#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:01:24 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229478 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/76/7047670.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_7047670
loop_
_publ_author_name
'Dopta, Joanna'
'Grzanna, Sven'
'Näther, Christian'
'Bensch, Wolfgang'
_publ_section_title
;
 On the influence of the titanium source on the composition and structure
 of novel titanoniobates.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15103
_journal_page_last               15113
_journal_paper_doi               10.1039/c8dt02835d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C40 H140 N16 Nb8 Ni4 O50 Ti2'
_chemical_formula_weight         2719.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-09-14 deposited with the CCDC.
2018-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 128.456(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.8775(6)
_cell_length_b                   21.9384(5)
_cell_length_c                   14.6624(4)
_cell_measurement_reflns_used    5340
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.005
_cell_measurement_theta_min      1.661
_cell_volume                     4755.1(3)
_computing_cell_refinement       'X-AREA (STOE, 2008)'
_computing_data_collection       'X-AREA (STOE, 2008)'
_computing_data_reduction        'X-AREA (STOE, 2008)'
_computing_molecular_graphics
'XP (Sheldrick, 2008) and Diamond (Brandenburg, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34711
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.005
_diffrn_reflns_theta_min         1.661
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.948
_exptl_absorpt_correction_T_max  0.8078
_exptl_absorpt_correction_T_min  0.5950
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'
_exptl_crystal_colour            'pale purple'
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0515P)²+12.0179P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4859
_reflns_number_total             5340
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt02835d2.cif
_cod_data_source_block           jo2314
_cod_depositor_comments
'Adding full bibliography for 7047668--7047670.cif.'
_cod_original_cell_volume        4755.1(2)
_cod_database_code               7047670
_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.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.40558(2) 0.35557(2) 0.99039(2) 0.01909(8) Uani 1 1 d . . . . .
Nb2 Nb 0.40805(2) 0.42741(2) 0.79335(2) 0.02091(8) Uani 1 1 d . . . . .
Ti1 Ti 0.40849(4) 0.5000 0.99205(6) 0.01727(14) Uani 1 2 d S T P . .
O1 O 0.33685(14) 0.29999(9) 0.98593(18) 0.0249(4) Uani 1 1 d . . . . .
O2 O 0.34736(13) 0.36983(9) 0.82291(17) 0.0212(4) Uani 1 1 d . . . . .
O3 O 0.50368(13) 0.37184(9) 0.83831(17) 0.0220(4) Uani 1 1 d . . . . .
O4 O 0.5000 0.30840(12) 1.0000 0.0217(6) Uani 1 2 d S T P . .
O5 O 0.35545(17) 0.5000 0.8253(2) 0.0179(5) Uani 1 2 d S T P . .
O6 O 0.34628(13) 0.43419(9) 0.98283(18) 0.0206(4) Uani 1 1 d . . . . .
O7 O 0.5000 0.56517(12) 1.0000 0.0178(5) Uani 1 2 d S T P . .
O8 O 0.50432(18) 0.5000 1.1614(2) 0.0188(5) Uani 1 2 d S T P . .
O9 O 0.33695(15) 0.43417(10) 0.64003(19) 0.0263(4) Uani 1 1 d . . . . .
Ni1 Ni 0.2500 0.2500 1.0000 0.02153(12) Uani 1 2 d S . P . .
N1 N 0.28508(19) 0.30439(12) 1.1372(3) 0.0322(6) Uani 1 1 d . . . . .
H1 H 0.3362 0.3311 1.1581 0.039 Uiso 1 1 calc R U . . .
C1 C 0.2058(3) 0.34397(16) 1.0892(3) 0.0380(8) Uani 1 1 d . . . . .
H1A H 0.2234 0.3796 1.1407 0.046 Uiso 1 1 calc R U . . .
H1B H 0.1583 0.3211 1.0844 0.046 Uiso 1 1 calc R U . . .
C2 C 0.1696(3) 0.36515(15) 0.9692(4) 0.0380(8) Uani 1 1 d . . . . .
H2A H 0.1154 0.3909 0.9351 0.046 Uiso 1 1 calc R U . . .
H2B H 0.2160 0.3898 0.9745 0.046 Uiso 1 1 calc R U . . .
N2 N 0.14610(18) 0.31179(12) 0.8951(3) 0.0305(6) Uani 1 1 d . . . . .
