#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:35:19 +0100 (vie 25 de mar de 2016) $
#$Revision: 179852 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/48/7014875.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_7014875
loop_
_publ_author_name
'Zhang, Furen'
'Song, Haibin'
'Zi, Guofu'
_publ_section_title
;
 Synthesis and catalytic activity of group 5 metal amides with chiral
 biaryldiamine-based ligands.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1547
_journal_page_last               1566
_journal_paper_doi               10.1039/c0dt01229g
_journal_volume                  40
_journal_year                    2011
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C55 H64 N5 Nb O2'
_chemical_formula_sum            'C55 H64 N5 Nb O2'
_chemical_formula_weight         920.02
_chemical_name_systematic
;
?
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.974(6)
_cell_angle_beta                 93.029(14)
_cell_angle_gamma                99.572(9)
_cell_formula_units_Z            1
_cell_length_a                   9.5500(10)
_cell_length_b                   10.9436(12)
_cell_length_c                   11.4253(14)
_cell_measurement_reflns_used    6108
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      34.82
_cell_measurement_theta_min      1.91
_cell_volume                     1162.5(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type  'Rigaku Saturn70 CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20069
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         35.12
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  0.9412
_exptl_absorpt_correction_T_min  0.9245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Crystalclear
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.519
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(14)
_refine_ls_extinction_coef       0.0609(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         15623
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0285P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                14011
_reflns_number_total             15623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT01229G.TXT
_cod_data_source_block           compound25
_cod_database_code               7014875
loop_
_symmetry_equiv_pos_as_xyz
'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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 1.004353(9) -0.003726(9) 1.001823(9) 0.01332(4) Uani 1 1 d . . .
O2 O 0.98752(14) 0.16744(12) 1.08245(12) 0.0153(2) Uani 1 1 d . . .
N3 N 1.08456(17) 0.13990(16) 0.86542(15) 0.0162(3) Uani 1 1 d . . .
O1 O 0.97281(15) -0.07907(14) 1.15397(12) 0.0167(3) Uani 1 1 d . . .
N2 N 0.94253(16) -0.12305(14) 0.87487(14) 0.0148(3) Uani 1 1 d . . .
N1 N 0.75522(16) -0.04481(15) 1.00754(14) 0.0143(3) Uani 1 1 d . . .
N5 N 1.20590(17) -0.02335(16) 1.02037(16) 0.0190(3) Uani 1 1 d . . .
C37 C 0.95749(19) 0.31412(17) 0.95113(16) 0.0143(3) Uani 1 1 d . . .
N4 N 0.98600(18) 0.27975(16) 0.73752(15) 0.0188(3) Uani 1 1 d . . .
C11 C 0.66908(19) -0.06110(16) 0.79807(16) 0.0137(3) Uani 1 1 d . . .
C32 C 0.95887(19) 0.28046(16) 1.06537(16) 0.0132(3) Uani 1 1 d . . .
C22 C 0.73019(19) -0.16563(17) 1.17086(17) 0.0161(3) Uani 1 1 d . . .
C1 C 0.70953(19) -0.18623(16) 0.76571(16) 0.0142(3) Uani 1 1 d . . .
C23 C 0.87600(19) -0.14010(17) 1.21286(17) 0.0142(3) Uani 1 1 d . . .
C42 C 0.97387(19) 0.22052(17) 0.84203(16) 0.0141(3) Uani 1 1 d . . .
H42 H 0.8810 0.1611 0.8281 0.017 Uiso 1 1 calc R . .
C2 C 0.84600(19) -0.20700(16) 0.79870(16) 0.0137(3) Uani 1 1 d . . .
C29 C 1.1231(3) -0.0105(2) 1.3958(2) 0.0259(4) Uani 1 1 d . . .
H29A H 1.1100 0.0242 1.3223 0.039 Uiso 1 1 calc R . .
H29B H 1.2242 0.0077 1.4239 0.039 Uiso 1 1 calc R . .
H29C H 1.0677 0.0275 1.4562 0.039 Uiso 1 1 calc R . .
C52 C 0.5134(3) 0.5260(3) -0.0439(3) 0.0405(8) Uani 1 1 d . . .
H52 H 0.5806 0.5329 -0.1021 0.049 Uiso 1 1 calc R . .
C51 C 0.5366(3) 0.4622(3) 0.0501(3) 0.0334(7) Uani 1 1 d . . .
H51 H 0.6191 0.4247 0.0555 0.040 Uiso 1 1 calc R . .
C6 C 0.6096(2) -0.28735(16) 0.69794(16) 0.0150(3) Uani 1 1 d . . .
C12 C 0.68550(19) 0.00108(18) 0.91349(17) 0.0140(3) Uani 1 1 d . . .
C47 C 1.2999(2) 0.0469(2) 1.1215(2) 0.0258(4) Uani 1 1 d . . .
