#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:47:02 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180276 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/62/7116212.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_7116212
loop_
_publ_author_name
'Son, Jung-Ho'
'Casey, William H.'
_publ_section_title
;
 Reversible capping/uncapping of phosphorous-centered Keggin-type
 polyoxoniobate clusters.
;
_journal_issue                   8
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1436
_journal_page_last               1438
_journal_paper_doi               10.1039/c4cc05689b
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         '10(C4 H12 N) H5 P Nb12 O40 30.5(H2 O)'
_chemical_formula_sum            'C40 H52 N10 Nb12 O70 P'
_chemical_formula_weight         2938.80
_chemical_name_common            'tetramethylammonium dodecaniobophosphate'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                70.1318(18)
_cell_angle_beta                 69.2539(18)
_cell_angle_gamma                74.0995(18)
_cell_formula_units_Z            1
_cell_length_a                   13.479(2)
_cell_length_b                   13.786(2)
_cell_length_c                   16.904(2)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.34
_cell_volume                     2720.2(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32376
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.343
_exptl_absorpt_coefficient_mu    1.328
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_description       block
_exptl_crystal_F_000             1429
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.227
_exptl_crystal_size_min          0.136
_refine_diff_density_max         2.554
_refine_diff_density_min         -1.745
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         11113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0966
_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)+(0.1031P)²+34.1113P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2440
_refine_ls_wR_factor_ref         0.2525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9520
_reflns_number_total             11113
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4cc05689b2.cif
_cod_data_source_block           TMA-PNb12O40
_cod_depositor_comments
'Adding full bibliography for 7116210--7116212.cif.'
_cod_original_cell_volume        2720.1(7)
_cod_database_code               7116212
#BEGIN Tags that were not found in dictionaries:
_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_min   0.599
_shelx_estimated_absorpt_t_max   0.840
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Nb1 Nb 0.46467(9) 0.60077(8) 0.27923(6) 0.0586(3) Uani 1 1 d . . .
Nb2 Nb 0.46811(7) 0.32276(6) 0.39417(6) 0.0487(2) Uani 1 1 d . . .
Nb3 Nb 0.72036(9) 0.42840(8) 0.31590(6) 0.0621(3) Uani 1 1 d . . .
Nb4 Nb 0.75076(10) 0.32520(9) 0.53772(9) 0.0778(4) Uani 1 1 d . . .
Nb5 Nb 0.75074(8) 0.60779(7) 0.41843(6) 0.0556(3) Uani 1 1 d . . .
Nb6 Nb 0.50079(7) 0.77934(6) 0.38175(7) 0.0572(3) Uani 1 1 d . . .
P1 P 0.5000 0.5000 0.5000 0.0345(6) Uani 1 2 d S . P
O1 O 0.4457(8) 0.6441(7) 0.1744(6) 0.085(3) Uani 1 1 d . . .
O2 O 0.4356(6) 0.4606(6) 0.3147(7) 0.087(3) Uani 1 1 d . . .
O3 O 0.6219(6) 0.5419(6) 0.2545(6) 0.080(3) Uani 1 1 d . . .
O4 O 0.5094(7) 0.7220(10) 0.2870(9) 0.115(4) Uani 1 1 d . . .
O5 O 0.3196(7) 0.6433(9) 0.3495(8) 0.107(4) Uani 1 1 d . . .
O6 O 0.4566(8) 0.5986(7) 0.4299(7) 0.032(3) Uani 0.49(2) 1 d . . .
O7 O 0.4528(8) 0.2395(7) 0.3438(7) 0.090(3) Uani 1 1 d . . .
O8 O 0.6241(6) 0.3294(6) 0.3422(7) 0.088(3) Uani 1 1 d . . .
O9 O 0.3208(6) 0.3524(8) 0.4699(5) 0.079(3) Uani 1 1 d . . .
O10 O 0.5203(9) 0.4712(8) 0.4170(7) 0.030(4) Uani 0.46(2) 1 d . . .
O11 O 0.8225(6) 0.3945(7) 0.2273(6) 0.078(2) Uani 1 1 d . . .
O12 O 0.7709(13) 0.3322(6) 0.4156(7) 0.126(5) Uani 1 1 d . . .
O13 O 0.7725(10) 0.5414(10) 0.3264(8) 0.109(3) Uiso 1 1 d . . .