H2 H 0.0899 0.2938 0.8769 0.037 Uiso 1 1 calc R U . . .
C3 C 0.1262(2) 0.32696(17) 0.7844(3) 0.0398(8) Uani 1 1 d . . . . .
H3A H 0.1787 0.3485 0.7995 0.048 Uiso 1 1 calc R U . . .
H3B H 0.0736 0.3548 0.7400 0.048 Uiso 1 1 calc R U . . .
C4 C 0.1057(3) 0.2701(2) 0.7115(3) 0.0490(10) Uani 1 1 d . . . . .
H4A H 0.0585 0.2463 0.7056 0.059 Uiso 1 1 calc R U . . .
H4B H 0.0802 0.2832 0.6318 0.059 Uiso 1 1 calc R U . . .
C5 C 0.1851(3) 0.22856(19) 0.7567(3) 0.0424(8) Uani 1 1 d . . . . .
H5A H 0.1680 0.1987 0.6954 0.051 Uiso 1 1 calc R U . . .
H5B H 0.2361 0.2531 0.7737 0.051 Uiso 1 1 calc R U . . .
Ni2 Ni 0.24240(3) 0.5000 0.52040(4) 0.02325(12) Uani 1 2 d S T P . .
N11 N 0.1765(3) 0.5104(4) 0.5940(4) 0.025(2) Uani 0.5 1 d . . P A -1
H11 H 0.2216 0.4977 0.6772 0.031 Uiso 0.5 1 calc R U P A -1
C11 C 0.1034(4) 0.4650(3) 0.5401(6) 0.0328(14) Uani 0.5 1 d . . P A -1
H11A H 0.0470 0.4827 0.4701 0.039 Uiso 0.5 1 calc R U P A -1
H11B H 0.0924 0.4536 0.5957 0.039 Uiso 0.5 1 calc R U P A -1
C12 C 0.1289(6) 0.4088(4) 0.5061(8) 0.0345(17) Uani 0.5 1 d . . P A -1
H12A H 0.1813 0.3881 0.5765 0.041 Uiso 0.5 1 calc R U P A -1
H12B H 0.0775 0.3799 0.4631 0.041 Uiso 0.5 1 calc R U P A -1
N12 N 0.1523(5) 0.4294(3) 0.4309(6) 0.0288(15) Uani 0.5 1 d . . P A -1
H12 H 0.0963 0.4460 0.3569 0.035 Uiso 0.5 1 calc R U P A -1
C13 C 0.1834(5) 0.3769(3) 0.4022(6) 0.0364(15) Uani 0.5 1 d . . P A -1
H13A H 0.1337 0.3468 0.3568 0.044 Uiso 0.5 1 calc R U P A -1
H13B H 0.2345 0.3569 0.4749 0.044 Uiso 0.5 1 calc R U P A -1
C14 C 0.2132(10) 0.3968(6) 0.3326(10) 0.034(2) Uani 0.5 1 d . . P A -1
H14A H 0.1651 0.4228 0.2678 0.041 Uiso 0.5 1 calc R U P A -1
H14B H 0.2185 0.3602 0.2978 0.041 Uiso 0.5 1 calc R U P A -1
C15 C 0.3015(5) 0.4314(3) 0.3987(7) 0.0371(16) Uani 0.5 1 d . . P A -1
H15A H 0.3486 0.4079 0.4691 0.044 Uiso 0.5 1 calc R U P A -1
H15B H 0.3204 0.4348 0.3492 0.044 Uiso 0.5 1 calc R U P A -1
N13 N 0.2964(3) 0.4915(6) 0.4333(4) 0.024(3) Uani 0.5 1 d . . P A -1
H13 H 0.3605 0.5058 0.4896 0.028 Uiso 0.5 1 calc R U P A -1
C16 C 0.2496(6) 0.5374(3) 0.3346(7) 0.0408(17) Uani 0.5 1 d . . P A -1
H16A H 0.2914 0.5504 0.3189 0.049 Uiso 0.5 1 calc R U P A -1
H16B H 0.1960 0.5183 0.2630 0.049 Uiso 0.5 1 calc R U P A -1
C17 C 0.2208(12) 0.5920(7) 0.3663(12) 0.045(3) Uani 0.5 1 d . . P A -1
H17A H 0.2748 0.6139 0.4322 0.054 Uiso 0.5 1 calc R U P A -1
