#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:35:19 +0100 (vie 25 de mar de 2016) $
#$Revision: 179852 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/48/7014862.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_7014862
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         'C46 H52 N5 Nb O2'
_chemical_formula_sum            'C46 H52 N5 Nb O2'
_chemical_formula_weight         799.84
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.561(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.6800(18)
_cell_length_b                   13.465(2)
_cell_length_c                   13.696(2)
_cell_measurement_reflns_used    6935
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.5
_cell_volume                     2041.9(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0648
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26215
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_T_max  0.8879
_exptl_absorpt_correction_T_min  0.8709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.025(18)
_refine_ls_extinction_coef       0.0470(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         9650
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0277P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                8460
_reflns_number_total             9650
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT01229G.TXT
_cod_data_source_block           compound12
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7014862
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 1.145192(15) 0.151981(16) 0.904740(12) 0.01791(6) Uani 1 1 d . . .
O2 O 1.05070(13) 0.02501(12) 0.83794(11) 0.0199(3) Uani 1 1 d . . .
O1 O 0.97351(13) 0.21894(13) 0.90106(11) 0.0209(3) Uani 1 1 d . . .
N2 N 0.95870(17) -0.05707(14) 0.68472(14) 0.0193(4) Uani 1 1 d . . .
N1 N 1.00989(16) 0.21033(14) 0.75448(13) 0.0177(4) Uani 1 1 d . . .
N3 N 1.29467(17) 0.10924(15) 0.87895(15) 0.0256(4) Uani 1 1 d . . .
N4 N 1.15234(16) 0.10631(15) 1.04262(13) 0.0219(4) Uani 1 1 d . . .
N5 N 1.22122(16) 0.28585(15) 0.95100(14) 0.0217(4) Uani 1 1 d . . .
C1 C 0.81290(19) 0.07718(17) 0.61818(16) 0.0180(5) Uani 1 1 d . . .
C2 C 0.8459(2) -0.01233(17) 0.66871(16) 0.0183(5) Uani 1 1 d . . .
C3 C 0.7571(2) -0.0719(2) 0.6929(2) 0.0237(6) Uani 1 1 d . . .
H3 H 0.7806 -0.1329 0.7285 0.028 Uiso 1 1 calc R . .
C4 C 0.6397(2) -0.04280(19) 0.66589(18) 0.0256(5) Uani 1 1 d . . .
H4 H 0.5829 -0.0831 0.6841 0.031 Uiso 1 1 calc R . .
C5 C 0.6009(2) 0.04672(18) 0.61089(17) 0.0228(5) Uani 1 1 d . . .
C6 C 0.6879(2) 0.10745(18) 0.58581(17) 0.0208(5) Uani 1 1 d . . .
C7 C 0.6469(2) 0.19527(19) 0.52899(17) 0.0238(5) Uani 1 1 d . . .
H7 H 0.7033 0.2365 0.5113 0.029 Uiso 1 1 calc R . .
C8 C 0.5278(2) 0.2223(2) 0.49893(18) 0.0318(6) Uani 1 1 d . . .
H8 H 0.5025 0.2818 0.4610 0.038 Uiso 1 1 calc R . .
C9 C 0.4421(2) 0.1618(3) 0.52419(17) 0.0349(6) Uani 1 1 d . . .
H9 H 0.3595 0.1807 0.5031 0.042 Uiso 1 1 calc R . .
C10 C 0.4781(2) 0.0774(2) 0.57829(18) 0.0306(6) Uani 1 1 d . . .
H10 H 0.4199 0.0375 0.5950 0.037 Uiso 1 1 calc R . .
C11 C 0.90141(18) 0.1387(2) 0.58358(15) 0.0186(5) Uani 1 1 d . . .
C12 C 0.98708(19) 0.20130(17) 0.64640(16) 0.0189(5) Uani 1 1 d . . .
C13 C 1.0650(2) 0.25682(18) 0.60596(17) 0.0222(5) Uani 1 1 d . . .
H13 H 1.1248 0.2981 0.6510 0.027 Uiso 1 1 calc R . .
C14 C 1.0568(2) 0.25282(18) 0.50523(17) 0.0235(5) Uani 1 1 d . . .
H14 H 1.1076 0.2932 0.4797 0.028 Uiso 1 1 calc R . .
