#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:51:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179309 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/06/4320682.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_4320682
loop_
_publ_author_name
'Carlos Yélamos'
'Karl R. Gust'
'Anwar G. Baboul'
'Mary Jane Heeg'
'H. Bernhard Schlegel'
'Charles H. Winter'
_publ_section_title
;
 Early Transition Metal Complexes Containing 1,2,4-Triazolato and
 Tetrazolato Ligands: Synthesis, Structure, and Molecular Orbital Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6451
_journal_page_last               6462
_journal_paper_doi               10.1021/ic0109389
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C47 H67 N14 Nb'
_chemical_formula_weight         921.06
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 112.8500(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.6843(2)
_cell_length_b                   18.3911(3)
_cell_length_c                   13.1692(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    295(2)
_cell_volume                     2831.00(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Bruker P4/CCD'
_diffrn_measurement_method       'SMART CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16587
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       rhomboids
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_coef       0.0029(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.041
_refine_ls_goodness_of_fit_obs   1.107
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         10128
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_restrained_S_obs      1.107
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_obs          0.0523
_refine_ls_shift/esd_max         -0.419
_refine_ls_shift/esd_mean        0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0902P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1459
_refine_ls_wR_factor_obs         0.1388
_reflns_number_observed          8182
_reflns_number_total             10128
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0109389_6.cif
_cod_data_source_block           oran(11)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4320682
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Nb1 Nb 0.84735(3) 1.00010(3) 0.16572(3) 0.03234(12) Uani 1 d . .
N1 N 0.8832(4) 1.0777(3) 0.2908(4) 0.0365(11) Uani 1 d . .
N2 N 0.9686(3) 1.0758(2) 0.2507(3) 0.0385(9) Uani 1 d . .
C1 C 0.9164(5) 1.1200(3) 0.3790(4) 0.0473(12) Uani 1 d . .
C2 C 1.0234(5) 1.1462(3) 0.3959(5) 0.0552(14) Uani 1 d . .
H2 H 1.0670(5) 1.1772(3) 0.4525(5) 0.066 Uiso 1 calc R .
C3 C 1.0546(5) 1.1191(3) 0.3156(5) 0.0505(13) Uani 1 d . .
C4 C 0.8430(7) 1.1333(4) 0.4450(6) 0.072(2) Uani 1 d . .
C5 C 0.7877(8) 1.0621(4) 0.4574(8) 0.096(3) Uani 1 d . .
H5A H 0.7370(35) 1.0711(6) 0.4944(39) 0.115 Uiso 1 calc R .
H5B H 0.8460(9) 1.0284(11) 0.4997(36) 0.115 Uiso 1 calc R .
H5C H 0.7451(37) 1.0420(15) 0.3859(8) 0.115 Uiso 1 calc R .
C6 C 0.9190(9) 1.1598(7) 0.5609(7) 0.135(5) Uani 1 d . .
H6A H 0.8735(15) 1.1651(37) 0.6042(19) 0.162 Uiso 1 calc R .
H6B H 0.9522(47) 1.2059(19) 0.5558(8) 0.162 Uiso 1 calc R .
H6C H 0.9787(36) 1.1250(19) 0.5954(22) 0.162 Uiso 1 calc R .
C7 C 0.7503(9) 1.1897(5) 0.3826(10) 0.124(4) Uani 1 d . .
H7A H 0.7862(9) 1.2334(14) 0.3719(50) 0.149 Uiso 1 calc R .
H7B H 0.7052(38) 1.2006(28) 0.4248(28) 0.149 Uiso 1 calc R .
H7C H 0.7018(36) 1.1702(15) 0.3123(25) 0.149 Uiso 1 calc R .
C8 C 1.1637(7) 1.1296(5) 0.2964(8) 0.079(2) Uani 1 d . .
