#------------------------------------------------------------------------------
#$Date: 2020-10-10 04:31:56 +0300 (Sat, 10 Oct 2020) $
#$Revision: 258285 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/93/1559329.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_1559329
loop_
_publ_author_name
'Fostvedt, Jade I.'
'Grant, Lauren N.'
'Kriegel, Benjamin M.'
'Obenhuber, Andreas H.'
'Lohrey, Trevor D.'
'Bergman, Robert G.'
'Arnold, John'
_publ_section_title
;
 1,2-Addition and cycloaddition reactions of niobium bis(imido) and oxo
 imido complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03489D
_journal_year                    2020
_chemical_formula_moiety         'C87 H121 N7 Nb2 O2, C4 H10 O'
_chemical_formula_sum            'C91 H131 N7 Nb2 O3'
_chemical_formula_weight         1556.84
_chemical_name_common            (κ1-BDI)Nb(Py)(NAr)-(μ-O)2-(NAr)Nb(BDI)
_chemical_name_systematic
'bis(μ2-oxido)-bis(2,6-diisopropylphenyl)imino-(N-(4-((2,6-diisopropylphenyl)imino)pent-2-en-2-yl)-2,6-diisopropylanilido)-pyridine-(N,N?-bis(2,6-diisopropylphenyl)-3,5-dimethyl-B-diketiminato)-diniobium(V) diethyl ether solvate'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-05-14
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-15 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.6670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6394(12)
_cell_length_b                   20.8107(13)
_cell_length_c                   25.0878(15)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.29
_cell_volume                     9050.3(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.989
_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  0.0546
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            83162
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.359
_diffrn_reflns_theta_min         1.280
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6621
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0497 before and 0.0413 after correction.
The Ratio of minimum to maximum transmission is 0.8885.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       block
_exptl_crystal_F_000             3328
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl ether'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         16411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0729P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12436
_reflns_number_total             16411
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc03489d2.cif
_cod_data_source_block           bmkxr72
_cod_database_code               1559329
_shelx_shelxl_version_number     2018/3
_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_max   0.970
_shelx_estimated_absorpt_t_min   0.948
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C36(H36), C39(H39), C53(H53),
 C56(H56), C65(H65), C68(H68), C77(H77), C80(H80)
2.b Secondary CH2 refined with riding coordinates:
 C89(H89A,H89B), C90(H90A,H90B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C32(H32),
 C33(H33), C34(H34), C43(H43), C49(H49), C50(H50), C51(H51), C61(H61), C62(H62),
  C63(H63), C73(H73), C74(H74), C75(H75), C83(H83), C84(H84), C85(H85),
 C86(H86), C87(H87)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C69(H69A,
 H69B,H69C), C70(H70A,H70B,H70C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C),
 C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), C88(H88A,H88B,H88C), C91(H91A,H91B,
 H91C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.46108(15) 0.19246(12) 0.02562(11) 0.0181(6) Uani 1 1 d . . . . .
C2 C 0.45547(16) 0.25291(12) 0.00065(12) 0.0194(6) Uani 1 1 d . . . . .
H2 H 0.439755 0.252796 -0.037674 0.023 Uiso 1 1 calc R . . . .
C3 C 0.46989(15) 0.31332(12) 0.02460(11) 0.0177(6) Uani 1 1 d . . . . .
C4 C 0.43202(17) 0.13630(12) -0.01124(11) 0.0241(7) Uani 1 1 d . . . . .
H4A H 0.475347 0.108092 -0.014658 0.036 Uiso 1 1 calc GR . . . .
H4B H 0.408270 0.152503 -0.047133 0.036 Uiso 1 1 calc GR . . . .
H4C H 0.393695 0.112090 0.004297 0.036 Uiso 1 1 calc GR . . . .
C5 C 0.44933(17) 0.37024(12) -0.01308(12) 0.0241(7) Uani 1 1 d . . . . .
H5A H 0.415867 0.399697 0.002420 0.036 Uiso 1 1 calc GR . . . .
H5B H 0.422262 0.355051 -0.048497 0.036 Uiso 1 1 calc GR . . . .
H5C H 0.496581 0.392738 -0.017498 0.036 Uiso 1 1 calc GR . . . .
C6 C 0.47880(16) 0.11791(12) 0.09771(11) 0.0207(6) Uani 1 1 d . . . . .
C7 C 0.53340(17) 0.06898(12) 0.09393(11) 0.0222(6) Uani 1 1 d . . . . .
C8 C 0.51392(18) 0.00643(13) 0.10661(12) 0.0255(7) Uani 1 1 d . . . . .