H17B H 0.1856 0.6202 0.2992 0.054 Uiso 0.5 1 calc R U P A -1
N14 N 0.1655(5) 0.5722(3) 0.3990(6) 0.0266(14) Uani 0.5 1 d . . P A -1
H14 H 0.1080 0.5546 0.3284 0.032 Uiso 0.5 1 calc R U P A -1
C18 C 0.1423(5) 0.6239(3) 0.4398(6) 0.0330(14) Uani 0.5 1 d . . P A -1
H18A H 0.1058 0.6535 0.3753 0.040 Uiso 0.5 1 calc R U P A -1
H18B H 0.1988 0.6446 0.5039 0.040 Uiso 0.5 1 calc R U P A -1
C19 C 0.0904(6) 0.6054(4) 0.4819(7) 0.0352(18) Uani 0.5 1 d . . P A -1
H19A H 0.0394 0.5792 0.4219 0.042 Uiso 0.5 1 calc R U P A -1
H19B H 0.0644 0.6425 0.4891 0.042 Uiso 0.5 1 calc R U P A -1
C20 C 0.1444(4) 0.5718(3) 0.5972(6) 0.0307(14) Uani 0.5 1 d . . P A -1
H20A H 0.1976 0.5968 0.6565 0.037 Uiso 0.5 1 calc R U P A -1
H20B H 0.1065 0.5671 0.6220 0.037 Uiso 0.5 1 calc R U P A -1
O11 O 0.1388(2) 0.22776(17) 0.4845(3) 0.0683(9) Uani 1 1 d . . . . .
O12 O 0.31607(19) 0.27001(12) 0.6712(2) 0.0472(7) Uani 1 1 d . . . . .
O13 O 0.46544(17) 0.20662(11) 0.8606(2) 0.0394(6) Uani 1 1 d . . . . .
O14 O 0.1058(3) 0.5000 0.0293(3) 0.0414(8) Uani 1 2 d S T P . .
O15 O 0.1763(2) 0.5000 0.8177(3) 0.0427(8) Uani 1 2 d S T P . .
O16 O -0.0129(2) 0.5000 0.2197(3) 0.0420(8) Uani 1 2 d S T P . .
O17 O 0.0000 0.39852(18) 0.0000 0.0469(9) Uani 1 2 d S T P . .
O18 O 0.2898(3) 0.5000 0.1239(4) 0.0710(14) 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
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'
N N 0.0061 0.0033 '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'
Ti Ti 0.2776 0.4457 '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'
Ni Ni 0.3393 1.1124 '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 Nb1 O4 104.52(10) . .
O1 Nb1 O2 103.59(9) . .
O4 Nb1 O2 87.26(6) . .
O1 Nb1 O3 101.91(9) . 2_657
O4 Nb1 O3 88.51(6) . 2_657
O2 Nb1 O3 154.40(8) . 2_657
O1 Nb1 O6 102.69(9) . .
O4 Nb1 O6 152.78(9) . .
O2 Nb1 O6 86.35(8) . .
O3 Nb1 O6 85.95(8) 2_657 .
O1 Nb1 O7 178.15(8) . 5_667
O4 Nb1 O7 77.03(8) . 5_667
O2 Nb1 O7 77.41(6) . 5_667
O3 Nb1 O7 77.04(6) 2_657 5_667
O6 Nb1 O7 75.76(7) . 5_667
O1 Nb1 Ti1 134.84(7) . .
O4 Nb1 Ti1 120.61(7) . .
O2 Nb1 Ti1 81.16(6) . .
O3 Nb1 Ti1 79.35(6) 2_657 .
O6 Nb1 Ti1 32.18(6) . .
O7 Nb1 Ti1 43.59(4) 5_667 .
O1 Nb1 Nb2 135.20(7) . .
O4 Nb1 Nb2 79.14(5) . .
O2 Nb1 Nb2 31.64(6) . .
O3 Nb1 Nb2 122.88(6) 2_657 .
O6 Nb1 Nb2 81.61(6) . .
O7 Nb1 Nb2 45.855(6) 5_667 .
Ti1 Nb1 Nb2 61.445(14) . .