H47A H 1.3272 -0.0113 1.1729 0.039 Uiso 1 1 calc R . .
H47B H 1.2499 0.1069 1.1666 0.039 Uiso 1 1 calc R . .
H47C H 1.3856 0.0922 1.0928 0.039 Uiso 1 1 calc R . .
C5 C 0.6550(2) -0.40161(17) 0.65381(17) 0.0166(3) Uani 1 1 d . . .
C24 C 0.9156(2) -0.18141(17) 1.32131(17) 0.0165(3) Uani 1 1 d . . .
C25 C 0.8094(2) -0.24686(18) 1.37805(18) 0.0201(4) Uani 1 1 d . . .
H25 H 0.8350 -0.2738 1.4505 0.024 Uiso 1 1 calc R . .
C21 C 0.67924(19) -0.11767(17) 1.06816(17) 0.0161(3) Uani 1 1 d . . .
H21 H 0.5809 -0.1421 1.0431 0.019 Uiso 1 1 calc R . .
C13 C 0.64195(19) 0.11871(17) 0.94479(18) 0.0165(3) Uani 1 1 d . . .
H13 H 0.6553 0.1591 1.0247 0.020 Uiso 1 1 calc R . .
C16 C 0.61398(19) 0.00161(17) 0.70695(17) 0.0158(3) Uani 1 1 d . . .
C7 C 0.4631(2) -0.28097(19) 0.67532(18) 0.0201(4) Uani 1 1 d . . .
H7 H 0.4286 -0.2073 0.7059 0.024 Uiso 1 1 calc R . .
C14 C 0.5810(2) 0.17338(17) 0.85962(18) 0.0177(3) Uani 1 1 d . . .
H14 H 0.5478 0.2499 0.8815 0.021 Uiso 1 1 calc R . .
C36 C 0.9262(2) 0.43079(18) 0.93575(18) 0.0188(4) Uani 1 1 d . . .
H36 H 0.9216 0.4530 0.8583 0.023 Uiso 1 1 calc R . .
C35 C 0.9015(2) 0.51508(19) 1.03088(19) 0.0213(4) Uani 1 1 d . . .
H35 H 0.8830 0.5954 1.0193 0.026 Uiso 1 1 calc R . .
C38 C 0.9269(2) 0.32683(18) 1.28904(17) 0.0186(4) Uani 1 1 d . . .
C27 C 0.6275(2) -0.23443(19) 1.23124(19) 0.0205(4) Uani 1 1 d . . .
H27 H 0.5306 -0.2527 1.2006 0.025 Uiso 1 1 calc R . .
C28 C 1.0720(2) -0.15302(19) 1.37262(18) 0.0199(4) Uani 1 1 d . . .
C45 C 0.9108(2) 0.2156(2) 0.62700(19) 0.0251(4) Uani 1 1 d . . .
H45A H 0.9775 0.1786 0.5766 0.038 Uiso 1 1 calc R . .
H45B H 0.8687 0.2754 0.5863 0.038 Uiso 1 1 calc R . .
H45C H 0.8352 0.1491 0.6433 0.038 Uiso 1 1 calc R . .
C34 C 0.9040(2) 0.48110(18) 1.14375(18) 0.0190(4) Uani 1 1 d . . .
H34 H 0.8874 0.5395 1.2089 0.023 Uiso 1 1 calc R . .
C33 C 0.9300(2) 0.36387(17) 1.16422(17) 0.0160(3) Uani 1 1 d . . .
C39 C 0.8198(2) 0.2058(2) 1.29019(19) 0.0237(4) Uani 1 1 d . . .
H39A H 0.8498 0.1365 1.2396 0.036 Uiso 1 1 calc R . .
H39B H 0.7253 0.2167 1.2602 0.036 Uiso 1 1 calc R . .
H39C H 0.8158 0.1870 1.3715 0.036 Uiso 1 1 calc R . .
C17 C 0.6112(2) -0.04425(19) 0.58455(18) 0.0199(4) Uani 1 1 d . . .
H17 H 0.6443 -0.1204 0.5607 0.024 Uiso 1 1 calc R . .
C26 C 0.6668(2) -0.27536(19) 1.33438(19) 0.0223(4) Uani 1 1 d . . .
H26 H 0.5979 -0.3223 1.3753 0.027 Uiso 1 1 calc R . .
C46 C 1.1055(2) 0.3745(2) 0.7223(2) 0.0247(4) Uani 1 1 d . . .
H46A H 1.1432 0.4221 0.7997 0.037 Uiso 1 1 calc R . .
H46B H 1.0744 0.4313 0.6712 0.037 Uiso 1 1 calc R . .
H46C H 1.1801 0.3343 0.6856 0.037 Uiso 1 1 calc R . .
C4 C 0.7971(2) -0.41491(17) 0.68207(18) 0.0188(4) Uani 1 1 d . . .