C15 C 0.9718(2) 0.18796(17) 0.43793(16) 0.0206(5) Uani 1 1 d . . .
C16 C 0.89606(18) 0.12925(15) 0.47679(15) 0.0185(5) Uani 1 1 d . . .
C17 C 0.8163(2) 0.06156(18) 0.40923(17) 0.0237(5) Uani 1 1 d . . .
H17 H 0.7673 0.0192 0.4347 0.028 Uiso 1 1 calc R . .
C18 C 0.8090(2) 0.0565(2) 0.30761(18) 0.0282(6) Uani 1 1 d . . .
H18 H 0.7550 0.0106 0.2634 0.034 Uiso 1 1 calc R . .
C19 C 0.8808(2) 0.11869(19) 0.26780(18) 0.0283(6) Uani 1 1 d . . .
H19 H 0.8730 0.1163 0.1966 0.034 Uiso 1 1 calc R . .
C20 C 0.9608(2) 0.18181(17) 0.33137(17) 0.0250(6) Uani 1 1 d . . .
H20 H 1.0102 0.2225 0.3046 0.030 Uiso 1 1 calc R . .
C31 C 1.0508(2) -0.03711(17) 0.76319(16) 0.0188(5) Uani 1 1 d . . .
C22 C 1.1645(2) -0.09297(17) 0.77178(17) 0.0204(5) Uani 1 1 d . . .
C23 C 1.20955(19) -0.09461(17) 0.68711(16) 0.0213(5) Uani 1 1 d . . .
C24 C 1.3102(2) -0.15295(18) 0.69447(18) 0.0246(5) Uani 1 1 d . . .
H24 H 1.3414 -0.1537 0.6383 0.029 Uiso 1 1 calc R . .
C25 C 1.3669(2) -0.21023(19) 0.78068(19) 0.0286(5) Uani 1 1 d . . .
C26 C 1.3212(2) -0.2070(2) 0.86207(19) 0.0297(6) Uani 1 1 d . . .
H26 H 1.3588 -0.2457 0.9217 0.036 Uiso 1 1 calc R . .
C27 C 1.2213(2) -0.14869(19) 0.85929(18) 0.0257(5) Uani 1 1 d . . .
C28 C 1.1517(2) -0.0369(2) 0.58940(17) 0.0261(5) Uani 1 1 d . . .
H28A H 1.2097 -0.0294 0.5515 0.039 Uiso 1 1 calc R . .
H28B H 1.1277 0.0288 0.6066 0.039 Uiso 1 1 calc R . .
H28C H 1.0803 -0.0727 0.5466 0.039 Uiso 1 1 calc R . .
C29 C 1.4706(2) -0.2768(2) 0.7825(2) 0.0418(7) Uani 1 1 d . . .
H29A H 1.5014 -0.3092 0.8499 0.063 Uiso 1 1 calc R . .
H29B H 1.5351 -0.2372 0.7701 0.063 Uiso 1 1 calc R . .
H29C H 1.4431 -0.3274 0.7287 0.063 Uiso 1 1 calc R . .
C30 C 1.1750(3) -0.1512(2) 0.9512(2) 0.0446(8) Uani 1 1 d . . .
H30A H 1.2022 -0.0915 0.9931 0.067 Uiso 1 1 calc R . .
H30B H 1.2065 -0.2103 0.9928 0.067 Uiso 1 1 calc R . .
H30C H 1.0866 -0.1534 0.9268 0.067 Uiso 1 1 calc R . .
C21 C 0.93308(19) 0.23568(17) 0.80274(16) 0.0182(5) Uani 1 1 d . . .
C32 C 0.8132(2) 0.28419(17) 0.76122(16) 0.0195(5) Uani 1 1 d . . .
C33 C 0.7150(2) 0.24311(18) 0.78673(17) 0.0215(5) Uani 1 1 d . . .
C34 C 0.6055(2) 0.2932(2) 0.75408(19) 0.0288(6) Uani 1 1 d . . .
H34 H 0.5385 0.2660 0.7699 0.035 Uiso 1 1 calc R . .
C35 C 0.5902(2) 0.3814(2) 0.6992(2) 0.0318(6) Uani 1 1 d . . .