H8 H 0.549375 -0.027391 0.104386 0.031 Uiso 1 1 calc R . . . .
C9 C 0.44524(18) -0.00762(13) 0.12215(12) 0.0288(7) Uani 1 1 d . . . . .
H9 H 0.433098 -0.050743 0.129740 0.035 Uiso 1 1 calc R . . . .
C10 C 0.39372(18) 0.04128(13) 0.12674(12) 0.0263(7) Uani 1 1 d . . . . .
H10 H 0.346458 0.031353 0.137905 0.032 Uiso 1 1 calc R . . . .
C11 C 0.40981(16) 0.10477(12) 0.11529(11) 0.0211(6) Uani 1 1 d . . . . .
C12 C 0.61011(17) 0.08195(12) 0.07691(12) 0.0232(6) Uani 1 1 d . . . . .
H12 H 0.608290 0.126162 0.061113 0.028 Uiso 1 1 calc R . . . .
C13 C 0.62821(18) 0.03429(13) 0.03394(12) 0.0290(7) Uani 1 1 d . . . . .
H13A H 0.638539 -0.008268 0.050399 0.044 Uiso 1 1 calc GR . . . .
H13B H 0.673633 0.049134 0.020127 0.044 Uiso 1 1 calc GR . . . .
H13C H 0.583949 0.031710 0.003968 0.044 Uiso 1 1 calc GR . . . .
C14 C 0.67499(17) 0.08023(13) 0.12708(12) 0.0275(7) Uani 1 1 d . . . . .
H14A H 0.664503 0.112134 0.153523 0.041 Uiso 1 1 calc GR . . . .
H14B H 0.724322 0.090137 0.116279 0.041 Uiso 1 1 calc GR . . . .
H14C H 0.677524 0.037340 0.143436 0.041 Uiso 1 1 calc GR . . . .
C15 C 0.35067(16) 0.15729(13) 0.11993(11) 0.0230(6) Uani 1 1 d . . . . .
H15 H 0.378869 0.199193 0.124574 0.028 Uiso 1 1 calc R . . . .
C16 C 0.28856(18) 0.16235(16) 0.06846(13) 0.0377(8) Uani 1 1 d . . . . .
H16A H 0.312188 0.177068 0.038211 0.057 Uiso 1 1 calc GR . . . .
H16B H 0.248933 0.193102 0.074497 0.057 Uiso 1 1 calc GR . . . .
H16C H 0.264906 0.120112 0.059799 0.057 Uiso 1 1 calc GR . . . .
C17 C 0.31179(17) 0.14816(14) 0.16939(12) 0.0290(7) Uani 1 1 d . . . . .
H17A H 0.276348 0.111523 0.163116 0.043 Uiso 1 1 calc GR . . . .
H17B H 0.282948 0.187080 0.174929 0.043 Uiso 1 1 calc GR . . . .
H17C H 0.351270 0.140047 0.201664 0.043 Uiso 1 1 calc GR . . . .
C18 C 0.49552(16) 0.38850(12) 0.09605(11) 0.0190(6) Uani 1 1 d . . . . .
C19 C 0.42786(16) 0.40783(13) 0.11363(12) 0.0229(6) Uani 1 1 d . . . . .
C20 C 0.42214(18) 0.47213(13) 0.12796(12) 0.0285(7) Uani 1 1 d . . . . .
H20 H 0.376605 0.486499 0.139410 0.034 Uiso 1 1 calc R . . . .
C21 C 0.48087(18) 0.51562(13) 0.12599(12) 0.0298(7) Uani 1 1 d . . . . .
H21 H 0.475449 0.559223 0.135866 0.036 Uiso 1 1 calc R . . . .
C22 C 0.54707(18) 0.49533(13) 0.10967(12) 0.0276(7) Uani 1 1 d . . . . .
H22 H 0.587480 0.525269 0.108812 0.033 Uiso 1 1 calc R . . . .
C23 C 0.55642(16) 0.43152(12) 0.09425(11) 0.0217(6) Uani 1 1 d . . . . .
C24 C 0.36173(16) 0.36193(13) 0.11616(12) 0.0258(7) Uani 1 1 d . . . . .
H24 H 0.384607 0.318510 0.125608 0.031 Uiso 1 1 calc R . . . .
C25 C 0.30480(18) 0.35547(16) 0.06190(13) 0.0356(8) Uani 1 1 d . . . . .
H25A H 0.287263 0.398250 0.048672 0.053 Uiso 1 1 calc GR . . . .
H25B H 0.260339 0.329696 0.067286 0.053 Uiso 1 1 calc GR . . . .