O14 O 0.6297(9) 0.4793(7) 0.4553(7) 0.038(4) Uani 0.51(2) 1 d . . .
O15 O 0.8701(6) 0.2429(5) 0.5556(5) 0.0611(18) Uani 1 1 d . . .
O16 O 0.7913(13) 0.4668(6) 0.4956(8) 0.133(6) Uani 1 1 d . . .
O17 O 0.8681(6) 0.6585(6) 0.3798(5) 0.0593(17) Uani 1 1 d . . .
O18 O 0.6534(6) 0.7240(8) 0.3638(5) 0.083(3) Uani 1 1 d . . .
O19 O 0.5013(8) 0.9103(5) 0.3279(5) 0.079(3) Uani 1 1 d . . .
O20 O 0.4888(6) 0.7760(7) 0.5016(5) 0.081(3) Uani 1 1 d . . .
O21 O 0.3442(7) 0.7748(10) 0.4290(9) 0.122(5) Uani 1 1 d . . .
O22 O 0.5427(8) 0.5948(7) 0.4890(7) 0.031(3) Uani 0.48(2) 1 d . . .
O23 O 1.0081(9) 0.1046(10) 0.4660(12) 0.153(7) Uani 1 1 d . . .
O24 O 0.9756(11) 0.2024(9) 0.3088(16) 0.203(10) Uani 1 1 d . . .
O25 O 0.963(4) 0.245(2) 0.166(2) 0.39(3) Uani 1 1 d . . .
O26 O 0.904(2) 0.103(3) 0.147(2) 0.328(19) Uani 1 1 d . . .
O27 O 0.985(3) 0.482(3) 0.0881(13) 0.293(16) Uani 1 1 d . . .
O28 O 0.497(2) 0.1122(8) 0.2475(7) 0.236(13) Uani 1 1 d . . .
O29 O 0.5814(14) 0.8869(14) 0.1122(10) 0.167(7) Uani 1 1 d . . .
O30 O 0.5262(10) 0.7863(10) 0.0264(8) 0.122(4) Uani 1 1 d . . .
O31 O 0.337(3) 0.298(3) 0.110(2) 0.303(15) Uiso 1 1 d . . .
O32 O 0.150(4) 0.328(4) 0.101(3) 0.39(2) Uiso 1 1 d . . .
O33 O 0.2187(9) 0.7154(9) 0.1751(7) 0.106(3) Uani 1 1 d . . .
O34 O 0.188(2) 0.8776(18) 0.0197(15) 0.219(9) Uani 1 1 d . . .
O35 O 0.017(5) 0.932(4) 0.142(5) 0.56(4) Uani 1 1 d . . .
O36 O 0.4039(14) 0.9107(12) 0.9236(10) 0.147(5) Uani 1 1 d . . .
O37 O 0.292(3) 0.826(3) 0.768(3) 0.092(17) Uani 0.29(4) 1 d . . .
O38 O 0.0406(6) 0.7549(6) 0.3202(5) 0.067(2) Uani 1 1 d . . .
N1 N 0.2700(10) 0.0212(8) 0.5670(11) 0.094(4) Uani 1 1 d . . .
N2 N 0.1106(10) 0.4081(8) 0.3425(7) 0.079(3) Uani 1 1 d . . .
N3 N 0.2419(13) -0.0029(14) 0.2223(11) 0.117(5) Uani 1 1 d . . .
N4 N 0.859(2) 0.773(2) 0.1239(14) 0.221(14) Uani 1 1 d . . .
N5 N 0.316(3) 0.626(3) 0.928(3) 0.265(19) Uani 1 1 d . . .
C1 C 0.2245(17) -0.0706(14) 0.5833(17) 0.145(9) Uani 1 1 d . . .
H1A H 0.2041 -0.1050 0.6465 0.218 Uiso 1 1 calc R U .
H1B H 0.2781 -0.1195 0.5521 0.218 Uiso 1 1 calc R U .
H1C H 0.1606 -0.0490 0.5623 0.218 Uiso 1 1 calc R U .
C2 C 0.312(2) 0.049(2) 0.476(2) 0.229(19) Uani 1 1 d . . .
H2A H 0.2554 0.0952 0.4497 0.343 Uiso 1 1 calc R U .
H2B H 0.3374 -0.0140 0.4552 0.343 Uiso 1 1 calc R U .
