#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:02:38 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179610 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/74/4507439.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_4507439
loop_
_publ_author_name
'Choi, Jonglak'
'King, Nacole'
'Maggard, Paul A.'
_publ_section_title
;
 Metastable cu(i)-niobate semiconductor with a low-temperature,
 nanoparticle-mediated synthesis.
;
_journal_issue                   2
_journal_name_full               'ACS nano'
_journal_page_first              1699
_journal_page_last               1708
_journal_paper_doi               10.1021/nn305707f
_journal_volume                  7
_journal_year                    2013
_chemical_formula_moiety         Cu2Nb8O21
_chemical_formula_sum            'Cu2 Nb8 O21'
_chemical_formula_weight         1206.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.2120(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5325(2)
_cell_length_b                   6.43060(10)
_cell_length_c                   10.1730(2)
_cell_measurement_reflns_used    2420
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      41.27
_cell_measurement_theta_min      2.03
_cell_volume                     678.11(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       'Omega scan b/P/b'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2420
_diffrn_reflns_theta_full        41.27
_diffrn_reflns_theta_max         41.27
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    9.698
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   'numerical from crystal shape'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    5.908
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle-plate
_exptl_crystal_F_000             1108.0
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.809
_refine_diff_density_min         -2.026
_refine_diff_density_rms         0.399
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         2420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0368P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0738
_reflns_number_gt                3385
_reflns_number_total             2420
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nn305707f_si_002.cif
_cod_data_source_block           cj3-7_c(wt)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4507439
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Nb1 Nb 0.24394(3) 0.0000 0.43480(3) 0.00624(5) Uani 1 2 d S
Nb2 Nb -0.30059(3) 0.0000 0.22784(3) 0.00566(5) Uani 1 2 d S
Nb3 Nb 0.00190(3) 0.0000 0.18547(3) 0.00611(6) Uani 1 2 d S
Nb4 Nb 0.37966(3) 0.0000 0.16619(3) 0.00573(6) Uani 1 2 d S
Cu1 Cu 0.5000 0.25022(8) 0.5000 0.01458(9) Uani 1 2 d S
O1 O 0.0512(3) 0.0000 0.3878(3) 0.0076(4) Uani 1 2 d S
O2 O 0.4100(3) 0.0000 0.3886(3) 0.0085(4) Uani 1 2 d S
O3 O 0.0000 0.0000 0.0000 0.0108(7) Uani 1 4 d S
O4 O -0.15832(18) -0.1839(3) 0.18690(18) 0.0080(3) Uani 1 1 d .
O5 O 0.2702(2) 0.1801(3) 0.60658(18) 0.0086(3) Uani 1 1 d .
O6 O -0.3365(3) 0.0000 0.0096(2) 0.0086(4) Uani 1 2 d S
O7 O 0.2023(3) 0.0000 0.2237(3) 0.0075(4) Uani 1 2 d S
O8 O 0.04682(18) 0.3139(3) 0.18716(18) 0.0080(3) 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
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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
O2 Nb1 O1 152.25(11) . .
O2 Nb1 O5 102.61(9) . .
O1 Nb1 O5 100.33(8) . .
O2 Nb1 O5 102.61(9) . 6
O1 Nb1 O5 100.33(8) . 6
O5 Nb1 O5 67.91(10) . 6
O2 Nb1 O5 89.20(6) . 7_556
O1 Nb1 O5 85.37(6) . 7_556
O5 Nb1 O5 67.41(8) . 7_556
O5 Nb1 O5 135.26(6) 6 7_556
O2 Nb1 O5 89.20(6) . 4_546
O1 Nb1 O5 85.36(6) . 4_546
O5 Nb1 O5 135.26(6) . 4_546
O5 Nb1 O5 67.41(8) 6 4_546
O5 Nb1 O5 156.87(10) 7_556 4_546
O2 Nb1 O7 77.41(11) . .
O1 Nb1 O7 74.84(10) . .
O5 Nb1 O7 145.95(5) . .
O5 Nb1 O7 145.95(5) 6 .
O5 Nb1 O7 78.57(5) 7_556 .
O5 Nb1 O7 78.57(5) 4_546 .
O2 Nb1 Cu1 41.15(5) . .
O1 Nb1 Cu1 148.831(9) . .
O5 Nb1 Cu1 63.26(6) . .
O5 Nb1 Cu1 97.36(5) 6 .
O5 Nb1 Cu1 64.14(6) 7_556 .
O5 Nb1 Cu1 125.30(6) 4_546 .
O7 Nb1 Cu1 103.45(6) . .