H4 H 0.8293 -0.4894 0.6505 0.023 Uiso 1 1 calc R . .
C50 C 0.4397(2) 0.4528(2) 0.1364(2) 0.0253(4) Uani 1 1 d . . .
C18 C 0.5621(3) 0.0182(2) 0.4998(2) 0.0257(4) Uani 1 1 d . . .
H18 H 0.5629 -0.0140 0.4183 0.031 Uiso 1 1 calc R . .
C19 C 0.5103(2) 0.1306(2) 0.5329(2) 0.0269(4) Uani 1 1 d . . .
H19 H 0.4736 0.1727 0.4740 0.032 Uiso 1 1 calc R . .
C40 C 1.0767(2) 0.3095(2) 1.33152(19) 0.0242(4) Uani 1 1 d . . .
H40A H 1.1419 0.3900 1.3401 0.036 Uiso 1 1 calc R . .
H40B H 1.1103 0.2485 1.2734 0.036 Uiso 1 1 calc R . .
H40C H 1.0734 0.2790 1.4082 0.036 Uiso 1 1 calc R . .
C8 C 0.3705(2) -0.3796(2) 0.6100(2) 0.0251(4) Uani 1 1 d . . .
H8 H 0.2731 -0.3733 0.5966 0.030 Uiso 1 1 calc R . .
C55 C 0.3194(2) 0.5079(2) 0.1264(2) 0.0272(5) Uani 1 1 d . . .
H55 H 0.2525 0.5023 0.1850 0.033 Uiso 1 1 calc R . .
C53 C 0.3930(3) 0.5797(3) -0.0533(2) 0.0378(6) Uani 1 1 d . . .
H53 H 0.3769 0.6227 -0.1181 0.045 Uiso 1 1 calc R . .
C41 C 0.8836(3) 0.4296(2) 1.3782(2) 0.0308(5) Uani 1 1 d . . .
H41A H 0.8801 0.4025 1.4564 0.046 Uiso 1 1 calc R . .
H41B H 0.7895 0.4450 1.3522 0.046 Uiso 1 1 calc R . .
H41C H 0.9536 0.5069 1.3830 0.046 Uiso 1 1 calc R . .
C30 C 1.1653(2) -0.2160(2) 1.2855(2) 0.0265(4) Uani 1 1 d . . .
H30A H 1.1387 -0.3073 1.2787 0.040 Uiso 1 1 calc R . .
H30B H 1.2657 -0.1904 1.3149 0.040 Uiso 1 1 calc R . .
H30C H 1.1510 -0.1903 1.2076 0.040 Uiso 1 1 calc R . .
C54 C 0.2959(3) 0.5706(2) 0.0322(2) 0.0320(5) Uani 1 1 d . . .
H54 H 0.2130 0.6075 0.0261 0.038 Uiso 1 1 calc R . .
C31 C 1.0901(3) -0.2009(2) 1.4912(2) 0.0301(5) Uani 1 1 d . . .
H31A H 1.0321 -0.1613 1.5483 0.045 Uiso 1 1 calc R . .
H31B H 1.1905 -0.1801 1.5213 0.045 Uiso 1 1 calc R . .
H31C H 1.0593 -0.2921 1.4799 0.045 Uiso 1 1 calc R . .
C49 C 0.4667(3) 0.3861(3) 0.2395(3) 0.0405(6) Uani 1 1 d . . .
H49A H 0.5173 0.4466 0.3057 0.061 Uiso 1 1 calc R . .
H49B H 0.5248 0.3222 0.2160 0.061 Uiso 1 1 calc R . .
H49C H 0.3757 0.3460 0.2640 0.061 Uiso 1 1 calc R . .
C3 C 0.8879(2) -0.32327(17) 0.75326(18) 0.0174(3) Uani 1 1 d . . .
H3 H 0.9816 -0.3362 0.7736 0.021 Uiso 1 1 calc R . .
C10 C 0.5568(2) -0.49964(18) 0.58456(18) 0.0223(4) Uani 1 1 d . . .
H10 H 0.5886 -0.5742 0.5526 0.027 Uiso 1 1 calc R . .
C44 C 1.2234(2) 0.21816(19) 0.91503(19) 0.0207(4) Uani 1 1 d . . .
H44A H 1.2947 0.1642 0.9223 0.031 Uiso 1 1 calc R . .
H44B H 1.2121 0.2630 0.9934 0.031 Uiso 1 1 calc R . .
H44C H 1.2549 0.2787 0.8620 0.031 Uiso 1 1 calc R . .
C43 C 1.1107(2) 0.0672(2) 0.75232(19) 0.0227(4) Uani 1 1 d . . .
H43A H 1.1544 0.1246 0.7005 0.034 Uiso 1 1 calc R . .
H43B H 1.0202 0.0197 0.7135 0.034 Uiso 1 1 calc R . .