H25C H 0.330600 0.334364 0.035232 0.053 Uiso 1 1 calc GR . . . .
C26 C 0.31580(18) 0.38036(15) 0.16020(13) 0.0342(8) Uani 1 1 d . . . . .
H26A H 0.351583 0.391741 0.193588 0.051 Uiso 1 1 calc GR . . . .
H26B H 0.283913 0.343892 0.167247 0.051 Uiso 1 1 calc GR . . . .
H26C H 0.282570 0.417222 0.147886 0.051 Uiso 1 1 calc GR . . . .
C27 C 0.63039(17) 0.41315(12) 0.07527(12) 0.0248(7) Uani 1 1 d . . . . .
H27 H 0.624575 0.367791 0.061987 0.030 Uiso 1 1 calc R . . . .
C28 C 0.64590(19) 0.45514(13) 0.02797(13) 0.0311(7) Uani 1 1 d . . . . .
H28A H 0.600233 0.455175 -0.000998 0.047 Uiso 1 1 calc GR . . . .
H28B H 0.690038 0.437796 0.013995 0.047 Uiso 1 1 calc GR . . . .
H28C H 0.657314 0.499190 0.040788 0.047 Uiso 1 1 calc GR . . . .
C29 C 0.70007(18) 0.41532(14) 0.12223(13) 0.0313(7) Uani 1 1 d . . . . .
H29A H 0.704508 0.458399 0.138279 0.047 Uiso 1 1 calc GR . . . .
H29B H 0.747175 0.405176 0.108465 0.047 Uiso 1 1 calc GR . . . .
H29C H 0.692934 0.383759 0.149871 0.047 Uiso 1 1 calc GR . . . .
C30 C 0.72066(16) 0.22444(12) 0.07135(12) 0.0224(6) Uani 1 1 d . . . . .
C31 C 0.71027(16) 0.21648(14) 0.01424(12) 0.0253(7) Uani 1 1 d . . . . .
C32 C 0.77314(19) 0.19984(17) -0.00932(14) 0.0395(8) Uani 1 1 d . . . . .
H32 H 0.766012 0.194492 -0.047526 0.047 Uiso 1 1 calc R . . . .
C33 C 0.8456(2) 0.19096(19) 0.02176(15) 0.0477(10) Uani 1 1 d . . . . .
H33 H 0.887966 0.179963 0.005068 0.057 Uiso 1 1 calc R . . . .
C34 C 0.85577(19) 0.19821(17) 0.07710(14) 0.0407(9) Uani 1 1 d . . . . .
H34 H 0.905766 0.192310 0.098314 0.049 Uiso 1 1 calc R . . . .
C35 C 0.79496(17) 0.21392(15) 0.10288(12) 0.0283(7) Uani 1 1 d . . . . .
C36 C 0.63290(17) 0.22800(14) -0.02195(12) 0.0254(7) Uani 1 1 d . . . . .
H36 H 0.592778 0.225182 0.001367 0.031 Uiso 1 1 calc R . . . .
C37 C 0.62857(18) 0.29592(14) -0.04623(13) 0.0306(7) Uani 1 1 d . . . . .
H37A H 0.636471 0.327683 -0.016886 0.046 Uiso 1 1 calc GR . . . .
H37B H 0.577761 0.302471 -0.069093 0.046 Uiso 1 1 calc GR . . . .
H37C H 0.668694 0.300947 -0.068204 0.046 Uiso 1 1 calc GR . . . .
C38 C 0.61213(19) 0.17802(14) -0.06743(13) 0.0325(8) Uani 1 1 d . . . . .
H38A H 0.644620 0.184622 -0.094699 0.049 Uiso 1 1 calc GR . . . .
H38B H 0.557761 0.182851 -0.084439 0.049 Uiso 1 1 calc GR . . . .
H38C H 0.620763 0.134722 -0.052153 0.049 Uiso 1 1 calc GR . . . .
C39 C 0.81113(17) 0.22144(15) 0.16442(12) 0.0297(7) Uani 1 1 d . . . . .
H39 H 0.760870 0.219885 0.177401 0.036 Uiso 1 1 calc R . . . .
C40 C 0.86314(19) 0.16827(15) 0.19295(13) 0.0364(8) Uani 1 1 d . . . . .
H40A H 0.913307 0.169951 0.181524 0.055 Uiso 1 1 calc GR . . . .
H40B H 0.839062 0.126385 0.183324 0.055 Uiso 1 1 calc GR . . . .
H40C H 0.870405 0.174364 0.232305 0.055 Uiso 1 1 calc GR . . . .