O1 Nb1 Nb2 133.30(7) . 2_657
O4 Nb1 Nb2 78.98(5) . 2_657
O2 Nb1 Nb2 123.11(6) . 2_657
O3 Nb1 Nb2 31.50(6) 2_657 2_657
O6 Nb1 Nb2 82.49(6) . 2_657
O7 Nb1 Nb2 45.754(7) 5_667 2_657
Ti1 Nb1 Nb2 61.011(13) . 2_657
Nb2 Nb1 Nb2 91.474(10) . 2_657
O9 Nb2 O3 107.30(10) . .
O9 Nb2 O2 104.69(9) . .
O3 Nb2 O2 94.01(9) . .
O9 Nb2 O5 97.54(10) . .
O3 Nb2 O5 152.43(10) . .
O2 Nb2 O5 90.99(8) . .
O9 Nb2 O8 99.51(10) . 5_667
O3 Nb2 O8 89.15(8) . 5_667
O2 Nb2 O8 153.39(10) . 5_667
O5 Nb2 O8 74.86(9) . 5_667
O9 Nb2 O7 171.10(9) . 5_667
O3 Nb2 O7 79.71(7) . 5_667
O2 Nb2 O7 79.84(7) . 5_667
O5 Nb2 O7 74.53(9) . 5_667
O8 Nb2 O7 74.74(9) 5_667 5_667
O9 Nb2 Nb2 85.19(7) . 6_565
O3 Nb2 Nb2 129.33(6) . 6_565
O2 Nb2 Nb2 130.96(6) . 6_565
O5 Nb2 Nb2 40.00(6) . 6_565
O8 Nb2 Nb2 40.20(6) 5_667 6_565
O7 Nb2 Nb2 86.08(6) 5_667 6_565
O9 Nb2 Ti1 133.56(7) . 5_667
O3 Nb2 Ti1 76.95(6) . 5_667
O2 Nb2 Ti1 121.36(6) . 5_667
O5 Nb2 Ti1 77.31(7) . 5_667
O8 Nb2 Ti1 34.21(7) 5_667 5_667
O7 Nb2 Ti1 41.54(4) 5_667 5_667
Nb2 Nb2 Ti1 61.126(7) 6_565 5_667
O9 Nb2 Ti1 131.47(7) . .
O3 Nb2 Ti1 120.95(6) . .
O2 Nb2 Ti1 78.13(6) . .
O5 Nb2 Ti1 34.35(7) . .
O8 Nb2 Ti1 77.62(7) 5_667 .
O7 Nb2 Ti1 41.25(4) 5_667 .
Nb2 Nb2 Ti1 61.295(7) 6_565 .
Ti1 Nb2 Ti1 60.16(2) 5_667 .
O9 Nb2 Nb1 137.46(7) . .
O3 Nb2 Nb1 85.35(6) . .
O2 Nb2 Nb1 32.88(6) . .
O5 Nb2 Nb1 84.27(6) . .
O8 Nb2 Nb1 121.60(8) 5_667 .
O7 Nb2 Nb1 47.05(4) 5_667 .
Nb2 Nb2 Nb1 118.372(6) 6_565 .
Ti1 Nb2 Nb1 88.492(13) 5_667 .
Ti1 Nb2 Nb1 57.083(8) . .
O9 Nb2 Nb1 140.29(7) . 2_657
O3 Nb2 Nb1 32.99(6) . 2_657
O2 Nb2 Nb1 84.22(6) . 2_657
O5 Nb2 Nb1 121.26(7) . 2_657
O8 Nb2 Nb1 84.20(6) 5_667 2_657
O7 Nb2 Nb1 46.94(4) 5_667 2_657
Nb2 Nb2 Nb1 118.313(6) 6_565 2_657
Ti1 Nb2 Nb1 57.189(9) 5_667 2_657
Ti1 Nb2 Nb1 88.093(12) . 2_657
Nb1 Nb2 Nb1 61.543(9) . 2_657
O6 Ti1 O6 105.62(13) 6_565 .
O6 Ti1 O8 97.99(8) 6_565 .
O6 Ti1 O8 97.99(8) . .
O6 Ti1 O5 95.80(8) 6_565 .
O6 Ti1 O5 95.80(8) . .