C9 C 1.2480(17) 1.1766(12) 0.3875(18) 0.105(6) Uiso 0.50 d P 1
H9A H 1.2466 1.1605 0.4607 0.126 Uiso 0.50 d P 1
H9B H 1.2296 1.2262 0.3800 0.126 Uiso 0.50 d P 1
H9C H 1.3256 1.1686 0.3947 0.126 Uiso 0.50 d P 1
C10 C 1.2544(22) 1.0671(16) 0.3672(24) 0.141(8) Uiso 0.50 d P 1
H10A H 1.2368 1.0517 0.4276 0.170 Uiso 0.50 d P 1
H10B H 1.3292 1.0822 0.3871 0.170 Uiso 0.50 d P 1
H10C H 1.2416 1.0235 0.3171 0.170 Uiso 0.50 d P 1
C11 C 1.1794(17) 1.0804(12) 0.2155(17) 0.106(6) Uiso 0.50 d P 1
H11A H 1.2104 1.0382 0.2428 0.127 Uiso 0.50 d P 1
H11B H 1.2255 1.1079 0.1811 0.127 Uiso 0.50 d P 1
H11C H 1.1032 1.0753 0.1534 0.127 Uiso 0.50 d P 1
C9' C 1.2124(13) 1.2049(8) 0.3290(13) 0.073(4) Uiso 0.50 d P 2
H9'1 H 1.2122 1.2153 0.4021 0.087 Uiso 0.50 d P 2
H9'2 H 1.1709 1.2391 0.2784 0.087 Uiso 0.50 d P 2
H9'3 H 1.2921 1.2040 0.3376 0.087 Uiso 0.50 d P 2
C10' C 1.2650(24) 1.1111(19) 0.4207(25) 0.156(9) Uiso 0.50 d P 2
H10D H 1.2392 1.1202 0.4734 0.187 Uiso 0.50 d P 2
H10E H 1.3324 1.1347 0.4252 0.187 Uiso 0.50 d P 2
H10F H 1.2793 1.0569 0.4169 0.187 Uiso 0.50 d P 2
C11' C 1.1419(17) 1.1258(12) 0.1767(17) 0.104(6) Uiso 0.50 d P 2
H11D H 1.0782 1.1633 0.1399 0.124 Uiso 0.50 d P 2
H11E H 1.1222 1.0830 0.1472 0.124 Uiso 0.50 d P 2
H11F H 1.2079 1.1480 0.1672 0.124 Uiso 0.50 d P 2
N3 N 0.9247(3) 0.9893(3) 0.0519(3) 0.0425(10) Uani 1 d . .
N4 N 0.9688(3) 0.9388(2) 0.1338(3) 0.0409(9) Uani 1 d . .
C12 C 0.9736(4) 0.9801(3) -0.0234(4) 0.0468(13) Uani 1 d . .
C13 C 1.0501(5) 0.9233(3) 0.0148(5) 0.0544(14) Uani 1 d . .
H13 H 1.0966(5) 0.9051(3) -0.0192(5) 0.065 Uiso 1 calc R .
C14 C 1.0462(4) 0.8979(3) 0.1116(4) 0.0433(11) Uani 1 d . .
C15 C 0.9479(5) 1.0254(3) -0.1227(5) 0.0568(15) Uani 1 d . .
C16 C 0.8480(8) 1.0787(5) -0.1376(7) 0.108(3) Uani 1 d . .
H16A H 0.8361(36) 1.1097(24) -0.1998(33) 0.130 Uiso 1 calc R .
H16B H 0.8667(23) 1.1078(22) -0.0724(22) 0.130 Uiso 1 calc R .
H16C H 0.7796(14) 1.0515(5) -0.1498(49) 0.130 Uiso 1 calc R .
C17 C 1.0573(7) 1.0645(6) -0.1157(7) 0.113(3) Uani 1 d . .
H17A H 1.0785(29) 1.1000(22) -0.0577(33) 0.136 Uiso 1 calc R .
H17B H 1.0440(17) 1.0883(28) -0.1844(18) 0.136 Uiso 1 calc R .
H17C H 1.1180(15) 1.0297(7) -0.1004(48) 0.136 Uiso 1 calc R .