C36 C 0.6892(2) 0.4217(2) 0.67772(18) 0.0290(6) Uani 1 1 d . . .
H36 H 0.6802 0.4826 0.6411 0.035 Uiso 1 1 calc R . .
C37 C 0.8007(2) 0.3749(2) 0.70852(18) 0.0226(6) Uani 1 1 d . . .
C38 C 0.72546(18) 0.1475(3) 0.84501(15) 0.0241(4) Uani 1 1 d . . .
H38A H 0.7657 0.1598 0.9185 0.036 Uiso 1 1 calc R . .
H38B H 0.7728 0.0999 0.8197 0.036 Uiso 1 1 calc R . .
H38C H 0.6446 0.1204 0.8349 0.036 Uiso 1 1 calc R . .
C39 C 0.4683(3) 0.4325(2) 0.6622(2) 0.0486(8) Uani 1 1 d . . .
H39A H 0.4767 0.4969 0.6318 0.073 Uiso 1 1 calc R . .
H39B H 0.4382 0.4427 0.7205 0.073 Uiso 1 1 calc R . .
H39C H 0.4113 0.3910 0.6102 0.073 Uiso 1 1 calc R . .
C40 C 0.9069(2) 0.42599(18) 0.68778(18) 0.0272(5) Uani 1 1 d . . .
H40A H 0.9796 0.4177 0.7475 0.041 Uiso 1 1 calc R . .
H40B H 0.8892 0.4969 0.6755 0.041 Uiso 1 1 calc R . .
H40C H 0.9202 0.3963 0.6270 0.041 Uiso 1 1 calc R . .
C41 C 1.3968(2) 0.0602(2) 0.9531(2) 0.0391(7) Uani 1 1 d . . .
H41A H 1.4124 -0.0033 0.9247 0.059 Uiso 1 1 calc R . .
H41B H 1.3783 0.0482 1.0171 0.059 Uiso 1 1 calc R . .
H41C H 1.4685 0.1026 0.9675 0.059 Uiso 1 1 calc R . .
C42 C 1.3188(2) 0.1271(2) 0.78207(19) 0.0361(7) Uani 1 1 d . . .
H42A H 1.3875 0.1725 0.7942 0.054 Uiso 1 1 calc R . .
H42B H 1.2473 0.1568 0.7321 0.054 Uiso 1 1 calc R . .
H42C H 1.3376 0.0640 0.7549 0.054 Uiso 1 1 calc R . .
C43 C 1.0552(2) 0.0433(2) 1.05623(18) 0.0309(6) Uani 1 1 d . . .
H43A H 1.0908 -0.0120 1.1024 0.046 Uiso 1 1 calc R . .
H43B H 1.0060 0.0172 0.9892 0.046 Uiso 1 1 calc R . .
H43C H 1.0043 0.0829 1.0861 0.046 Uiso 1 1 calc R . .
C44 C 1.2180(2) 0.1534(3) 1.14059(16) 0.0425(6) Uani 1 1 d . . .
H44A H 1.1608 0.1882 1.1677 0.064 Uiso 1 1 calc R . .
H44B H 1.2763 0.2011 1.1299 0.064 Uiso 1 1 calc R . .
H44C H 1.2609 0.1026 1.1899 0.064 Uiso 1 1 calc R . .
C45 C 1.1617(2) 0.3661(2) 0.9886(2) 0.0429(7) Uani 1 1 d . . .
H45A H 1.2158 0.3907 1.0545 0.064 Uiso 1 1 calc R . .
H45B H 1.0872 0.3410 0.9982 0.064 Uiso 1 1 calc R . .
H45C H 1.1421 0.4203 0.9383 0.064 Uiso 1 1 calc R . .
C46 C 1.3355(2) 0.3250(2) 0.9443(2) 0.0330(6) Uani 1 1 d . . .
H46A H 1.3189 0.3763 0.8909 0.050 Uiso 1 1 calc R . .
H46B H 1.3818 0.2711 0.9269 0.050 Uiso 1 1 calc R . .
H46C H 1.3821 0.3539 1.0108 0.050 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
N4 Nb1 N3 108.16(8) . . ?
N4 Nb1 N5 95.63(8) . . ?
N3 Nb1 N5 89.47(8) . . ?