O8 Ti1 O5 157.08(12) . .
O6 Ti1 O7 167.87(8) 6_565 5_667
O6 Ti1 O7 86.38(8) . 5_667
O8 Ti1 O7 81.76(6) . 5_667
O5 Ti1 O7 80.93(6) . 5_667
O6 Ti1 O7 86.39(8) 6_565 .
O6 Ti1 O7 167.86(8) . .
O8 Ti1 O7 81.76(6) . .
O5 Ti1 O7 80.94(6) . .
O7 Ti1 O7 81.56(10) 5_667 .
O6 Ti1 Nb1 36.44(6) 6_565 6_565
O6 Ti1 Nb1 142.06(7) . 6_565
O8 Ti1 Nb1 90.440(13) . 6_565
O5 Ti1 Nb1 89.855(13) . 6_565
O7 Ti1 Nb1 131.52(6) 5_667 6_565
O7 Ti1 Nb1 49.96(5) . 6_565
O6 Ti1 Nb1 142.06(7) 6_565 .
O6 Ti1 Nb1 36.44(6) . .
O8 Ti1 Nb1 90.440(13) . .
O5 Ti1 Nb1 89.854(13) . .
O7 Ti1 Nb1 49.96(5) 5_667 .
O7 Ti1 Nb1 131.52(6) . .
Nb1 Ti1 Nb1 178.40(2) 6_565 .
O6 Ti1 Nb2 86.20(6) 6_565 5_667
O6 Ti1 Nb2 134.68(7) . 5_667
O8 Ti1 Nb2 36.69(5) . 5_667
O5 Ti1 Nb2 126.98(6) . 5_667
O7 Ti1 Nb2 86.50(4) 5_667 5_667
O7 Ti1 Nb2 46.220(12) . 5_667
Nb1 Ti1 Nb2 61.799(9) 6_565 5_667
Nb1 Ti1 Nb2 119.542(18) . 5_667
O6 Ti1 Nb2 134.68(7) 6_565 2_657
O6 Ti1 Nb2 86.20(6) . 2_657
O8 Ti1 Nb2 36.69(5) . 2_657
O5 Ti1 Nb2 126.98(6) . 2_657
O7 Ti1 Nb2 46.220(12) 5_667 2_657
O7 Ti1 Nb2 86.50(4) . 2_657
Nb1 Ti1 Nb2 119.542(18) 6_565 2_657
Nb1 Ti1 Nb2 61.799(9) . 2_657
Nb2 Ti1 Nb2 57.745(14) 5_667 2_657
O6 Ti1 Ti1 127.15(6) 6_565 5_667
O6 Ti1 Ti1 127.15(6) . 5_667
O8 Ti1 Ti1 79.09(8) . 5_667
O5 Ti1 Ti1 77.99(8) . 5_667
O7 Ti1 Ti1 40.78(5) 5_667 5_667
O7 Ti1 Ti1 40.78(5) . 5_667
Nb1 Ti1 Ti1 90.739(12) 6_565 5_667
Nb1 Ti1 Ti1 90.738(12) . 5_667
Nb2 Ti1 Ti1 60.183(18) 5_667 5_667
Nb2 Ti1 Ti1 60.183(18) 2_657 5_667
O6 Ti1 Nb2 84.52(7) 6_565 6_565
O6 Ti1 Nb2 132.04(7) . 6_565
O8 Ti1 Nb2 127.47(7) . 6_565
O5 Ti1 Nb2 36.25(5) . 6_565
O7 Ti1 Nb2 86.05(4) 5_667 6_565
O7 Ti1 Nb2 45.871(12) . 6_565
Nb1 Ti1 Nb2 61.475(9) 6_565 6_565
Nb1 Ti1 Nb2 118.876(19) . 6_565
Nb2 Ti1 Nb2 91.932(14) 5_667 6_565
Nb2 Ti1 Nb2 119.84(2) 2_657 6_565
Ti1 Ti1 Nb2 59.654(18) 5_667 6_565
Nb1 O1 Ni1 166.26(13) . .
Nb2 O2 Nb1 115.48(9) . .
Nb2 O3 Nb1 115.51(10) . 2_657
Nb1 O4 Nb1 117.29(13) . 2_657
Ti1 O5 Nb2 109.40(9) . 6_565
Ti1 O5 Nb2 109.40(9) . .