H2C H 0.3718 0.0861 0.4592 0.343 Uiso 1 1 calc R U .
C3 C 0.192(2) 0.0975(17) 0.6002(18) 0.178(12) Uani 1 1 d . . .
H3A H 0.2264 0.1469 0.6072 0.267 Uiso 1 1 calc R U .
H3B H 0.1454 0.0647 0.6574 0.267 Uiso 1 1 calc R U .
H3C H 0.1485 0.1351 0.5595 0.267 Uiso 1 1 calc R U .
C4 C 0.364(3) -0.015(2) 0.603(4) 0.30(3) Uani 1 1 d . . .
C5 C 0.1811(19) 0.3075(14) 0.3353(18) 0.144(9) Uani 1 1 d . . .
C6 C 0.1572(18) 0.4982(14) 0.3140(18) 0.147(9) Uani 1 1 d . . .
C7 C 0.0246(18) 0.4283(17) 0.3008(14) 0.141(9) Uani 1 1 d . . .
C8 C 0.0535(19) 0.392(2) 0.4398(12) 0.154(10) Uani 1 1 d . . .
C9 C 0.3057(18) -0.108(2) 0.2142(18) 0.170(11) Uani 1 1 d . . .
C10 C 0.276(5) 0.074(3) 0.169(3) 0.44(5) Uani 1 1 d . . .
H10A H 0.2777 0.1307 0.1886 0.533 Uiso 1 1 calc R U .
H10B H 0.2996 0.0788 0.1082 0.533 Uiso 1 1 calc R U .
C11 C 0.135(2) -0.018(2) 0.218(3) 0.220(17) Uani 1 1 d . . .
H11A H 0.0806 0.0447 0.2238 0.330 Uiso 1 1 calc R U .
H11B H 0.1101 -0.0785 0.2664 0.330 Uiso 1 1 calc R U .
H11C H 0.1462 -0.0315 0.1619 0.330 Uiso 1 1 calc R U .
C12 C 0.207(3) -0.0072(18) 0.3109(19) 0.201(15) Uani 1 1 d . . .
H12A H 0.2628 0.0099 0.3263 0.301 Uiso 1 1 calc R U .
H12B H 0.1938 -0.0779 0.3459 0.301 Uiso 1 1 calc R U .
H12C H 0.1405 0.0434 0.3231 0.301 Uiso 1 1 calc R U .
C13 C 0.775(4) 0.708(4) 0.127(3) 0.27(2) Uiso 1 1 d . . .
C14 C 0.952(3) 0.700(3) 0.1559(19) 0.217(16) Uani 1 1 d . . .
C15 C 0.895(3) 0.845(3) 0.0327(14) 0.26(2) Uani 1 1 d . . .
H15A H 0.9683 0.8158 0.0029 0.391 Uiso 1 1 calc R U .
H15B H 0.8935 0.9144 0.0368 0.391 Uiso 1 1 calc R U .
H15C H 0.8463 0.8504 -0.0008 0.391 Uiso 1 1 calc R U .
C16 C 0.802(3) 0.863(2) 0.183(2) 0.184(12) Uiso 1 1 d . . .
H16A H 0.8556 0.9046 0.1739 0.277 Uiso 1 1 calc R U .
H16B H 0.7781 0.8262 0.2458 0.277 Uiso 1 1 calc R U .
H16C H 0.7404 0.9088 0.1644 0.277 Uiso 1 1 calc R U .
C17 C 0.181(5) 0.627(4) 0.982(3) 0.30(2) Uiso 1 1 d . . .
C18 C 0.371(3) 0.615(3) 0.997(3) 0.28(2) Uiso 1 1 d . . .
H18A H 0.3276 0.5818 1.0558 0.417 Uiso 1 1 calc R U .
H18B H 0.3781 0.6846 0.9960 0.417 Uiso 1 1 calc R U .
H18C H 0.4428 0.5718 0.9842 0.417 Uiso 1 1 calc R U .
C19 C 0.336(4) 0.516(3) 0.922(3) 0.33(3) Uani 1 1 d . . .
C20 C 0.302(5) 0.740(5) 0.831(5) 0.39(5) 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'
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'
P P 0.1023 0.0942 '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
O1 Nb1 O2 99.7(5) . .
O1 Nb1 O5 100.3(5) . .