N4 Nb1 O2 91.13(7) . . ?
N3 Nb1 O2 93.29(7) . . ?
N5 Nb1 O2 171.53(7) . . ?
N4 Nb1 O1 84.78(7) . . ?
N3 Nb1 O1 166.87(7) . . ?
N5 Nb1 O1 87.00(7) . . ?
O2 Nb1 O1 88.54(6) . . ?
N4 Nb1 N1 140.85(7) . . ?
N3 Nb1 N1 109.56(7) . . ?
N5 Nb1 N1 94.82(7) . . ?
O2 Nb1 N1 76.70(6) . . ?
O1 Nb1 N1 58.24(6) . . ?
N4 Nb1 C21 112.53(7) . . ?
N3 Nb1 C21 138.96(7) . . ?
N5 Nb1 C21 91.68(7) . . ?
O2 Nb1 C21 80.98(7) . . ?
O1 Nb1 C21 28.76(6) . . ?
N1 Nb1 C21 29.49(6) . . ?
C31 O2 Nb1 136.77(14) . . ?
C21 O1 Nb1 97.11(12) . . ?
C31 N2 C2 122.45(19) . . ?
C21 N1 C12 127.73(18) . . ?
C21 N1 Nb1 91.34(13) . . ?
C12 N1 Nb1 138.58(14) . . ?
C41 N3 C42 110.9(2) . . ?
C41 N3 Nb1 125.61(16) . . ?
C42 N3 Nb1 123.47(17) . . ?
C44 N4 C43 109.47(18) . . ?
C44 N4 Nb1 126.64(18) . . ?
C43 N4 Nb1 120.20(14) . . ?
C45 N5 C46 107.5(2) . . ?
C45 N5 Nb1 123.92(16) . . ?
C46 N5 Nb1 128.32(16) . . ?
C2 C1 C6 119.6(2) . . ?
C2 C1 C11 121.6(2) . . ?
C6 C1 C11 118.3(2) . . ?
C1 C2 N2 123.52(19) . . ?
C1 C2 C3 119.8(2) . . ?
N2 C2 C3 115.9(2) . . ?
C4 C3 C2 121.2(2) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 121.0(2) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C10 122.3(2) . . ?
C4 C5 C6 118.8(2) . . ?
C10 C5 C6 118.8(2) . . ?
C7 C6 C5 118.0(2) . . ?
C7 C6 C1 122.5(2) . . ?
C5 C6 C1 119.5(2) . . ?
C8 C7 C6 121.4(2) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C7 C8 C9 120.2(3) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C10 C9 C8 119.9(2) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C5 121.6(2) . . ?
C9 C10 H10 119.2 . . ?
C5 C10 H10 119.2 . . ?
C12 C11 C16 118.19(19) . . ?
C12 C11 C1 124.83(18) . . ?
C16 C11 C1 116.97(19) . . ?
C11 C12 C13 120.42(19) . . ?
C11 C12 N1 124.00(19) . . ?
C13 C12 N1 115.45(19) . . ?
C14 C13 C12 122.0(2) . . ?
C14 C13 H13 119.0 . . ?
C12 C13 H13 119.0 . . ?
C13 C14 C15 119.7(2) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C16 C15 C14 119.50(19) . . ?
C16 C15 C20 119.4(2) . . ?
C14 C15 C20 121.1(2) . . ?
C15 C16 C17 118.37(19) . . ?
C15 C16 C11 120.0(2) . . ?
C17 C16 C11 121.6(2) . . ?
C18 C17 C16 120.8(2) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C17 C18 C19 120.7(2) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C20 C19 C18 119.8(2) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C15 120.9(2) . . ?
C19 C20 H20 119.6 . . ?
C15 C20 H20 119.6 . . ?
N2 C31 O2 125.0(2) . . ?
N2 C31 C22 116.5(2) . . ?
O2 C31 C22 118.43(19) . . ?
C27 C22 C23 119.8(2) . . ?
C27 C22 C31 120.4(2) . . ?
C23 C22 C31 119.61(19) . . ?
C24 C23 C22 118.3(2) . . ?
C24 C23 C28 119.0(2) . . ?
C22 C23 C28 122.7(2) . . ?
C25 C24 C23 122.6(2) . . ?
C25 C24 H24 118.7 . . ?