H43C H 1.1749 0.0092 0.7678 0.034 Uiso 1 1 calc R . .
C48 C 1.2786(2) -0.1123(2) 0.9513(2) 0.0267(5) Uani 1 1 d . . .
H48A H 1.3585 -0.0665 0.9157 0.040 Uiso 1 1 calc R . .
H48B H 1.2117 -0.1639 0.8885 0.040 Uiso 1 1 calc R . .
H48C H 1.3144 -0.1663 1.0032 0.040 Uiso 1 1 calc R . .
C9 C 0.4182(3) -0.4897(2) 0.5627(2) 0.0265(4) Uani 1 1 d . . .
H9 H 0.3541 -0.5565 0.5159 0.032 Uiso 1 1 calc R . .
C15 C 0.5665(2) 0.11778(17) 0.73938(18) 0.0178(3) Uani 1 1 d . . .
C20 C 0.5132(2) 0.1784(2) 0.6499(2) 0.0239(4) Uani 1 1 d . . .
H20 H 0.4786 0.2542 0.6716 0.029 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'
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'
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
_geom_angle_publ_flag
N2 Nb1 N5 99.92(7) . . ?
N2 Nb1 O2 145.03(6) . . ?
N5 Nb1 O2 108.26(6) . . ?
N2 Nb1 O1 109.48(7) . . ?
N5 Nb1 O1 88.27(7) . . ?
O2 Nb1 O1 91.96(6) . . ?
N2 Nb1 N1 75.37(6) . . ?
N5 Nb1 N1 160.26(6) . . ?
O2 Nb1 N1 84.08(6) . . ?
O1 Nb1 N1 75.68(6) . . ?
N2 Nb1 N3 88.43(7) . . ?
N5 Nb1 N3 85.36(7) . . ?
O2 Nb1 N3 73.99(6) . . ?
O1 Nb1 N3 161.80(5) . . ?
N1 Nb1 N3 113.33(6) . . ?
C32 O2 Nb1 144.63(12) . . ?
C43 N3 C44 106.99(16) . . ?
C43 N3 C42 109.15(15) . . ?
C44 N3 C42 111.45(15) . . ?
C43 N3 Nb1 109.13(12) . . ?
C44 N3 Nb1 108.88(12) . . ?
C42 N3 Nb1 111.12(11) . . ?
C23 O1 Nb1 143.85(13) . . ?
C2 N2 Nb1 156.90(13) . . ?
C21 N1 C12 118.40(16) . . ?
C21 N1 Nb1 128.88(13) . . ?
C12 N1 Nb1 111.55(11) . . ?
C48 N5 C47 110.46(17) . . ?
C48 N5 Nb1 128.50(14) . . ?
C47 N5 Nb1 120.70(14) . . ?
C36 C37 C32 118.90(16) . . ?
C36 C37 C42 119.28(17) . . ?
C32 C37 C42 121.49(16) . . ?
C42 N4 C46 123.00(17) . . ?
C42 N4 C45 119.37(16) . . ?
C46 N4 C45 113.61(17) . . ?
C12 C11 C16 117.60(16) . . ?
C12 C11 C1 122.43(17) . . ?
C16 C11 C1 119.95(16) . . ?
O2 C32 C37 120.06(15) . . ?
O2 C32 C33 118.97(16) . . ?
C37 C32 C33 120.97(16) . . ?
C27 C22 C23 121.05(18) . . ?
C27 C22 C21 116.92(17) . . ?
C23 C22 C21 121.96(17) . . ?
C2 C1 C6 118.94(16) . . ?
C2 C1 C11 120.73(16) . . ?
C6 C1 C11 120.32(16) . . ?
O1 C23 C22 120.94(17) . . ?
O1 C23 C24 120.69(17) . . ?
C22 C23 C24 118.37(17) . . ?
N4 C42 N3 116.38(15) . . ?
N4 C42 C37 111.46(15) . . ?
N3 C42 C37 112.50(14) . . ?
N4 C42 H42 105.1 . . ?
N3 C42 H42 105.1 . . ?
C37 C42 H42 105.1 . . ?
N2 C2 C1 123.58(16) . . ?
N2 C2 C3 117.07(16) . . ?
C1 C2 C3 119.34(16) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C53 C52 C51 120.3(3) . . ?
C53 C52 H52 119.9 . . ?
C51 C52 H52 119.9 . . ?
C52 C51 C50 120.3(3) . . ?
C52 C51 H51 119.8 . . ?
C50 C51 H51 119.8 . . ?
C7 C6 C5 117.28(17) . . ?
C7 C6 C1 122.81(17) . . ?
C5 C6 C1 119.88(17) . . ?
C11 C12 C13 122.27(17) . . ?
C11 C12 N1 122.17(16) . . ?
C13 C12 N1 115.45(17) . . ?