Nb2 O5 Nb2 100.01(11) 6_565 .
Ti1 O6 Nb1 111.38(10) . .
Ti1 O7 Ti1 98.44(10) . 5_667
Ti1 O7 Nb2 92.23(4) . 5_667
Ti1 O7 Nb2 92.88(4) 5_667 5_667
Ti1 O7 Nb2 92.88(4) . 6_565
Ti1 O7 Nb2 92.23(4) 5_667 6_565
Nb2 O7 Nb2 172.17(12) 5_667 6_565
Ti1 O7 Nb1 175.09(9) . 5_667
Ti1 O7 Nb1 86.456(16) 5_667 5_667
Nb2 O7 Nb1 87.10(5) 5_667 5_667
Nb2 O7 Nb1 87.30(5) 6_565 5_667
Ti1 O7 Nb1 86.456(15) . 6_565
Ti1 O7 Nb1 175.09(9) 5_667 6_565
Nb2 O7 Nb1 87.30(5) 5_667 6_565
Nb2 O7 Nb1 87.10(5) 6_565 6_565
Nb1 O7 Nb1 88.66(8) 5_667 6_565
Ti1 O8 Nb2 109.10(10) . 5_667
Ti1 O8 Nb2 109.10(10) . 2_657
Nb2 O8 Nb2 99.59(11) 5_667 2_657
Nb2 O9 Ni2 134.04(12) . .
N1 Ni1 N1 180.0 . 7_557
N1 Ni1 N2 85.81(12) . .
N1 Ni1 N2 94.19(12) 7_557 .
N1 Ni1 N2 94.19(12) . 7_557
N1 Ni1 N2 85.81(12) 7_557 7_557
N2 Ni1 N2 180.00(11) . 7_557
N1 Ni1 O1 89.82(10) . .
N1 Ni1 O1 90.18(10) 7_557 .
N2 Ni1 O1 91.27(9) . .
N2 Ni1 O1 88.73(9) 7_557 .
N1 Ni1 O1 90.18(10) . 7_557
N1 Ni1 O1 89.83(10) 7_557 7_557
N2 Ni1 O1 88.73(9) . 7_557
N2 Ni1 O1 91.27(9) 7_557 7_557
O1 Ni1 O1 180.0 . 7_557
C5 N1 C1 113.6(3) 7_557 .
C5 N1 Ni1 115.2(2) 7_557 .
C1 N1 Ni1 105.1(2) . .
N1 C1 C2 109.0(3) . .
N2 C2 C1 109.0(3) . .
C3 N2 C2 113.1(3) . .
C3 N2 Ni1 116.4(2) . .
C2 N2 Ni1 105.2(2) . .
N2 C3 C4 111.7(3) . .
C5 C4 C3 115.8(3) . .
N1 C5 C4 112.5(3) 7_557 .
N12 Ni2 N13 93.9(4) . .
N12 Ni2 N11 83.7(3) . .
N13 Ni2 N11 174.8(2) . .
N12 Ni2 O9 87.2(2) . .
N13 Ni2 O9 88.0(3) . .
N11 Ni2 O9 96.4(2) . .
N12 Ni2 O9 168.8(2) . 6_565
N13 Ni2 O9 95.0(3) . 6_565
N11 Ni2 O9 87.9(2) . 6_565
O9 Ni2 O9 86.37(12) . 6_565
N12 Ni2 N14 99.3(2) . .
N13 Ni2 N14 83.9(4) . .
N11 Ni2 N14 92.0(3) . .
O9 Ni2 N14 169.9(2) . .
O9 Ni2 N14 88.32(19) 6_565 .
C11 N11 C20 111.4(5) . .
C11 N11 Ni2 107.9(5) . .
C20 N11 Ni2 119.7(5) . .
N11 C11 C12 110.1(6) . .
N12 C12 C11 107.2(6) . .
C13 N12 C12 109.2(6) . .
C13 N12 Ni2 117.0(5) . .
C12 N12 Ni2 105.3(5) . .
N12 C13 C14 110.5(7) . .
C13 C14 C15 116.1(8) . .
N13 C15 C14 113.4(7) . .
C15 N13 C16 113.5(6) . .
C15 N13 Ni2 117.7(7) . .