C41 C 0.8483(2) 0.28616(16) 0.17958(15) 0.0460(9) Uani 1 1 d . . . . .
H41A H 0.861493 0.289785 0.219157 0.069 Uiso 1 1 calc GR . . . .
H41B H 0.812151 0.320456 0.165202 0.069 Uiso 1 1 calc GR . . . .
H41C H 0.895230 0.290112 0.164171 0.069 Uiso 1 1 calc GR . . . .
C42 C 0.44796(16) 0.23576(12) 0.28817(12) 0.0196(6) Uani 1 1 d . . . . .
C43 C 0.39711(16) 0.21989(12) 0.32093(12) 0.0220(6) Uani 1 1 d . . . . .
H43 H 0.417740 0.195461 0.352250 0.026 Uiso 1 1 calc R . . . .
C44 C 0.31499(17) 0.23553(13) 0.31420(13) 0.0239(7) Uani 1 1 d . . . . .
C45 C 0.42341(16) 0.26541(13) 0.23274(12) 0.0215(6) Uani 1 1 d . . . . .
H45A H 0.367151 0.270019 0.224840 0.032 Uiso 1 1 calc GR . . . .
H45B H 0.439698 0.237665 0.205366 0.032 Uiso 1 1 calc GR . . . .
H45C H 0.447434 0.307782 0.232017 0.032 Uiso 1 1 calc GR . . . .
C46 C 0.27822(18) 0.21156(15) 0.36061(13) 0.0349(8) Uani 1 1 d . . . . .
H46A H 0.227817 0.232120 0.358777 0.052 Uiso 1 1 calc GR . . . .
H46B H 0.311577 0.222230 0.395218 0.052 Uiso 1 1 calc GR . . . .
H46C H 0.271515 0.164861 0.357783 0.052 Uiso 1 1 calc GR . . . .
C47 C 0.55056(16) 0.18101(12) 0.34722(12) 0.0209(6) Uani 1 1 d . . . . .
C48 C 0.53287(16) 0.11513(13) 0.33853(12) 0.0243(7) Uani 1 1 d . . . . .
C49 C 0.54723(17) 0.07393(14) 0.38305(13) 0.0297(7) Uani 1 1 d . . . . .
H49 H 0.536130 0.029464 0.377788 0.036 Uiso 1 1 calc R . . . .
C50 C 0.57725(18) 0.09598(14) 0.43482(13) 0.0332(8) Uani 1 1 d . . . . .
H50 H 0.584806 0.067372 0.464843 0.040 Uiso 1 1 calc R . . . .
C51 C 0.59593(18) 0.16002(14) 0.44197(13) 0.0316(7) Uani 1 1 d . . . . .
H51 H 0.617212 0.175082 0.477326 0.038 Uiso 1 1 calc R . . . .
C52 C 0.58457(17) 0.20341(13) 0.39894(12) 0.0247(7) Uani 1 1 d . . . . .
C53 C 0.49723(16) 0.08776(13) 0.28370(12) 0.0251(7) Uani 1 1 d . . . . .
H53 H 0.484573 0.124595 0.258004 0.030 Uiso 1 1 calc R . . . .
C54 C 0.55390(19) 0.04411(15) 0.26147(14) 0.0366(8) Uani 1 1 d . . . . .
H54A H 0.598541 0.069367 0.255628 0.055 Uiso 1 1 calc GR . . . .
H54B H 0.528315 0.025336 0.226980 0.055 Uiso 1 1 calc GR . . . .
H54C H 0.571139 0.009685 0.287554 0.055 Uiso 1 1 calc GR . . . .
C55 C 0.42212(18) 0.05195(14) 0.28566(14) 0.0354(8) Uani 1 1 d . . . . .
H55A H 0.433486 0.012924 0.307543 0.053 Uiso 1 1 calc GR . . . .
H55B H 0.397031 0.040254 0.248756 0.053 Uiso 1 1 calc GR . . . .
H55C H 0.387706 0.079702 0.301918 0.053 Uiso 1 1 calc GR . . . .
C56 C 0.60639(19) 0.27311(14) 0.41035(13) 0.0304(7) Uani 1 1 d . . . . .
H56 H 0.602713 0.295431 0.374664 0.036 Uiso 1 1 calc R . . . .
C57 C 0.6898(2) 0.28017(16) 0.44119(14) 0.0476(10) Uani 1 1 d . . . . .
H57A H 0.695474 0.257767 0.476068 0.071 Uiso 1 1 calc GR . . . .
H57B H 0.701919 0.325811 0.447523 0.071 Uiso 1 1 calc GR . . . .