O2 Nb1 Cu1 41.15(5) . 5_656
O1 Nb1 Cu1 148.831(9) . 5_656
O5 Nb1 Cu1 97.36(5) . 5_656
O5 Nb1 Cu1 63.26(6) 6 5_656
O5 Nb1 Cu1 125.30(6) 7_556 5_656
O5 Nb1 Cu1 64.14(6) 4_546 5_656
O7 Nb1 Cu1 103.45(6) . 5_656
Cu1 Nb1 Cu1 62.328(18) . 5_656
O2 Nb1 Cu1 149.844(9) . 3_445
O1 Nb1 Cu1 39.76(5) . 3_445
O5 Nb1 Cu1 95.61(6) . 3_445
O5 Nb1 Cu1 62.40(6) 6 3_445
O5 Nb1 Cu1 120.17(6) 7_556 3_445
O5 Nb1 Cu1 61.21(6) 4_546 3_445
O7 Nb1 Cu1 100.43(6) . 3_445
Cu1 Nb1 Cu1 156.079(11) . 3_445
Cu1 Nb1 Cu1 113.218(4) 5_656 3_445
O2 Nb1 Cu1 149.844(9) . 7_556
O1 Nb1 Cu1 39.76(5) . 7_556
O5 Nb1 Cu1 62.40(6) . 7_556
O5 Nb1 Cu1 95.61(6) 6 7_556
O5 Nb1 Cu1 61.21(6) 7_556 7_556
O5 Nb1 Cu1 120.17(6) 4_546 7_556
O7 Nb1 Cu1 100.43(6) . 7_556
Cu1 Nb1 Cu1 113.218(4) . 7_556
Cu1 Nb1 Cu1 156.079(11) 5_656 7_556
Cu1 Nb1 Cu1 60.305(17) 3_445 7_556
O2 Nb1 Nb3 115.91(8) . .
O1 Nb1 Nb3 36.34(7) . .
O5 Nb1 Nb3 128.64(5) . .
O5 Nb1 Nb3 128.64(5) 6 .
O5 Nb1 Nb3 79.99(5) 7_556 .
O5 Nb1 Nb3 79.99(5) 4_546 .
O7 Nb1 Nb3 38.50(7) . .
Cu1 Nb1 Nb3 133.997(10) . .
Cu1 Nb1 Nb3 133.997(10) 5_656 .
Cu1 Nb1 Nb3 67.378(8) 3_445 .
Cu1 Nb1 Nb3 67.378(8) 7_556 .
O8 Nb2 O8 74.03(11) 3_445 8_455
O8 Nb2 O4 156.39(8) 3_445 6
O8 Nb2 O4 101.99(8) 8_455 6
O8 Nb2 O4 101.99(8) 3_445 .
O8 Nb2 O4 156.39(8) 8_455 .
O4 Nb2 O4 72.10(11) 6 .
O8 Nb2 O5 121.39(8) 3_445 2_556
O8 Nb2 O5 80.29(8) 8_455 2_556
O4 Nb2 O5 79.74(8) 6 2_556
O4 Nb2 O5 119.73(8) . 2_556
O8 Nb2 O5 80.29(8) 3_445 5_556
O8 Nb2 O5 121.39(8) 8_455 5_556
O4 Nb2 O5 119.73(8) 6 5_556
O4 Nb2 O5 79.74(8) . 5_556
O5 Nb2 O5 69.88(10) 2_556 5_556
O8 Nb2 O6 78.50(8) 3_445 .
O8 Nb2 O6 78.50(8) 8_455 .
O4 Nb2 O6 77.90(8) 6 .
O4 Nb2 O6 77.90(8) . .
O5 Nb2 O6 145.04(5) 2_556 .
O5 Nb2 O6 145.04(5) 5_556 .
O8 Nb2 Nb3 137.64(6) 3_445 .
O8 Nb2 Nb3 137.64(6) 8_455 .
O4 Nb2 Nb3 36.67(5) 6 .
O4 Nb2 Nb3 36.67(5) . .
O5 Nb2 Nb3 95.47(6) 2_556 .
O5 Nb2 Nb3 95.47(6) 5_556 .
O6 Nb2 Nb3 82.18(7) . .
O8 Nb2 Nb4 37.21(5) 3_445 1_455
O8 Nb2 Nb4 37.21(5) 8_455 1_455
O4 Nb2 Nb4 136.95(5) 6 1_455
O4 Nb2 Nb4 136.95(5) . 1_455
O5 Nb2 Nb4 99.38(6) 2_556 1_455
O5 Nb2 Nb4 99.38(6) 5_556 1_455
O6 Nb2 Nb4 79.68(7) . 1_455
Nb3 Nb2 Nb4 161.859(12) . 1_455
O3 Nb3 O1 166.04(8) . .
O3 Nb3 O4 98.26(5) . .
O1 Nb3 O4 93.16(8) . .
O3 Nb3 O4 98.26(5) . 6
O1 Nb3 O4 93.16(8) . 6
O4 Nb3 O4 69.97(10) . 6
O3 Nb3 O8 88.29(5) . .