C18 C 0.9061(9) 0.9736(5) -0.2257(7) 0.112(3) Uani 1 d . .
H18A H 0.8890(47) 1.0018(6) -0.2915(7) 0.134 Uiso 1 calc R .
H18B H 0.8386(30) 0.9482(24) -0.2294(28) 0.134 Uiso 1 calc R .
H18C H 0.9652(21) 0.9391(20) -0.2192(24) 0.134 Uiso 1 calc R .
C19 C 1.1127(5) 0.8357(3) 0.1855(6) 0.058(2) Uani 1 d . .
C20 C 1.1832(10) 0.7966(6) 0.1328(10) 0.139(4) Uani 1 d . .
H20A H 1.2175(55) 0.7543(24) 0.1754(37) 0.166 Uiso 1 calc R .
H20B H 1.2421(41) 0.8285(16) 0.1302(57) 0.166 Uiso 1 calc R .
H20C H 1.1348(15) 0.7823(36) 0.0593(26) 0.166 Uiso 1 calc R .
C21 C 1.0263(10) 0.7845(6) 0.2040(12) 0.163(6) Uani 1 d . .
H21A H 1.0573(35) 0.7670(39) 0.2785(23) 0.196 Uiso 1 calc R .
H21B H 1.0110(58) 0.7441(26) 0.1542(50) 0.196 Uiso 1 calc R .
H21C H 0.9564(30) 0.8103(15) 0.1908(75) 0.196 Uiso 1 calc R .
C22 C 1.1901(10) 0.8708(7) 0.2999(10) 0.140(5) Uani 1 d . .
H22A H 1.2235(56) 0.8330(7) 0.3530(20) 0.168 Uiso 1 calc R .
H22B H 1.1441(16) 0.9017(35) 0.3249(33) 0.168 Uiso 1 calc R .
H22C H 1.2497(41) 0.8990(35) 0.2912(17) 0.168 Uiso 1 calc R .
N5 N 0.7243(4) 0.9245(3) 0.0840(4) 0.0419(11) Uani 1 d . .
N6 N 0.6801(3) 0.9706(2) 0.1419(3) 0.0367(9) Uani 1 d . .
C23 C 0.6384(5) 0.8796(3) 0.0194(5) 0.0498(13) Uani 1 d . .
C24 C 0.5426(5) 0.8990(3) 0.0379(5) 0.058(2) Uani 1 d . .
H24 H 0.4710(5) 0.8773(3) 0.0052(5) 0.069 Uiso 1 calc R .
C25 C 0.5688(4) 0.9554(3) 0.1121(4) 0.0472(13) Uani 1 d . .
C26 C 0.6573(6) 0.8240(4) -0.0552(7) 0.072(2) Uani 1 d . .
C27 C 0.5433(8) 0.7960(6) -0.1396(9) 0.129(4) Uani 1 d . .
H27A H 0.4923(23) 0.7857(36) -0.1034(13) 0.155 Uiso 1 calc R .
H27B H 0.5563(12) 0.7523(22) -0.1731(44) 0.155 Uiso 1 calc R .
H27C H 0.5099(30) 0.8322(17) -0.1954(32) 0.155 Uiso 1 calc R .
C28 C 0.7320(12) 0.8530(6) -0.1097(10) 0.156(6) Uani 1 d . .
H28A H 0.7086(50) 0.9015(21) -0.1353(67) 0.188 Uiso 1 calc R .
H28B H 0.7254(64) 0.8225(31) -0.1711(49) 0.188 Uiso 1 calc R .
H28C H 0.8100(14) 0.8535(46) -0.0578(25) 0.188 Uiso 1 calc R .
C29 C 0.7194(11) 0.7572(6) 0.0193(9) 0.137(4) Uani 1 d . .
H29A H 0.7665(48) 0.7331(24) -0.0124(34) 0.164 Uiso 1 calc R .
H29B H 0.6632(11) 0.7237(20) 0.0237(48) 0.164 Uiso 1 calc R .