O2 Nb1 O5 88.8(4) . .
O1 Nb1 O4 102.9(5) . .
O2 Nb1 O4 157.3(5) . .
O5 Nb1 O4 89.7(4) . .
O1 Nb1 O3 102.7(4) . .
O2 Nb1 O3 89.0(3) . .
O5 Nb1 O3 156.9(5) . .
O4 Nb1 O3 83.6(4) . .
O1 Nb1 O6 160.9(4) . .
O2 Nb1 O6 94.4(4) . .
O5 Nb1 O6 66.9(4) . .
O4 Nb1 O6 64.3(5) . .
O3 Nb1 O6 90.4(4) . .
O7 Nb2 O2 102.1(5) . .
O7 Nb2 O9 101.2(5) . .
O2 Nb2 O9 86.5(3) . .
O7 Nb2 O8 101.9(5) . .
O2 Nb2 O8 89.4(3) . .
O9 Nb2 O8 156.9(5) . .
O7 Nb2 O20 102.7(5) . 2_666
O2 Nb2 O20 155.1(5) . 2_666
O9 Nb2 O20 89.6(3) . 2_666
O8 Nb2 O20 84.6(3) . 2_666
O7 Nb2 O10 161.5(5) . .
O2 Nb2 O10 64.8(4) . .
O9 Nb2 O10 91.3(4) . .
O8 Nb2 O10 66.5(4) . .
O20 Nb2 O10 90.8(4) 2_666 .
O7 Nb2 O22 161.6(5) . 2_666
O2 Nb2 O22 91.4(4) . 2_666
O9 Nb2 O22 66.9(4) . 2_666
O8 Nb2 O22 90.5(4) . 2_666
O20 Nb2 O22 64.6(4) 2_666 2_666
O10 Nb2 O22 36.9(3) . 2_666
O11 Nb3 O13 100.8(5) . .
O11 Nb3 O12 101.6(5) . .
O13 Nb3 O12 89.7(4) . .
O11 Nb3 O8 100.7(4) . .
O13 Nb3 O8 158.5(5) . .
O12 Nb3 O8 86.4(4) . .
O11 Nb3 O3 101.2(4) . .
O13 Nb3 O3 86.2(4) . .
O12 Nb3 O3 157.2(5) . .
O8 Nb3 O3 89.3(3) . .
O11 Nb3 O14 160.1(4) . .
O13 Nb3 O14 64.8(4) . .
O12 Nb3 O14 66.3(4) . .
O8 Nb3 O14 94.4(4) . .
O3 Nb3 O14 91.8(4) . .
O15 Nb4 O5 101.2(5) . 2_666
O15 Nb4 O21 102.0(4) . 2_666
O5 Nb4 O21 89.5(4) 2_666 2_666
O15 Nb4 O12 101.4(5) . .
O5 Nb4 O12 157.3(5) 2_666 .
O21 Nb4 O12 87.0(5) 2_666 .
O15 Nb4 O16 102.1(5) . .
O5 Nb4 O16 85.6(5) 2_666 .
O21 Nb4 O16 155.9(5) 2_666 .
O12 Nb4 O16 88.5(4) . .
O17 Nb5 O13 100.3(4) . .
O17 Nb5 O18 101.9(4) . .
O13 Nb5 O18 88.4(5) . .
O17 Nb5 O9 102.0(4) . 2_666
O13 Nb5 O9 157.6(5) . 2_666
O18 Nb5 O9 88.9(3) . 2_666
O17 Nb5 O16 102.3(5) . .
O13 Nb5 O16 88.9(4) . .
O18 Nb5 O16 155.7(5) . .
O9 Nb5 O16 84.5(4) 2_666 .
O17 Nb5 O14 158.7(3) . .
O13 Nb5 O14 64.2(4) . .
O18 Nb5 O14 92.5(4) . .
O9 Nb5 O14 93.7(4) 2_666 .
O16 Nb5 O14 64.7(5) . .
O19 Nb6 O18 101.8(4) . .
O19 Nb6 O20 101.9(4) . .
O18 Nb6 O20 89.0(3) . .
O19 Nb6 O4 101.7(5) . .
O18 Nb6 O4 87.4(4) . .
O20 Nb6 O4 156.4(5) . .
O19 Nb6 O21 101.9(5) . .
O18 Nb6 O21 156.2(5) . .
