 19_666 1_665
O2 Cu1 O2 180.0(4) . 19_666
Ta1 O1 Ta1 116.9(2) 3_565 2_665
Ta1 O1 Ta1 116.9(2) 3_565 .
Ta1 O1 Ta1 116.9(2) 2_665 .
Ta1 O2 Ta2 136.1(4) . .
Cu1 O2 Ta1 116.4(4) . .
Cu1 O2 Ta2 105.9(4) . .
Ta1 O3 Ta1 101.6(3) 3_665 2_665
Ta1 O3 Ta1 101.6(3) . 2_665
Ta1 O3 Ta1 156.8(7) 3_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ta1 O1 2.021(2) .
Ta1 O1 2.021(2) 16_445
Ta1 O2 1.973(8) .
Ta1 O2 1.972(8) 17
Ta1 O3 1.994(3) .
Ta1 O3 1.994(2) 2_655
Ta1 O3 2.435(12) 3_565
Ta2 Cu1 3.10950(10) 1_445
Ta2 Cu1 3.10950(10) 2_655
Ta2 Cu1 3.10950(10) 2
Ta2 Cu1 3.10950(10) 3_565
Ta2 Cu1 3.10950(10) .
Ta2 Cu1 3.10950(10) 3
Ta2 O2 1.990(8) .
Ta2 O2 1.990(8) 3
Ta2 O2 1.990(8) 2
Ta2 O2 1.990(8) 21_556
Ta2 O2 1.990(8) 20_556
Ta2 O2 1.990(8) 19_556
Cu1 Ta2 3.10950(10) 1_665
Cu1 O2 1.905(8) 19_666
Cu1 O2 1.905(8) .
O1 Ta1 2.021(2) 3_565
O1 Ta1 2.021(2) 2_665
O3 Ta1 1.994(2) 3_665
O3 Ta1 2.435(12) 2_665
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_4
Ta2 Cu1 O2 Ta1 168.0(7) . .
Ta2 Cu1 O2 Ta1 -12.0(7) 1_665 .
Ta2 Cu1 O2 Ta2 180.0 1_665 .
Cu1 Ta2 O2 Ta1 -164.4(9) . .
Cu1 Ta2 O2 Ta1 15.6(9) 1_445 .
Cu1 Ta2 O2 Ta1 79.8(6) 2 .
Cu1 Ta2 O2 Ta1 117.2(7) 3_565 .
Cu1 Ta2 O2 Ta1 -62.8(7) 3 .
Cu1 Ta2 O2 Ta1 -100.2(6) 2_655 .
Cu1 Ta2 O2 Cu1 180.000(1) 1_445 .
Cu1 Ta2 O2 Cu1 101.7(3) 3 .
Cu1 Ta2 O2 Cu1 -78.3(3) 3_565 .
Cu1 Ta2 O2 Cu1 64.2(3) 2_655 .
Cu1 Ta2 O2 Cu1 -115.8(3) 2 .
O1 Ta1 O2 Ta2 -5.0(6) 16_445 .
O1 Ta1 O2 Ta2 -135.2(6) . .
O1 Ta1 O2 Cu1 -168.3(4) 16_445 .
O1 Ta1 O2 Cu1 61.5(4) . .
O1 Ta1 O3 Ta1 10.7(4) . 2_665
O1 Ta1 O3 Ta1 24.9(9) 16_445 3_665
O1 Ta1 O3 Ta1 -169.3(4) . 3_665
O1 Ta1 O3 Ta1 -155.1(9) 16_445 2_665
O2 Ta1 O2 Ta2 -69.9(6) 17 .
O2 Ta1 O2 Cu1 126.9(4) 17 .
O2 Ta1 O3 Ta1 100.9(2) 17 3_665
O2 Ta1 O3 Ta1 92.4(2) . 2_665
O2 Ta1 O3 Ta1 -87.6(2) . 3_665
O2 Ta1 O3 Ta1 -79.1(2) 17 2_665
O2 Ta2 O2 Ta1 48.4(4) 2 .
O2 Ta2 O2 Ta1 -131.6(4) 20_556 .
O2 Ta2 O2 Ta1 138.8(5) 21_556 .
O2 Ta2 O2 Ta1 -41.2(5) 3 .
O2 Ta2 O2 Cu1 -147.1(5) 2 .
O2 Ta2 O2 Cu1 -56.8(5) 21_556 .
O2 Ta2 O2 Cu1 32.9(5) 20_556 .
O2 Ta2 O2 Cu1 123.2(5) 3 .
O3 Ta1 O2 Ta2 -69.9(6) 3_565 .
O3 Ta1 O2 Ta2 69.1(7) 2_655 .
O3 Ta1 O2 Ta2 152.0(6) . .
O3 Ta1 O2 Cu1 -11.3(5) . .
O3 Ta1 O2 Cu1 -94.1(5) 2_655 .
O3 Ta1 O2 Cu1 126.9(4) 3_565 .
O3 Ta1 O3 Ta1 180.0 2_655 2_665
O3 Ta1 O3 Ta1 -179.992(0) 3_565 3_665
O3 Ta1 O3 Ta1 0.0 3_565 2_665
O3 Ta1 O3 Ta1 0.003(0) 2_655 3_665