H29C H 0.7662(50) 0.7740(7) 0.0919(20) 0.164 Uiso 1 calc R .
C30 C 0.4928(4) 0.9959(5) 0.1559(4) 0.0611(13) Uani 1 d . .
C31 C 0.5254(7) 1.0753(4) 0.1737(8) 0.090(2) Uani 1 d . .
H31A H 0.4982(37) 1.0955(8) 0.2263(31) 0.108 Uiso 1 calc R .
H31B H 0.4915(35) 1.1009(7) 0.1052(11) 0.108 Uiso 1 calc R .
H31C H 0.6071(8) 1.0798(5) 0.2011(39) 0.108 Uiso 1 calc R .
C32 C 0.3667(5) 0.9837(6) 0.0747(7) 0.103(3) Uani 1 d . .
H32A H 0.3166(7) 1.0115(26) 0.0987(29) 0.123 Uiso 1 calc R .
H32B H 0.3480(16) 0.9331(8) 0.0732(36) 0.123 Uiso 1 calc R .
H32C H 0.3578(13) 0.9992(30) 0.0022(13) 0.123 Uiso 1 calc R .
C33 C 0.5087(6) 0.9624(5) 0.2654(6) 0.082(2) Uani 1 d . .
H33A H 0.4703(33) 0.9916(14) 0.3009(17) 0.098 Uiso 1 calc R .
H33B H 0.5888(7) 0.9601(23) 0.3110(15) 0.098 Uiso 1 calc R .
H33C H 0.4771(34) 0.9142(10) 0.2539(7) 0.098 Uiso 1 calc R .
N7 N 0.8935(4) 0.9308(3) 0.3126(4) 0.0407(12) Uani 1 d . .
N8 N 0.9855(3) 0.9428(2) 0.4049(3) 0.0446(10) Uani 1 d . .
N9 N 0.8838(5) 0.8514(3) 0.4269(4) 0.068(2) Uani 1 d . .
N10 N 0.8329(4) 0.8763(3) 0.3239(4) 0.0621(14) Uani 1 d . .
C34 C 0.9781(4) 0.8928(3) 0.4744(4) 0.0404(11) Uani 1 d . .
C35 C 1.0585(5) 0.8824(3) 0.5882(4) 0.0484(12) Uani 1 d . .
C36 C 1.0389(6) 0.8317(3) 0.6548(5) 0.0594(15) Uani 1 d . .
H36 H 0.9713(6) 0.8050(3) 0.6281(5) 0.071 Uiso 1 calc R .
C37 C 1.1168(7) 0.8191(4) 0.7602(5) 0.075(2) Uani 1 d . .
H37 H 1.1030(7) 0.7834(4) 0.8035(5) 0.090 Uiso 1 calc R .
C38 C 1.2136(6) 0.8592(5) 0.8003(6) 0.085(2) Uani 1 d . .
H38 H 1.2651(6) 0.8528(5) 0.8726(6) 0.102 Uiso 1 calc R .
C39 C 1.2357(7) 0.9089(5) 0.7347(6) 0.106(3) Uani 1 d . .
H39 H 1.3052(7) 0.9336(5) 0.7603(6) 0.128 Uiso 1 calc R .
C40 C 1.1560(6) 0.9230(4) 0.6308(6) 0.083(2) Uani 1 d . .
H40 H 1.1686(6) 0.9604(4) 0.5893(6) 0.100 Uiso 1 calc R .
N11 N 0.7510(4) 1.0887(2) 0.0607(4) 0.0425(11) Uani 1 d . .
N12 N 0.6507(3) 1.0799(2) -0.0240(3) 0.0433(10) Uani 1 d . .
N13 N 0.6912(4) 1.1957(3) 0.0001(5) 0.0563(13) Uani 1 d . .
N14 N 0.7776(4) 1.1601(2) 0.0783(4) 0.0552(12) Uani 1 d . .
C41 C 0.6184(5) 1.1466(3) -0.0566(4) 0.0406(12) Uani 1 d . .