C23 C24 H24 118.7 . . ?
C26 C25 C24 117.8(2) . . ?
C26 C25 C29 121.5(2) . . ?
C24 C25 C29 120.6(2) . . ?
C25 C26 C27 122.0(2) . . ?
C25 C26 H26 119.0 . . ?
C27 C26 H26 119.0 . . ?
C22 C27 C26 119.5(2) . . ?
C22 C27 C30 121.9(2) . . ?
C26 C27 C30 118.6(2) . . ?
C23 C28 H28A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C23 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C29 H29A 109.5 . . ?
C25 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C25 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O1 C21 N1 113.25(19) . . ?
O1 C21 C32 117.48(18) . . ?
N1 C21 C32 129.18(19) . . ?
O1 C21 Nb1 54.13(10) . . ?
N1 C21 Nb1 59.17(11) . . ?
C32 C21 Nb1 171.58(15) . . ?
C37 C32 C33 120.6(2) . . ?
C37 C32 C21 120.7(2) . . ?
C33 C32 C21 118.3(2) . . ?
C34 C33 C32 117.8(2) . . ?
C34 C33 C38 119.9(2) . . ?
C32 C33 C38 122.2(2) . . ?
C35 C34 C33 122.5(2) . . ?
C35 C34 H34 118.7 . . ?
C33 C34 H34 118.7 . . ?
C34 C35 C36 118.4(2) . . ?
C34 C35 C39 121.0(3) . . ?
C36 C35 C39 120.5(3) . . ?
C37 C36 C35 121.5(3) . . ?
C37 C36 H36 119.2 . . ?
C35 C36 H36 119.2 . . ?
C36 C37 C32 119.1(2) . . ?
C36 C37 C40 118.7(2) . . ?
C32 C37 C40 122.2(2) . . ?
C33 C38 H38A 109.5 . . ?
C33 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C33 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35 C39 H39A 109.5 . . ?
C35 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C35 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N3 C41 H41A 109.5 . . ?
N3 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
N3 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N3 C42 H42A 109.5 . . ?
N3 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N3 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N4 C43 H43A 109.5 . . ?
N4 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N4 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N4 C44 H44A 109.5 . . ?
N4 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N4 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N5 C45 H45A 109.5 . . ?
N5 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N5 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N5 C46 H46A 109.5 . . ?
N5 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N5 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
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 N4 1.9623(18) . ?
Nb1 N3 1.9740(19) . ?
Nb1 N5 2.020(2) . ?
Nb1 O2 2.0821(15) . ?
Nb1 O1 2.1845(15) . ?
Nb1 N1 2.2977(18) . ?
Nb1 C21 2.675(2) . ?
O2 C31 1.322(3) . ?
O1 C21 1.297(2) . ?
N2 C31 1.284(3) . ?
N2 C2 1.401(3) . ?
N1 C21 1.317(3) . ?
N1 C12 1.423(3) . ?
N3 C41 1.456(3) . ?
N3 C42 1.461(3) . ?
N4 C44 1.461(3) . ?
N4 C43 1.475(3) . ?
N5 C45 1.464(3) . ?
N5 C46 1.465(3) . ?
C1 C2 1.382(3) . ?
C1 C6 1.443(3) . ?
C1 C11 1.514(3) . ?
C2 C3 1.432(3) . ?
C3 C4 1.359(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.417(3) . ?
C4 H4 0.9500 . ?
C5 C10 1.421(3) . ?
C5 C6 1.429(3) . ?
C6 C7 1.413(3) . ?
C7 C8 1.369(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.416(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.348(4) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.380(3) . ?
C11 C16 1.449(3) . ?
C12 C13 1.420(3) . ?
C13 C14 1.353(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.419(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.411(3) . ?
C15 C20 1.426(3) . ?
C16 C17 1.416(3) . ?
C17 C18 1.369(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.412(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.355(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C31 C22 1.498(3) . ?
C22 C27 1.391(3) . ?
C22 C23 1.418(3) . ?
C23 C24 1.391(3) . ?
C23 C28 1.508(3) . ?
C24 C25 1.389(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.382(3) . ?
C25 C29 1.501(3) . ?
C26 C27 1.397(3) . ?
C26 H26 0.9500 . ?