O1 Nb3 O8 88.55(6) . .
O4 Nb3 O8 138.08(7) . .
O4 Nb3 O8 68.12(7) 6 .
O3 Nb3 O8 88.29(5) . 6
O1 Nb3 O8 88.55(6) . 6
O4 Nb3 O8 68.12(7) . 6
O4 Nb3 O8 138.08(7) 6 6
O8 Nb3 O8 153.77(11) . 6
O3 Nb3 O7 91.02(7) . .
O1 Nb3 O7 75.03(11) . .
O4 Nb3 O7 143.51(6) . .
O4 Nb3 O7 143.51(6) 6 .
O8 Nb3 O7 77.03(5) . .
O8 Nb3 O7 77.03(5) 6 .
O3 Nb3 Nb1 130.319(15) . .
O1 Nb3 Nb1 35.72(8) . .
O4 Nb3 Nb1 121.47(5) . .
O4 Nb3 Nb1 121.47(5) 6 .
O8 Nb3 Nb1 81.24(5) . .
O8 Nb3 Nb1 81.24(5) 6 .
O7 Nb3 Nb1 39.30(7) . .
O3 Nb3 Nb2 107.022(14) . .
O1 Nb3 Nb2 86.93(8) . .
O4 Nb3 Nb2 35.58(5) . .
O4 Nb3 Nb2 35.58(5) 6 .
O8 Nb3 Nb2 102.93(5) . .
O8 Nb3 Nb2 102.93(5) 6 .
O7 Nb3 Nb2 161.96(7) . .
Nb1 Nb3 Nb2 122.658(12) . .
O6 Nb4 O7 101.81(11) 5 .
O6 Nb4 O4 94.74(6) 5 3
O7 Nb4 O4 76.78(5) . 3
O6 Nb4 O4 94.74(6) 5 8_545
O7 Nb4 O4 76.78(5) . 8_545
O4 Nb4 O4 153.21(10) 3 8_545
O6 Nb4 O8 99.39(9) 5 8
O7 Nb4 O8 139.16(6) . 8
O4 Nb4 O8 66.98(7) 3 8
O4 Nb4 O8 135.51(7) 8_545 8
O6 Nb4 O8 99.39(9) 5 3_545
O7 Nb4 O8 139.16(6) . 3_545
O4 Nb4 O8 135.51(7) 3 3_545
O4 Nb4 O8 66.98(7) 8_545 3_545
O8 Nb4 O8 69.17(10) 8 3_545
O6 Nb4 O2 173.42(12) 5 .
O7 Nb4 O2 71.61(10) . .
O4 Nb4 O2 83.87(5) 3 .
O4 Nb4 O2 83.87(5) 8_545 .
O8 Nb4 O2 86.01(8) 8 .
O8 Nb4 O2 86.01(8) 3_545 .
O6 Nb4 Nb1 140.08(9) 5 .
O7 Nb4 Nb1 38.27(7) . .
O4 Nb4 Nb1 78.33(5) 3 .
O4 Nb4 Nb1 78.33(5) 8_545 .
O8 Nb4 Nb1 113.12(5) 8 .
O8 Nb4 Nb1 113.12(5) 3_545 .
O2 Nb4 Nb1 33.34(7) . .
O6 Nb4 Nb2 105.21(9) 5 1_655
O7 Nb4 Nb2 152.98(7) . 1_655
O4 Nb4 Nb2 100.79(5) 3 1_655
O4 Nb4 Nb2 100.79(5) 8_545 1_655
O8 Nb4 Nb2 34.76(5) 8 1_655
O8 Nb4 Nb2 34.76(5) 3_545 1_655
O2 Nb4 Nb2 81.37(7) . 1_655
Nb1 Nb4 Nb2 114.707(12) . 1_655
O2 Cu1 O2 79.66(11) . 5_656
O2 Cu1 O1 115.44(9) . 3
O2 Cu1 O1 138.40(10) 5_656 3
O2 Cu1 O1 138.40(10) . 7_556
O2 Cu1 O1 115.44(9) 5_656 7_556
O1 Cu1 O1 79.91(11) 3 7_556
O2 Cu1 Nb1 36.40(8) . .
O2 Cu1 Nb1 90.58(7) 5_656 .
O1 Cu1 Nb1 125.28(8) 3 .
O1 Cu1 Nb1 102.46(7) 7_556 .