C42 C 0.5040(5) 1.1643(3) -0.1468(5) 0.0547(15) Uani 1 d . .
C43 C 0.4227(6) 1.1125(4) -0.1835(6) 0.084(2) Uani 1 d . .
H43 H 0.4392(6) 1.0653(4) -0.1566(6) 0.101 Uiso 1 calc R .
C44 C 0.3139(7) 1.1289(5) -0.2618(7) 0.109(3) Uani 1 d . .
H44 H 0.2572(7) 1.0936(5) -0.2874(7) 0.131 Uiso 1 calc R .
C45 C 0.2936(7) 1.1995(5) -0.2997(7) 0.097(3) Uani 1 d . .
H45 H 0.2224(7) 1.2117(5) -0.3528(7) 0.117 Uiso 1 calc R .
C46 C 0.3724(7) 1.2495(5) -0.2627(7) 0.091(2) Uani 1 d . .
H46 H 0.3558(7) 1.2968(5) -0.2892(7) 0.109 Uiso 1 calc R .
C47 C 0.4809(5) 1.2335(4) -0.1843(6) 0.067(2) Uani 1 d . .
H47 H 0.5363(5) 1.2696(4) -0.1583(6) 0.081 Uiso 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'
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
N5 Nb1 N2 178.4(2) . . ?
N5 Nb1 N4 89.9(2) . . ?
N2 Nb1 N4 91.2(2) . . ?
N5 Nb1 N1 139.7(2) . . ?
N2 Nb1 N1 38.8(2) . . ?
N4 Nb1 N1 125.3(2) . . ?
N5 Nb1 N6 39.3(2) . . ?
N2 Nb1 N6 139.3(2) . . ?
N4 Nb1 N6 128.1(2) . . ?
N1 Nb1 N6 101.1(2) . . ?
N5 Nb1 N3 91.9(2) . . ?
N2 Nb1 N3 89.7(2) . . ?
N4 Nb1 N3 38.2(2) . . ?
N1 Nb1 N3 127.5(2) . . ?
N6 Nb1 N3 126.7(2) . . ?
N5 Nb1 N11 92.8(2) . . ?
N2 Nb1 N11 87.5(2) . . ?
N4 Nb1 N11 123.6(2) . . ?
N1 Nb1 N11 83.5(2) . . ?
N6 Nb1 N11 79.2(2) . . ?
N3 Nb1 N11 85.4(2) . . ?
N5 Nb1 N7 87.6(2) . . ?
N2 Nb1 N7 91.5(2) . . ?
N4 Nb1 N7 84.2(2) . . ?
N1 Nb1 N7 78.5(2) . . ?
N6 Nb1 N7 83.7(2) . . ?
N3 Nb1 N7 122.4(2) . . ?
N11 Nb1 N7 152.2(2) . . ?
C1 N1 N2 108.8(4) . . ?
C1 N1 Nb1 171.8(4) . . ?
N2 N1 Nb1 69.1(3) . . ?
C3 N2 N1 107.7(4) . . ?
C3 N2 Nb1 173.0(4) . . ?
N1 N2 Nb1 72.1(2) . . ?
N1 C1 C2 107.8(5) . . ?
N1 C1 C4 122.7(5) . . ?
C2 C1 C4 129.5(5) . . ?
C3 C2 C1 108.2(5) . . ?
N2 C3 C2 107.5(5) . . ?
N2 C3 C8 122.3(5) . . ?
C2 C3 C8 130.1(5) . . ?
C1 C4 C5 109.4(6) . . ?
C1 C4 C6 109.4(7) . . ?
C5 C4 C6 107.7(7) . . ?
C1 C4 C7 108.2(6) . . ?
C5 C4 C7 110.3(7) . . ?
C6 C4 C7 111.7(8) . . ?
C11' C8 C9' 103.3(12) . . ?
C11 C8 C3 115.7(9) . . ?
C11' C8 C3 111.4(9) . . ?
C9' C8 C3 111.7(8) . . ?
C11 C8 C9 131.8(12) . . ?