N5 C47 H47A 109.5 . . ?
N5 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
N5 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C4 C5 C10 121.52(18) . . ?
C4 C5 C6 118.91(17) . . ?
C10 C5 C6 119.56(18) . . ?
C25 C24 C23 117.97(18) . . ?
C25 C24 C28 121.56(18) . . ?
C23 C24 C28 120.48(17) . . ?
C24 C25 C26 123.46(19) . . ?
C24 C25 H25 118.3 . . ?
C26 C25 H25 118.3 . . ?
N1 C21 C22 125.80(17) . . ?
N1 C21 H21 117.1 . . ?
C22 C21 H21 117.1 . . ?
C14 C13 C12 119.78(17) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C17 C16 C15 117.61(18) . . ?
C17 C16 C11 122.64(17) . . ?
C15 C16 C11 119.68(17) . . ?
C8 C7 C6 121.16(19) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C13 C14 C15 120.93(16) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C35 C36 C37 121.29(19) . . ?
C35 C36 H36 119.4 . . ?
C37 C36 H36 119.4 . . ?
C36 C35 C34 119.30(18) . . ?
C36 C35 H35 120.4 . . ?
C34 C35 H35 120.4 . . ?
C41 C38 C39 107.60(18) . . ?
C41 C38 C40 107.42(18) . . ?
C39 C38 C40 110.05(18) . . ?
C41 C38 C33 111.27(17) . . ?
C39 C38 C33 111.13(16) . . ?
C40 C38 C33 109.30(16) . . ?
C26 C27 C22 120.15(19) . . ?
C26 C27 H27 119.9 . . ?
C22 C27 H27 119.9 . . ?
C31 C28 C29 107.00(17) . . ?
C31 C28 C30 108.12(18) . . ?
C29 C28 C30 110.43(19) . . ?
C31 C28 C24 111.99(18) . . ?
C29 C28 C24 109.30(16) . . ?
C30 C28 C24 109.96(16) . . ?
N4 C45 H45A 109.5 . . ?
N4 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N4 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C35 C34 C33 122.05(17) . . ?
C35 C34 H34 119.0 . . ?
C33 C34 H34 119.0 . . ?
C34 C33 C32 117.42(17) . . ?
C34 C33 C38 121.05(16) . . ?
C32 C33 C38 121.52(16) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C18 C17 C16 121.69(19) . . ?
C18 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
C27 C26 C25 118.95(19) . . ?
C27 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
N4 C46 H46A 109.5 . . ?
N4 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N4 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C3 C4 C5 121.07(17) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C51 C50 C55 118.9(2) . . ?
C51 C50 C49 120.2(2) . . ?
C55 C50 C49 120.9(2) . . ?
C17 C18 C19 120.3(2) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C20 C19 C18 119.6(2) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C7 C8 C9 120.9(2) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C54 C55 C50 120.7(2) . . ?
C54 C55 H55 119.7 . . ?
C50 C55 H55 119.7 . . ?
C52 C53 C54 119.7(3) . . ?
C52 C53 H53 120.1 . . ?
C54 C53 H53 120.1 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C55 C54 C53 120.1(2) . . ?
C55 C54 H54 120.0 . . ?
C53 C54 H54 120.0 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C50 C49 H49A 109.5 . . ?
C50 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C50 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C4 C3 C2 121.43(18) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C9 C10 C5 121.66(19) . . ?
C9 C10 H10 119.2 . . ?
C5 C10 H10 119.2 . . ?
N3 C44 H44A 109.5 . . ?
N3 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N3 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N3 C43 H43A 109.5 . . ?
N3 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N3 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N5 C48 H48A 109.5 . . ?
N5 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
N5 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C10 C9 C8 119.35(19) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C20 C15 C14 121.17(18) . . ?
C20 C15 C16 119.25(19) . . ?
C14 C15 C16 119.48(17) . . ?
C19 C20 C15 121.5(2) . . ?
C19 C20 H20 119.2 . . ?
C15 C20 H20 119.2 . . ?
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
Nb1 N2 1.8125(15) . ?
Nb1 N5 1.9756(16) . ?
Nb1 O2 2.0051(13) . ?
Nb1 O1 2.0402(14) . ?
Nb1 N1 2.3528(16) . ?
Nb1 N3 2.4272(17) . ?
O2 C32 1.348(2) . ?
N3 C43 1.476(3) . ?
N3 C44 1.491(2) . ?
N3 C42 1.521(2) . ?
O1 C23 1.319(2) . ?
N2 C2 1.365(2) . ?
N1 C21 1.287(3) . ?
N1 C12 1.427(2) . ?
N5 C48 1.456(3) . ?
N5 C47 1.466(3) . ?
C37 C36 1.391(3) . ?
C37 C32 1.404(3) . ?
C37 C42 1.532(2) . ?
N4 C42 1.437(2) . ?