C27 C30 1.520(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C21 C32 1.485(3) . ?
C32 C37 1.402(3) . ?
C32 C33 1.413(3) . ?
C33 C34 1.388(3) . ?
C33 C38 1.499(4) . ?
C34 C35 1.386(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.391(4) . ?
C35 C39 1.516(3) . ?
C36 C37 1.386(3) . ?
C36 H36 0.9500 . ?
C37 C40 1.522(3) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
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
N4 Nb1 O2 C31 -139.7(2) . . . . ?
N3 Nb1 O2 C31 -31.4(2) . . . . ?
N5 Nb1 O2 C31 77.4(5) . . . . ?
O1 Nb1 O2 C31 135.6(2) . . . . ?
N1 Nb1 O2 C31 77.9(2) . . . . ?
C21 Nb1 O2 C31 107.7(2) . . . . ?
N4 Nb1 O1 C21 -165.04(14) . . . . ?
N3 Nb1 O1 C21 24.4(4) . . . . ?
N5 Nb1 O1 C21 99.02(14) . . . . ?
O2 Nb1 O1 C21 -73.77(13) . . . . ?
N1 Nb1 O1 C21 1.46(12) . . . . ?
N4 Nb1 N1 C21 20.16(19) . . . . ?
N3 Nb1 N1 C21 -176.03(13) . . . . ?
N5 Nb1 N1 C21 -84.88(14) . . . . ?
O2 Nb1 N1 C21 95.20(13) . . . . ?
O1 Nb1 N1 C21 -1.43(12) . . . . ?
N4 Nb1 N1 C12 -142.0(2) . . . . ?
N3 Nb1 N1 C12 21.8(2) . . . . ?
N5 Nb1 N1 C12 113.0(2) . . . . ?
O2 Nb1 N1 C12 -66.9(2) . . . . ?
O1 Nb1 N1 C12 -163.6(2) . . . . ?
C21 Nb1 N1 C12 -162.1(3) . . . . ?
N4 Nb1 N3 C41 -5.0(2) . . . . ?
N5 Nb1 N3 C41 90.8(2) . . . . ?
O2 Nb1 N3 C41 -97.2(2) . . . . ?
O1 Nb1 N3 C41 165.1(3) . . . . ?
N1 Nb1 N3 C41 -174.3(2) . . . . ?
C21 Nb1 N3 C41 -177.27(18) . . . . ?
N4 Nb1 N3 C42 177.66(18) . . . . ?
N5 Nb1 N3 C42 -86.59(19) . . . . ?
O2 Nb1 N3 C42 85.39(18) . . . . ?
O1 Nb1 N3 C42 -12.3(4) . . . . ?
N1 Nb1 N3 C42 8.3(2) . . . . ?
C21 Nb1 N3 C42 5.4(2) . . . . ?
N3 Nb1 N4 C44 80.1(2) . . . . ?
N5 Nb1 N4 C44 -11.2(2) . . . . ?
O2 Nb1 N4 C44 174.0(2) . . . . ?
O1 Nb1 N4 C44 -97.6(2) . . . . ?
N1 Nb1 N4 C44 -115.9(2) . . . . ?
C21 Nb1 N4 C44 -105.3(2) . . . . ?
N3 Nb1 N4 C43 -123.89(18) . . . . ?
N5 Nb1 N4 C43 144.82(18) . . . . ?
O2 Nb1 N4 C43 -30.06(18) . . . . ?
O1 Nb1 N4 C43 58.37(18) . . . . ?
N1 Nb1 N4 C43 40.1(2) . . . . ?
C21 Nb1 N4 C43 50.6(2) . . . . ?
N4 Nb1 N5 C45 -70.0(2) . . . . ?
N3 Nb1 N5 C45 -178.2(2) . . . . ?
O2 Nb1 N5 C45 72.7(5) . . . . ?
O1 Nb1 N5 C45 14.5(2) . . . . ?
N1 Nb1 N5 C45 72.2(2) . . . . ?
C21 Nb1 N5 C45 42.8(2) . . . . ?
N4 Nb1 N5 C46 116.8(2) . . . . ?
N3 Nb1 N5 C46 8.6(2) . . . . ?
O2 Nb1 N5 C46 -100.5(5) . . . . ?