C3 C8 C9 110.4(10) . . ?
C11' C8 C10' 141.1(15) . . ?
C9' C8 C10' 80.5(13) . . ?
C3 C8 C10' 102.4(12) . . ?
C11 C8 C10 73.6(13) . . ?
C3 C8 C10 107.6(11) . . ?
C9 C8 C10 80.0(13) . . ?
C8 C10 C11 49.1(10) . . ?
C8 C11 C10 57.3(12) . . ?
C8 C9' C10' 53.4(10) . . ?
C8 C10' C9' 46.2(9) . . ?
N4 N3 C12 109.0(4) . . ?
N4 N3 Nb1 70.2(2) . . ?
C12 N3 Nb1 178.1(4) . . ?
C14 N4 N3 108.4(4) . . ?
C14 N4 Nb1 178.8(4) . . ?
N3 N4 Nb1 71.5(2) . . ?
N3 C12 C13 106.3(5) . . ?
N3 C12 C15 124.4(4) . . ?
C13 C12 C15 129.2(5) . . ?
C14 C13 C12 108.7(5) . . ?
N4 C14 C13 107.5(4) . . ?
N4 C14 C19 123.1(5) . . ?
C13 C14 C19 129.4(5) . . ?
C12 C15 C17 109.1(5) . . ?
C12 C15 C16 110.9(5) . . ?
C17 C15 C16 112.7(7) . . ?
C12 C15 C18 107.9(5) . . ?
C17 C15 C18 109.3(7) . . ?
C16 C15 C18 106.7(6) . . ?
C20 C19 C14 110.1(6) . . ?
C20 C19 C21 111.6(8) . . ?
C14 C19 C21 108.0(5) . . ?
C20 C19 C22 111.9(8) . . ?
C14 C19 C22 106.7(6) . . ?
C21 C19 C22 108.5(9) . . ?
C23 N5 N6 108.3(4) . . ?
C23 N5 Nb1 173.3(4) . . ?
N6 N5 Nb1 71.8(2) . . ?
C25 N6 N5 108.4(4) . . ?
C25 N6 Nb1 171.8(4) . . ?
N5 N6 Nb1 68.9(2) . . ?
N5 C23 C24 106.2(5) . . ?
N5 C23 C26 121.8(5) . . ?
C24 C23 C26 131.9(5) . . ?
C25 C24 C23 109.5(5) . . ?
N6 C25 C24 107.6(5) . . ?
N6 C25 C30 123.1(5) . . ?
C24 C25 C30 129.3(5) . . ?
C28 C26 C23 111.4(6) . . ?
C28 C26 C27 111.6(8) . . ?
C23 C26 C27 111.1(7) . . ?
C28 C26 C29 108.6(9) . . ?
C23 C26 C29 107.0(7) . . ?
C27 C26 C29 106.9(8) . . ?
C25 C30 C31 111.2(5) . . ?
C25 C30 C33 107.4(6) . . ?
C31 C30 C33 108.6(6) . . ?
C25 C30 C32 107.9(6) . . ?
C31 C30 C32 113.0(7) . . ?
C33 C30 C32 108.6(6) . . ?
N10 N7 N8 111.6(4) . . ?
N10 N7 Nb1 125.2(3) . . ?
N8 N7 Nb1 123.0(3) . . ?
C34 N8 N7 104.0(4) . . ?
N10 N9 C34 105.6(5) . . ?
N7 N10 N9 107.7(4) . . ?
N8 C34 N9 111.0(4) . . ?
N8 C34 C35 126.1(4) . . ?
N9 C34 C35 122.8(5) . . ?
C40 C35 C36 118.1(5) . . ?
C40 C35 C34 120.7(5) . . ?
C36 C35 C34 121.2(5) . . ?
C35 C36 C37 121.5(6) . . ?
C38 C37 C36 119.3(7) . . ?
C37 C38 C39 120.0(6) . . ?
C38 C39 C40 120.4(7) . . ?
C35 C40 C39 120.4(7) . . ?