N4 C46 1.444(3) . ?
N4 C45 1.447(3) . ?
C11 C12 1.386(3) . ?
C11 C16 1.446(3) . ?
C11 C1 1.487(2) . ?
C32 C33 1.420(2) . ?
C22 C27 1.405(3) . ?
C22 C23 1.418(3) . ?
C22 C21 1.444(3) . ?
C1 C2 1.401(2) . ?
C1 C6 1.438(2) . ?
C23 C24 1.430(3) . ?
C42 H42 1.0000 . ?
C2 C3 1.434(2) . ?
C29 C28 1.536(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C52 C53 1.382(4) . ?
C52 C51 1.388(4) . ?
C52 H52 0.9500 . ?
C51 C50 1.390(4) . ?
C51 H51 0.9500 . ?
C6 C7 1.424(3) . ?
C6 C5 1.426(3) . ?
C12 C13 1.423(3) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C5 C4 1.414(3) . ?
C5 C10 1.417(3) . ?
C24 C25 1.385(3) . ?
C24 C28 1.541(3) . ?
C25 C26 1.394(3) . ?
C25 H25 0.9500 . ?
C21 H21 0.9500 . ?
C13 C14 1.364(3) . ?
C13 H13 0.9500 . ?
C16 C17 1.416(3) . ?
C16 C15 1.428(3) . ?
C7 C8 1.376(3) . ?
C7 H7 0.9500 . ?
C14 C15 1.413(3) . ?
C14 H14 0.9500 . ?
C36 C35 1.382(3) . ?
C36 H36 0.9500 . ?
C35 C34 1.391(3) . ?
C35 H35 0.9500 . ?
C38 C41 1.535(3) . ?
C38 C39 1.535(3) . ?
C38 C40 1.536(3) . ?
C38 C33 1.536(3) . ?
C27 C26 1.373(3) . ?
C27 H27 0.9500 . ?
C28 C31 1.531(3) . ?
C28 C30 1.538(3) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C34 C33 1.395(3) . ?
C34 H34 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C17 C18 1.367(3) . ?
C17 H17 0.9500 . ?
C26 H26 0.9500 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C4 C3 1.353(3) . ?
C4 H4 0.9500 . ?
C50 C55 1.390(3) . ?
C50 C49 1.502(4) . ?
C18 C19 1.412(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.363(3) . ?
C19 H19 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C8 C9 1.407(3) . ?
C8 H8 0.9500 . ?
C55 C54 1.383(4) . ?
C55 H55 0.9500 . ?
C53 C54 1.383(4) . ?
C53 H53 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C54 H54 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C3 H3 0.9500 . ?
C10 C9 1.359(3) . ?
C10 H10 0.9500 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C9 H9 0.9500 . ?
C15 C20 1.410(3) . ?
C20 H20 0.9500 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Nb1 O2 C32 -28.8(3) . . . . ?
N5 Nb1 O2 C32 113.3(2) . . . . ?
O1 Nb1 O2 C32 -157.9(2) . . . . ?
N1 Nb1 O2 C32 -82.5(2) . . . . ?
N3 Nb1 O2 C32 33.8(2) . . . . ?
N2 Nb1 N3 C43 -24.37(13) . . . . ?
N5 Nb1 N3 C43 75.72(13) . . . . ?
O2 Nb1 N3 C43 -173.76(14) . . . . ?
O1 Nb1 N3 C43 145.62(17) . . . . ?
N1 Nb1 N3 C43 -97.68(13) . . . . ?
N2 Nb1 N3 C44 -140.83(12) . . . . ?
N5 Nb1 N3 C44 -40.74(12) . . . . ?
O2 Nb1 N3 C44 69.77(12) . . . . ?
O1 Nb1 N3 C44 29.2(2) . . . . ?
N1 Nb1 N3 C44 145.85(11) . . . . ?
N2 Nb1 N3 C42 96.05(12) . . . . ?
N5 Nb1 N3 C42 -163.86(12) . . . . ?
O2 Nb1 N3 C42 -53.35(11) . . . . ?
O1 Nb1 N3 C42 -94.0(2) . . . . ?
N1 Nb1 N3 C42 22.73(13) . . . . ?
N2 Nb1 O1 C23 -55.3(2) . . . . ?
N5 Nb1 O1 C23 -155.2(2) . . . . ?
O2 Nb1 O1 C23 96.6(2) . . . . ?
N1 Nb1 O1 C23 13.2(2) . . . . ?
N3 Nb1 O1 C23 135.3(2) . . . . ?
N5 Nb1 N2 C2 159.0(4) . . . . ?
O2 Nb1 N2 C2 -57.3(4) . . . . ?
O1 Nb1 N2 C2 67.3(4) . . . . ?
N1 Nb1 N2 C2 -1.3(4) . . . . ?
N3 Nb1 N2 C2 -116.0(4) . . . . ?