C16 N13 Ni2 108.0(6) . .
C17 C16 N13 110.0(7) . .
N14 C17 C16 109.6(10) . .
C17 N14 C18 111.0(8) . .
C17 N14 Ni2 103.9(7) . .
C18 N14 Ni2 116.9(5) . .
N14 C18 C19 113.1(6) . .
C18 C19 C20 115.6(7) . .
N11 C20 C19 114.2(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 O1 1.752(2) .
Nb1 O4 1.9888(14) .
Nb1 O2 1.995(2) .
Nb1 O3 2.005(2) 2_657
Nb1 O6 2.0213(19) .
Nb1 O7 2.4305(19) 5_667
Nb1 Ti1 3.1688(2) .
Nb1 Nb2 3.3165(4) .
Nb1 Nb2 3.3227(4) 2_657
Nb2 O9 1.768(2) .
Nb2 O3 1.924(2) .
Nb2 O2 1.927(2) .
Nb2 O5 2.0787(17) .
Nb2 O8 2.0852(17) 5_667
Nb2 O7 2.3829(3) 5_667
Nb2 Nb2 3.1849(5) 6_565
Nb2 Ti1 3.2980(6) 5_667
Nb2 Ti1 3.3156(6) .
Nb2 Nb1 3.3227(4) 2_657
Ti1 O6 1.8124(19) 6_565
Ti1 O6 1.812(2) .
Ti1 O8 1.962(3) .
Ti1 O5 1.983(3) .
Ti1 O7 2.1889(17) 5_667
Ti1 O7 2.1889(17) .
Ti1 Nb1 3.1688(2) 6_565
Ti1 Nb2 3.2979(6) 5_667
Ti1 Nb2 3.2979(6) 2_657
Ti1 Ti1 3.3149(13) 5_667
Ti1 Nb2 3.3156(6) 6_565
O1 Ni1 2.087(2) .
O3 Nb1 2.005(2) 2_657
O4 Nb1 1.9888(14) 2_657
O5 Nb2 2.0787(17) 6_565
O7 Ti1 2.1889(17) 5_667
O7 Nb2 2.3829(3) 5_667
O7 Nb2 2.3829(3) 6_565
O7 Nb1 2.4305(18) 5_667
O7 Nb1 2.4305(18) 6_565
O8 Nb2 2.0850(17) 5_667
O8 Nb2 2.0850(17) 2_657
O9 Ni2 2.110(2) .
Ni1 N1 2.062(3) .
Ni1 N1 2.062(3) 7_557
Ni1 N2 2.073(3) .
Ni1 N2 2.073(3) 7_557
Ni1 O1 2.087(2) 7_557
N1 C5 1.474(5) 7_557
N1 C1 1.477(4) .
C1 C2 1.512(5) .
C2 N2 1.465(5) .
N2 C3 1.460(5) .
C3 C4 1.527(6) .
C4 C5 1.510(6) .
C5 N1 1.474(5) 7_557
Ni2 N12 2.058(7) .
Ni2 N13 2.080(5) .
Ni2 N11 2.105(5) .
Ni2 O9 2.111(2) 6_565
Ni2 N14 2.138(6) .
N11 C11 1.471(9) .
N11 C20 1.489(10) .
C11 C12 1.515(10) .
C12 N12 1.491(11) .
N12 C13 1.470(9) .
C13 C14 1.504(16) .
C14 C15 1.512(17) .
C15 N13 1.437(14) .
N13 C16 1.517(12) .
C16 C17 1.504(19) .
C17 N14 1.459(16) .
N14 C18 1.470(10) .
C18 C19 1.503(11) .
C19 C20 1.516(11) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2 H2B O6 0.99 2.58 3.553(4) 169.0 .
N2 H2 O13 1.00 2.21 3.147(4) 155.6 8_455
C5 H5B O1 0.99 2.65 3.160(4) 112.5 .
N11 H11 O5 1.00 2.07 2.953(5) 146.3 .
N12 H12 O16 1.00 2.13 3.114(7) 167.3 .
C13 H13B O9 0.99 2.58 3.093(7) 112.3 .
N14 H14 O16 1.00 2.16 3.122(7) 161.3 .
C20 H20A O2 0.99 2.43 3.391(7) 163.8 6_565