N12 N11 N14 110.7(4) . . ?
N12 N11 Nb1 123.9(3) . . ?
N14 N11 Nb1 125.2(3) . . ?
C41 N12 N11 103.7(4) . . ?
C41 N13 N14 106.7(4) . . ?
N13 N14 N11 105.5(4) . . ?
N13 C41 N12 113.5(5) . . ?
N13 C41 C42 123.6(5) . . ?
N12 C41 C42 122.8(5) . . ?
C43 C42 C47 120.4(6) . . ?
C43 C42 C41 119.8(5) . . ?
C47 C42 C41 119.6(6) . . ?
C42 C43 C44 120.6(7) . . ?
C45 C44 C43 117.6(7) . . ?
C46 C45 C44 121.3(7) . . ?
C45 C46 C47 121.4(7) . . ?
C42 C47 C46 118.6(7) . . ?
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 N5 2.056(4) . ?
Nb1 N2 2.054(4) . ?
Nb1 N4 2.080(4) . ?
Nb1 N1 2.092(5) . ?
Nb1 N6 2.093(4) . ?
Nb1 N3 2.096(4) . ?
Nb1 N11 2.179(5) . ?
Nb1 N7 2.198(5) . ?
N1 C1 1.324(7) . ?
N1 N2 1.377(6) . ?
N2 C3 1.352(7) . ?
C1 C2 1.375(8) . ?
C1 C4 1.520(8) . ?
C2 C3 1.359(8) . ?
C3 C8 1.512(9) . ?
C4 C5 1.524(10) . ?
C4 C6 1.534(10) . ?
C4 C7 1.544(12) . ?
C8 C11 1.47(2) . ?
C8 C11' 1.49(2) . ?
C8 C9' 1.51(2) . ?
C8 C9 1.53(2) . ?
C8 C10' 1.68(3) . ?
C8 C10 1.64(3) . ?
C10 C11 1.87(3) . ?
C9' C10' 2.06(3) . ?
N3 N4 1.368(6) . ?
N3 C12 1.369(6) . ?
N4 C14 1.355(6) . ?
C12 C13 1.381(7) . ?
C12 C15 1.476(7) . ?
C13 C14 1.376(7) . ?
C14 C19 1.526(7) . ?
C15 C17 1.534(10) . ?
C15 C16 1.552(9) . ?
C15 C18 1.572(10) . ?
C19 C20 1.510(11) . ?
C19 C21 1.535(12) . ?
C19 C22 1.581(13) . ?
N5 C23 1.367(7) . ?
N5 N6 1.396(6) . ?
N6 C25 1.339(6) . ?
C23 C24 1.376(8) . ?
C23 C26 1.500(9) . ?
C24 C25 1.375(8) . ?
C25 C30 1.498(8) . ?
C26 C28 1.492(12) . ?
C26 C27 1.531(11) . ?
C26 C29 1.579(13) . ?
C30 C31 1.511(12) . ?
C30 C33 1.508(9) . ?
C30 C32 1.557(8) . ?
N7 N10 1.306(6) . ?
N7 N8 1.336(6) . ?
N8 C34 1.327(6) . ?
N9 N10 1.338(7) . ?
N9 C34 1.350(7) . ?
C34 C35 1.461(7) . ?
C35 C40 1.365(8) . ?
C35 C36 1.369(8) . ?
C36 C37 1.376(9) . ?
C37 C38 1.351(10) . ?
C38 C39 1.360(11) . ?
C39 C40 1.374(9) . ?
N11 N12 1.336(6) . ?
N11 N14 1.354(6) . ?
N12 C41 1.312(6) . ?
N13 C41 1.300(7) . ?
N13 N14 1.346(6) . ?
C41 C42 1.511(7) . ?
C42 C43 1.349(9) . ?
C42 C47 1.355(8) . ?
C43 C44 1.398(9) . ?
C44 C45 1.378(12) . ?
C45 C46 1.305(12) . ?
C46 C47 1.394(9) . ?