O20 Nb6 O21 84.5(4) . .
O4 Nb6 O21 89.6(4) . .
O19 Nb6 O6 160.2(4) . .
O18 Nb6 O6 91.8(4) . .
O20 Nb6 O6 92.6(4) . .
O4 Nb6 O6 64.2(5) . .
O21 Nb6 O6 65.8(4) . .
O22 P1 O22 180.0 . 2_666
O22 P1 O10 64.5(6) . 2_666
O22 P1 O10 115.5(6) 2_666 2_666
O22 P1 O10 115.5(6) . .
O22 P1 O10 64.5(6) 2_666 .
O10 P1 O10 180.0(7) 2_666 .
O22 P1 O6 69.2(5) . .
O22 P1 O6 110.8(5) 2_666 .
O10 P1 O6 109.9(5) 2_666 .
O10 P1 O6 70.1(5) . .
O22 P1 O6 110.8(5) . 2_666
O22 P1 O6 69.2(5) 2_666 2_666
O10 P1 O6 70.1(5) 2_666 2_666
O10 P1 O6 109.9(5) . 2_666
O6 P1 O6 180.0 . 2_666
O22 P1 O14 71.6(5) . .
O22 P1 O14 108.4(5) 2_666 .
O10 P1 O14 107.5(6) 2_666 .
O10 P1 O14 72.5(6) . .
O6 P1 O14 104.0(5) . .
O6 P1 O14 76.0(5) 2_666 .
O22 P1 O14 108.4(5) . 2_666
O22 P1 O14 71.6(5) 2_666 2_666
O10 P1 O14 72.5(6) 2_666 2_666
O10 P1 O14 107.5(6) . 2_666
O6 P1 O14 76.0(5) . 2_666
O6 P1 O14 104.0(5) 2_666 2_666
O14 P1 O14 180.0 . 2_666
Nb1 O2 Nb2 140.6(6) . .
Nb1 O3 Nb3 137.8(4) . .
Nb6 O4 Nb1 136.2(7) . .
Nb1 O5 Nb4 138.4(6) . 2_666
P1 O6 O22 52.7(5) . .
P1 O6 O10 52.3(5) . .
O22 O6 O10 91.4(7) . .
P1 O6 Nb1 125.5(5) . .
O22 O6 Nb1 139.8(6) . .
O10 O6 Nb1 73.2(5) . .
P1 O6 Nb6 126.1(6) . .
O22 O6 Nb6 73.4(5) . .
O10 O6 Nb6 139.0(6) . .
Nb1 O6 Nb6 94.0(3) . .
Nb3 O8 Nb2 137.9(5) . .
Nb2 O9 Nb5 137.8(5) . 2_666
P1 O10 O22 57.7(5) . 2_666
P1 O10 O6 57.5(5) . .
O22 O10 O6 97.8(7) 2_666 .
P1 O10 Nb2 129.9(6) . .
O22 O10 Nb2 72.2(5) 2_666 .
O6 O10 Nb2 136.4(7) . .
Nb4 O12 Nb3 137.9(6) . .
Nb3 O13 Nb5 136.8(7) . .
P1 O14 Nb3 124.9(6) . .
P1 O14 Nb5 124.7(5) . .
Nb3 O14 Nb5 93.7(4) . .
Nb5 O16 Nb4 138.3(6) . .
Nb6 O18 Nb5 140.2(5) . .
Nb6 O20 Nb2 139.0(5) . 2_666
Nb4 O21 Nb6 138.4(6) 2_666 .
P1 O22 O10 57.8(5) . 2_666
P1 O22 O6 58.1(5) . .
O10 O22 O6 97.9(8) 2_666 .
P1 O22 Nb2 128.7(6) . 2_666
O10 O22 Nb2 70.9(5) 2_666 2_666
O6 O22 Nb2 136.0(6) . 2_666
C3 N1 C2 114.3(19) . .
C3 N1 C1 110.7(18) . .
C2 N1 C1 102(2) . .
C3 N1 C4 115(2) . .
C2 N1 C4 107(3) . .
C1 N1 C4 107.2(18) . .
C6 N2 C5 118.9(16) . .
C6 N2 C7 109.5(16) . .
C5 N2 C7 110.4(13) . .
C6 N2 C8 107.2(17) . .
C5 N2 C8 104.6(17) . .