N2 Nb1 N1 C21 96.85(17) . . . . ?
N5 Nb1 N1 C21 18.4(3) . . . . ?
O2 Nb1 N1 C21 -111.68(16) . . . . ?
O1 Nb1 N1 C21 -18.13(16) . . . . ?
N3 Nb1 N1 C21 178.61(15) . . . . ?
N2 Nb1 N1 C12 -70.35(12) . . . . ?
N5 Nb1 N1 C12 -148.80(18) . . . . ?
O2 Nb1 N1 C12 81.12(12) . . . . ?
O1 Nb1 N1 C12 174.67(13) . . . . ?
N3 Nb1 N1 C12 11.40(13) . . . . ?
N2 Nb1 N5 C48 -1.4(2) . . . . ?
O2 Nb1 N5 C48 -160.45(18) . . . . ?
O1 Nb1 N5 C48 108.05(19) . . . . ?
N1 Nb1 N5 C48 72.8(3) . . . . ?
N3 Nb1 N5 C48 -89.01(19) . . . . ?
N2 Nb1 N5 C47 -174.06(17) . . . . ?
O2 Nb1 N5 C47 26.91(18) . . . . ?
O1 Nb1 N5 C47 -64.58(17) . . . . ?
N1 Nb1 N5 C47 -99.8(2) . . . . ?
N3 Nb1 N5 C47 98.35(17) . . . . ?
Nb1 O2 C32 C37 -14.7(3) . . . . ?
Nb1 O2 C32 C33 165.19(15) . . . . ?
C36 C37 C32 O2 179.34(17) . . . . ?
C42 C37 C32 O2 5.9(3) . . . . ?
C36 C37 C32 C33 -0.5(3) . . . . ?
C42 C37 C32 C33 -173.90(16) . . . . ?
C12 C11 C1 C2 -52.9(3) . . . . ?
C16 C11 C1 C2 125.32(19) . . . . ?
C12 C11 C1 C6 128.2(2) . . . . ?
C16 C11 C1 C6 -53.5(2) . . . . ?
Nb1 O1 C23 C22 -5.3(3) . . . . ?
Nb1 O1 C23 C24 175.16(14) . . . . ?
C27 C22 C23 O1 177.77(17) . . . . ?
C21 C22 C23 O1 -5.2(3) . . . . ?
C27 C22 C23 C24 -2.7(3) . . . . ?
C21 C22 C23 C24 174.33(16) . . . . ?
C46 N4 C42 N3 -65.1(2) . . . . ?
C45 N4 C42 N3 90.9(2) . . . . ?
C46 N4 C42 C37 65.8(2) . . . . ?
C45 N4 C42 C37 -138.25(18) . . . . ?
C43 N3 C42 N4 -40.6(2) . . . . ?
C44 N3 C42 N4 77.33(19) . . . . ?
Nb1 N3 C42 N4 -161.03(12) . . . . ?
C43 N3 C42 C37 -170.99(16) . . . . ?
C44 N3 C42 C37 -53.0(2) . . . . ?
Nb1 N3 C42 C37 68.61(16) . . . . ?
C36 C37 C42 N4 13.4(2) . . . . ?
C32 C37 C42 N4 -173.20(16) . . . . ?
C36 C37 C42 N3 146.24(17) . . . . ?
C32 C37 C42 N3 -40.4(2) . . . . ?
Nb1 N2 C2 C1 36.5(5) . . . . ?
Nb1 N2 C2 C3 -142.1(3) . . . . ?
C6 C1 C2 N2 -171.61(18) . . . . ?
C11 C1 C2 N2 9.5(3) . . . . ?
C6 C1 C2 C3 6.9(3) . . . . ?
C11 C1 C2 C3 -171.92(17) . . . . ?
C53 C52 C51 C50 -0.7(4) . . . . ?
C2 C1 C6 C7 170.56(18) . . . . ?
C11 C1 C6 C7 -10.6(3) . . . . ?
C2 C1 C6 C5 -7.2(3) . . . . ?
C11 C1 C6 C5 171.62(17) . . . . ?
C16 C11 C12 C13 4.0(3) . . . . ?
C1 C11 C12 C13 -177.69(16) . . . . ?
C16 C11 C12 N1 -171.98(16) . . . . ?
C1 C11 C12 N1 6.3(3) . . . . ?
C21 N1 C12 C11 -91.5(2) . . . . ?
Nb1 N1 C12 C11 77.24(19) . . . . ?
C21 N1 C12 C13 92.3(2) . . . . ?
Nb1 N1 C12 C13 -99.03(15) . . . . ?
C7 C6 C5 C4 -175.32(18) . . . . ?
C1 C6 C5 C4 2.6(3) . . . . ?
C7 C6 C5 C10 3.7(3) . . . . ?
C1 C6 C5 C10 -178.40(18) . . . . ?