O1 Nb1 N5 C46 -158.8(2) . . . . ?
N1 Nb1 N5 C46 -101.0(2) . . . . ?
C21 Nb1 N5 C46 -130.4(2) . . . . ?
C6 C1 C2 N2 166.8(2) . . . . ?
C11 C1 C2 N2 -5.2(3) . . . . ?
C6 C1 C2 C3 -3.0(3) . . . . ?
C11 C1 C2 C3 -175.1(2) . . . . ?
C31 N2 C2 C1 87.3(3) . . . . ?
C31 N2 C2 C3 -102.5(3) . . . . ?
C1 C2 C3 C4 0.9(4) . . . . ?
N2 C2 C3 C4 -169.7(2) . . . . ?
C2 C3 C4 C5 1.3(4) . . . . ?
C3 C4 C5 C10 177.7(2) . . . . ?
C3 C4 C5 C6 -1.2(3) . . . . ?
C4 C5 C6 C7 178.6(2) . . . . ?
C10 C5 C6 C7 -0.3(3) . . . . ?
C4 C5 C6 C1 -0.9(3) . . . . ?
C10 C5 C6 C1 -179.9(2) . . . . ?
C2 C1 C6 C7 -176.48(19) . . . . ?
C11 C1 C6 C7 -4.1(3) . . . . ?
C2 C1 C6 C5 3.0(3) . . . . ?
C11 C1 C6 C5 175.37(19) . . . . ?
C5 C6 C7 C8 0.3(3) . . . . ?
C1 C6 C7 C8 179.8(2) . . . . ?
C6 C7 C8 C9 -0.2(4) . . . . ?
C7 C8 C9 C10 0.2(4) . . . . ?
C8 C9 C10 C5 -0.2(4) . . . . ?
C4 C5 C10 C9 -178.6(2) . . . . ?
C6 C5 C10 C9 0.3(3) . . . . ?
C2 C1 C11 C12 -80.9(3) . . . . ?
C6 C1 C11 C12 106.9(3) . . . . ?
C2 C1 C11 C16 98.1(2) . . . . ?
C6 C1 C11 C16 -74.1(3) . . . . ?
C16 C11 C12 C13 1.8(3) . . . . ?
C1 C11 C12 C13 -179.2(2) . . . . ?
C16 C11 C12 N1 -173.77(19) . . . . ?
C1 C11 C12 N1 5.2(4) . . . . ?
C21 N1 C12 C11 -58.2(3) . . . . ?
Nb1 N1 C12 C11 99.0(3) . . . . ?
C21 N1 C12 C13 126.0(2) . . . . ?
Nb1 N1 C12 C13 -76.8(3) . . . . ?
C11 C12 C13 C14 1.7(3) . . . . ?
N1 C12 C13 C14 177.7(2) . . . . ?
C12 C13 C14 C15 -3.0(4) . . . . ?
C13 C14 C15 C16 0.7(3) . . . . ?
C13 C14 C15 C20 -179.9(2) . . . . ?
C14 C15 C16 C17 -176.9(2) . . . . ?
C20 C15 C16 C17 3.7(3) . . . . ?
C14 C15 C16 C11 2.8(3) . . . . ?
C20 C15 C16 C11 -176.6(2) . . . . ?
C12 C11 C16 C15 -4.0(3) . . . . ?
C1 C11 C16 C15 176.9(2) . . . . ?
C12 C11 C16 C17 175.7(2) . . . . ?
C1 C11 C16 C17 -3.4(3) . . . . ?
C15 C16 C17 C18 -2.9(3) . . . . ?
C11 C16 C17 C18 177.4(2) . . . . ?
C16 C17 C18 C19 -0.1(4) . . . . ?
C17 C18 C19 C20 2.3(4) . . . . ?
C18 C19 C20 C15 -1.4(4) . . . . ?
C16 C15 C20 C19 -1.6(3) . . . . ?
C14 C15 C20 C19 179.0(2) . . . . ?
C2 N2 C31 O2 1.3(3) . . . . ?
C2 N2 C31 C22 178.22(19) . . . . ?
Nb1 O2 C31 N2 -123.2(2) . . . . ?
Nb1 O2 C31 C22 59.9(3) . . . . ?
N2 C31 C22 C27 -123.5(2) . . . . ?