O2 Cu1 Nb1 90.58(7) . 5_656
O2 Cu1 Nb1 36.40(8) 5_656 5_656
O1 Cu1 Nb1 102.46(7) 3 5_656
O1 Cu1 Nb1 125.28(8) 7_556 5_656
Nb1 Cu1 Nb1 117.672(18) . 5_656
O2 Cu1 Nb1 125.22(8) . 3
O2 Cu1 Nb1 101.23(7) 5_656 3
O1 Cu1 Nb1 37.66(8) 3 3
O1 Cu1 Nb1 91.24(7) 7_556 3
Nb1 Cu1 Nb1 156.079(11) . 3
Nb1 Cu1 Nb1 66.782(4) 5_656 3
O2 Cu1 Nb1 101.23(7) . 7_556
O2 Cu1 Nb1 125.22(8) 5_656 7_556
O1 Cu1 Nb1 91.24(7) 3 7_556
O1 Cu1 Nb1 37.66(8) 7_556 7_556
Nb1 Cu1 Nb1 66.782(4) . 7_556
Nb1 Cu1 Nb1 156.079(11) 5_656 7_556
Nb1 Cu1 Nb1 119.695(17) 3 7_556
Nb1 O1 Nb3 107.94(12) . .
Nb1 O1 Cu1 102.58(9) . 7_556
Nb3 O1 Cu1 120.51(8) . 7_556
Nb1 O1 Cu1 102.58(9) . 3_445
Nb3 O1 Cu1 120.51(8) . 3_445
Cu1 O1 Cu1 100.09(11) 7_556 3_445
Nb1 O2 Cu1 102.45(10) . .
Nb1 O2 Cu1 102.45(10) . 5_656
Cu1 O2 Cu1 100.34(11) . 5_656
Nb1 O2 Nb4 106.26(12) . .
Cu1 O2 Nb4 121.25(8) . .
Cu1 O2 Nb4 121.25(8) 5_656 .
Nb3 O3 Nb3 180.000(19) 5 .
Nb2 O4 Nb3 107.76(8) . .
Nb2 O4 Nb4 139.15(10) . 3_445
Nb3 O4 Nb4 112.68(9) . 3_445
Nb2 O5 Nb1 111.09(8) 5_556 .
Nb2 O5 Nb1 136.32(9) 5_556 7_556
Nb1 O5 Nb1 112.59(8) . 7_556
Nb4 O6 Nb2 175.11(16) 5 .
Nb4 O7 Nb3 153.08(14) . .
Nb4 O7 Nb1 104.72(12) . .
Nb3 O7 Nb1 102.20(11) . .
Nb2 O8 Nb3 139.73(10) 3 .
Nb2 O8 Nb4 108.02(8) 3 3_455
Nb3 O8 Nb4 111.51(9) . 3_455
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 O2 1.890(3) .
Nb1 O1 2.002(3) .
Nb1 O5 2.0737(18) .
Nb1 O5 2.0737(18) 6
Nb1 O5 2.0997(18) 7_556
Nb1 O5 2.0997(18) 4_546
Nb1 O7 2.114(3) .
Nb1 Cu1 3.1094(4) .
Nb1 Cu1 3.1094(4) 5_656
Nb1 Cu1 3.1977(4) 3_445
Nb1 Cu1 3.1977(4) 7_556
Nb1 Nb3 3.2619(4) .
Nb2 O8 1.9875(19) 3_445
Nb2 O8 1.9875(19) 8_455
Nb2 O4 2.0097(19) 6
Nb2 O4 2.0097(19) .
Nb2 O5 2.0224(18) 2_556
Nb2 O5 2.0224(18) 5_556
Nb2 O6 2.185(2) .
Nb2 Nb3 3.2898(5) .
Nb2 Nb4 3.3146(4) 1_455
Nb3 O3 1.8834(3) .
Nb3 O1 2.032(3) .
Nb3 O4 2.0628(19) .
Nb3 O4 2.0628(19) 6
Nb3 O8 2.0729(19) .
Nb3 O8 2.0729(19) 6
Nb3 O7 2.077(3) .
Nb4 O6 1.765(2) 5
Nb4 O7 2.054(3) .
Nb4 O4 2.0895(19) 3
Nb4 O4 2.0895(19) 8_545
Nb4 O8 2.1080(19) 8
Nb4 O8 2.1080(19) 3_545
Nb4 O2 2.229(3) .
Nb4 Nb2 3.3146(4) 1_655
Cu1 O2 2.0953(17) .
Cu1 O2 2.0953(17) 5_656
Cu1 O1 2.0954(17) 3
Cu1 O1 2.0954(17) 7_556
Cu1 Nb1 3.1094(4) 5_656
Cu1 Nb1 3.1977(4) 3
Cu1 Nb1 3.1977(4) 7_556
O1 Cu1 2.0954(17) 7_556
O1 Cu1 2.0954(17) 3_445
O2 Cu1 2.0953(17) 5_656
O3 Nb3 1.8834(3) 5
O4 Nb4 2.0895(19) 3_445
O5 Nb2 2.0224(18) 5_556
O5 Nb1 2.0997(18) 7_556
O6 Nb4 1.765(2) 5
O8 Nb2 1.9875(19) 3
O8 Nb4 2.1080(19) 3_455