O1 C23 C24 C25 -178.96(17) . . . . ?
C22 C23 C24 C25 1.5(3) . . . . ?
O1 C23 C24 C28 1.2(3) . . . . ?
C22 C23 C24 C28 -178.36(16) . . . . ?
C23 C24 C25 C26 0.6(3) . . . . ?
C28 C24 C25 C26 -179.53(18) . . . . ?
C12 N1 C21 C22 -175.53(17) . . . . ?
Nb1 N1 C21 C22 18.0(3) . . . . ?
C27 C22 C21 N1 174.18(18) . . . . ?
C23 C22 C21 N1 -2.9(3) . . . . ?
C11 C12 C13 C14 0.4(3) . . . . ?
N1 C12 C13 C14 176.65(17) . . . . ?
C12 C11 C16 C17 170.96(18) . . . . ?
C1 C11 C16 C17 -7.4(3) . . . . ?
C12 C11 C16 C15 -5.8(3) . . . . ?
C1 C11 C16 C15 175.84(17) . . . . ?
C5 C6 C7 C8 -2.2(3) . . . . ?
C1 C6 C7 C8 179.9(2) . . . . ?
C12 C13 C14 C15 -3.1(3) . . . . ?
C32 C37 C36 C35 2.3(3) . . . . ?
C42 C37 C36 C35 175.83(18) . . . . ?
C37 C36 C35 C34 -1.9(3) . . . . ?
C23 C22 C27 C26 1.7(3) . . . . ?
C21 C22 C27 C26 -175.41(18) . . . . ?
C25 C24 C28 C31 -2.1(3) . . . . ?
C23 C24 C28 C31 177.78(17) . . . . ?
C25 C24 C28 C29 -120.5(2) . . . . ?
C23 C24 C28 C29 59.4(2) . . . . ?
C25 C24 C28 C30 118.2(2) . . . . ?
C23 C24 C28 C30 -62.0(2) . . . . ?
C36 C35 C34 C33 -0.3(3) . . . . ?
C35 C34 C33 C32 2.0(3) . . . . ?
C35 C34 C33 C38 -177.78(19) . . . . ?
O2 C32 C33 C34 178.59(17) . . . . ?
C37 C32 C33 C34 -1.6(3) . . . . ?
O2 C32 C33 C38 -1.6(3) . . . . ?
C37 C32 C33 C38 178.21(17) . . . . ?
C41 C38 C33 C34 3.6(3) . . . . ?
C39 C38 C33 C34 123.5(2) . . . . ?
C40 C38 C33 C34 -114.9(2) . . . . ?
C41 C38 C33 C32 -176.19(19) . . . . ?
C39 C38 C33 C32 -56.3(2) . . . . ?
C40 C38 C33 C32 65.4(2) . . . . ?
C15 C16 C17 C18 -1.4(3) . . . . ?
C11 C16 C17 C18 -178.24(19) . . . . ?
C22 C27 C26 C25 0.4(3) . . . . ?
C24 C25 C26 C27 -1.6(3) . . . . ?
C10 C5 C4 C3 -176.6(2) . . . . ?
C6 C5 C4 C3 2.4(3) . . . . ?
C52 C51 C50 C55 0.3(3) . . . . ?
C52 C51 C50 C49 -178.6(2) . . . . ?
C16 C17 C18 C19 -1.0(3) . . . . ?
C17 C18 C19 C20 1.8(3) . . . . ?
C6 C7 C8 C9 -0.5(3) . . . . ?
C51 C50 C55 C54 0.2(3) . . . . ?
C49 C50 C55 C54 179.1(2) . . . . ?
C51 C52 C53 C54 0.6(4) . . . . ?
C50 C55 C54 C53 -0.3(3) . . . . ?
C52 C53 C54 C55 -0.1(4) . . . . ?
C5 C4 C3 C2 -2.7(3) . . . . ?
N2 C2 C3 C4 176.58(19) . . . . ?
C1 C2 C3 C4 -2.0(3) . . . . ?
C4 C5 C10 C9 176.4(2) . . . . ?
C6 C5 C10 C9 -2.6(3) . . . . ?
C5 C10 C9 C8 -0.1(3) . . . . ?
C7 C8 C9 C10 1.7(3) . . . . ?
C13 C14 C15 C20 -175.27(19) . . . . ?
C13 C14 C15 C16 1.1(3) . . . . ?
C17 C16 C15 C20 2.9(3) . . . . ?
C11 C16 C15 C20 179.86(18) . . . . ?
C17 C16 C15 C14 -173.58(18) . . . . ?
C11 C16 C15 C14 3.4(3) . . . . ?
C18 C19 C20 C15 -0.3(3) . . . . ?
C14 C15 C20 C19 174.3(2) . . . . ?
C16 C15 C20 C19 -2.1(3) . . . . ?