O2 C31 C22 C27 53.7(3) . . . . ?
N2 C31 C22 C23 52.1(3) . . . . ?
O2 C31 C22 C23 -130.8(2) . . . . ?
C27 C22 C23 C24 0.2(3) . . . . ?
C31 C22 C23 C24 -175.4(2) . . . . ?
C27 C22 C23 C28 179.3(2) . . . . ?
C31 C22 C23 C28 3.8(3) . . . . ?
C22 C23 C24 C25 0.8(4) . . . . ?
C28 C23 C24 C25 -178.4(2) . . . . ?
C23 C24 C25 C26 -0.9(4) . . . . ?
C23 C24 C25 C29 176.3(2) . . . . ?
C24 C25 C26 C27 0.0(4) . . . . ?
C29 C25 C26 C27 -177.1(3) . . . . ?
C23 C22 C27 C26 -1.0(4) . . . . ?
C31 C22 C27 C26 174.5(2) . . . . ?
C23 C22 C27 C30 -178.7(2) . . . . ?
C31 C22 C27 C30 -3.2(4) . . . . ?
C25 C26 C27 C22 0.9(4) . . . . ?
C25 C26 C27 C30 178.7(3) . . . . ?
Nb1 O1 C21 N1 -2.4(2) . . . . ?
Nb1 O1 C21 C32 -179.29(17) . . . . ?
C12 N1 C21 O1 167.4(2) . . . . ?
Nb1 N1 C21 O1 2.23(19) . . . . ?
C12 N1 C21 C32 -16.2(4) . . . . ?
Nb1 N1 C21 C32 178.7(2) . . . . ?
C12 N1 C21 Nb1 165.1(2) . . . . ?
N4 Nb1 C21 O1 16.16(15) . . . . ?
N3 Nb1 C21 O1 -171.77(14) . . . . ?
N5 Nb1 C21 O1 -80.64(13) . . . . ?
O2 Nb1 C21 O1 103.62(13) . . . . ?
N1 Nb1 C21 O1 -177.5(2) . . . . ?
N4 Nb1 C21 N1 -166.37(13) . . . . ?
N3 Nb1 C21 N1 5.70(19) . . . . ?
N5 Nb1 C21 N1 96.83(14) . . . . ?
O2 Nb1 C21 N1 -78.91(13) . . . . ?
O1 Nb1 C21 N1 177.5(2) . . . . ?
N4 Nb1 C21 C32 20.5(11) . . . . ?
N3 Nb1 C21 C32 -167.4(11) . . . . ?
N5 Nb1 C21 C32 -76.3(11) . . . . ?
O2 Nb1 C21 C32 108.0(11) . . . . ?
O1 Nb1 C21 C32 4.3(10) . . . . ?
N1 Nb1 C21 C32 -173.1(12) . . . . ?
O1 C21 C32 C37 121.1(2) . . . . ?
N1 C21 C32 C37 -55.3(3) . . . . ?
Nb1 C21 C32 C37 117.1(10) . . . . ?
O1 C21 C32 C33 -51.4(3) . . . . ?
N1 C21 C32 C33 132.2(2) . . . . ?
Nb1 C21 C32 C33 -55.4(12) . . . . ?
C37 C32 C33 C34 2.7(3) . . . . ?
C21 C32 C33 C34 175.2(2) . . . . ?
C37 C32 C33 C38 -178.6(2) . . . . ?
C21 C32 C33 C38 -6.1(3) . . . . ?
C32 C33 C34 C35 -0.8(3) . . . . ?
C38 C33 C34 C35 -179.5(2) . . . . ?
C33 C34 C35 C36 -1.0(4) . . . . ?
C33 C34 C35 C39 178.2(2) . . . . ?
C34 C35 C36 C37 1.0(4) . . . . ?
C39 C35 C36 C37 -178.3(2) . . . . ?
C35 C36 C37 C32 0.9(4) . . . . ?
C35 C36 C37 C40 -176.6(2) . . . . ?
C33 C32 C37 C36 -2.8(3) . . . . ?
C21 C32 C37 C36 -175.1(2) . . . . ?
C33 C32 C37 C40 174.6(2) . . . . ?
C21 C32 C37 C40 2.3(3) . . . . ?