C7 N2 C8 105.3(14) . .
C10 N3 C12 119(3) . .
C10 N3 C9 118(3) . .
C12 N3 C9 107.0(18) . .
C10 N3 C11 115(4) . .
C12 N3 C11 96(2) . .
C9 N3 C11 97.6(19) . .
C15 N4 C14 113(3) . .
C15 N4 C13 110(3) . .
C14 N4 C13 110(3) . .
C15 N4 C16 101(3) . .
C14 N4 C16 109(3) . .
C13 N4 C16 114(3) . .
C19 N5 C18 103(4) . .
C19 N5 C17 94(4) . .
C18 N5 C17 107(4) . .
C19 N5 C20 121(3) . .
C18 N5 C20 128(4) . .
C17 N5 C20 98(3) . .
N1 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
N1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N1 C3 H3A 109.5 . .
N1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N3 C10 H10A 120.0 . .
N3 C10 H10B 120.0 . .
H10A C10 H10B 120.0 . .
N3 C11 H11A 109.5 . .
N3 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
N3 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N3 C12 H12A 109.5 . .
N3 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
N3 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N4 C15 H15A 109.5 . .
N4 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
N4 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
N4 C16 H16A 109.5 . .
N4 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
N4 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
N5 C18 H18A 109.5 . .
N5 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
N5 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
O37 C20 N5 173(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 O1 1.755(8) .
Nb1 O2 1.926(8) .
Nb1 O5 1.943(8) .
Nb1 O4 1.983(9) .
Nb1 O3 1.997(8) .
Nb1 O6 2.501(11) .
Nb2 O7 1.734(7) .
Nb2 O2 1.957(7) .
Nb2 O9 1.964(8) .
Nb2 O8 1.985(8) .
Nb2 O20 1.989(8) 2_666
Nb2 O10 2.520(10) .
Nb2 O22 2.538(10) 2_666
Nb3 O11 1.738(8) .
Nb3 O13 1.958(12) .
Nb3 O12 1.966(9) .
Nb3 O8 1.973(9) .
Nb3 O3 2.005(8) .
Nb3 O14 2.481(11) .
Nb4 O15 1.755(7) .
Nb4 O5 1.944(9) 2_666
Nb4 O21 1.945(10) 2_666
Nb4 O12 1.955(10) .
Nb4 O16 1.995(10) .
Nb5 O17 1.727(7) .
Nb5 O13 1.959(12) .
Nb5 O18 1.960(8) .
Nb5 O9 1.980(8) 2_666
Nb5 O16 1.995(8) .
Nb5 O14 2.510(11) .
Nb6 O19 1.724(7) .
Nb6 O18 1.940(8) .
Nb6 O20 1.960(9) .
Nb6 O4 1.971(10) .
Nb6 O21 1.985(8) .
Nb6 O6 2.513(10) .
P1 O22 1.499(10) .
P1 O22 1.499(10) 2_666
P1 O10 1.500(11) 2_666
P1 O10 1.500(11) .
P1 O6 1.598(10) .
P1 O6 1.598(10) 2_666
P1 O14 1.627(12) .
P1 O14 1.627(12) 2_666
O5 Nb4 1.944(9) 2_666
O6 O22 1.761(15) .
O6 O10 1.781(13) .
O9 Nb5 1.980(8) 2_666
O10 O22 1.600(15) 2_666
O20 Nb2 1.989(8) 2_666
O21 Nb4 1.945(10) 2_666
O22 O10 1.600(15) 2_666
O22 Nb2 2.538(10) 2_666
O37 C20 1.30(8) .
N1 C3 1.38(2) .
N1 C2 1.39(3) .
N1 C1 1.457(17) .
N1 C4 1.49(3) .
N2 C6 1.40(2) .
N2 C5 1.468(19) .
N2 C7 1.48(2) .
N2 C8 1.51(2) .
N3 C10 1.21(3) .
N3 C12 1.39(3) .
N3 C9 1.49(3) .
N3 C11 1.54(3) .
N4 C15 1.51(2) .
N4 C14 1.52(3) .
N4 C13 1.60(5) .
N4 C16 1.70(4) .
N5 C19 1.50(5) .
N5 C18 1.55(5) .
N5 C17 1.71(6) .
N5 C20 1.87(8) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C10 H10A 0.9500 .
C10 H10B 0.9500 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