H57C H 0.725280 0.261421 0.419650 0.071 Uiso 1 1 calc GR . . . .
C58 C 0.5499(2) 0.30592(16) 0.44109(14) 0.0476(10) Uani 1 1 d . . . . .
H58A H 0.497246 0.301261 0.420549 0.071 Uiso 1 1 calc GR . . . .
H58B H 0.562759 0.351650 0.445595 0.071 Uiso 1 1 calc GR . . . .
H58C H 0.553494 0.285878 0.476816 0.071 Uiso 1 1 calc GR . . . .
C59 C 0.20261(16) 0.29068(14) 0.27170(12) 0.0262(7) Uani 1 1 d . . . . .
C60 C 0.19549(17) 0.35752(14) 0.28086(12) 0.0267(7) Uani 1 1 d . . . . .
C61 C 0.12191(19) 0.38374(15) 0.27609(13) 0.0340(8) Uani 1 1 d . . . . .
H61 H 0.116427 0.428353 0.282436 0.041 Uiso 1 1 calc R . . . .
C62 C 0.05711(19) 0.34628(16) 0.26238(14) 0.0372(8) Uani 1 1 d . . . . .
H62 H 0.007402 0.365040 0.259401 0.045 Uiso 1 1 calc R . . . .
C63 C 0.06415(18) 0.28148(16) 0.25293(14) 0.0357(8) Uani 1 1 d . . . . .
H63 H 0.018910 0.256109 0.243310 0.043 Uiso 1 1 calc R . . . .
C64 C 0.13624(18) 0.25235(14) 0.25720(14) 0.0291(7) Uani 1 1 d . . . . .
C65 C 0.26844(17) 0.39791(13) 0.29788(13) 0.0285(7) Uani 1 1 d . . . . .
H65 H 0.310631 0.376624 0.282699 0.034 Uiso 1 1 calc R . . . .
C66 C 0.2928(2) 0.39821(16) 0.35949(14) 0.0396(8) Uani 1 1 d . . . . .
H66A H 0.251155 0.416123 0.375868 0.059 Uiso 1 1 calc GR . . . .
H66B H 0.339308 0.424559 0.369732 0.059 Uiso 1 1 calc GR . . . .
H66C H 0.303750 0.354147 0.372449 0.059 Uiso 1 1 calc GR . . . .
C67 C 0.26102(19) 0.46658(14) 0.27595(14) 0.0387(8) Uani 1 1 d . . . . .
H67A H 0.240568 0.465677 0.236876 0.058 Uiso 1 1 calc GR . . . .
H67B H 0.311864 0.487166 0.282549 0.058 Uiso 1 1 calc GR . . . .
H67C H 0.225871 0.490925 0.294355 0.058 Uiso 1 1 calc GR . . . .
C68 C 0.14125(18) 0.18104(15) 0.24405(14) 0.0346(8) Uani 1 1 d . . . . .
H68 H 0.196954 0.168556 0.251228 0.042 Uiso 1 1 calc R . . . .
C69 C 0.0995(2) 0.13911(16) 0.28005(16) 0.0479(10) Uani 1 1 d . . . . .
H69A H 0.120778 0.147748 0.318299 0.072 Uiso 1 1 calc GR . . . .
H69B H 0.106933 0.093657 0.272177 0.072 Uiso 1 1 calc GR . . . .
H69C H 0.044320 0.149211 0.272618 0.072 Uiso 1 1 calc GR . . . .
C70 C 0.1089(2) 0.16829(18) 0.18417(15) 0.0480(10) Uani 1 1 d . . . . .
H70A H 0.053243 0.176701 0.176798 0.072 Uiso 1 1 calc GR . . . .
H70B H 0.118274 0.123373 0.175609 0.072 Uiso 1 1 calc GR . . . .
H70C H 0.134321 0.196604 0.161698 0.072 Uiso 1 1 calc GR . . . .
C71 C 0.76675(16) 0.25169(12) 0.30768(12) 0.0189(6) Uani 1 1 d . . . . .
C72 C 0.79800(16) 0.19111(12) 0.32478(11) 0.0217(6) Uani 1 1 d . . . . .
C73 C 0.87770(16) 0.18640(13) 0.34307(11) 0.0230(6) Uani 1 1 d . . . . .
H73 H 0.899807 0.145637 0.353502 0.028 Uiso 1 1 calc R . . . .
C74 C 0.92479(17) 0.23960(13) 0.34627(12) 0.0238(7) Uani 1 1 d . . . . .
H74 H 0.978930 0.235183 0.357897 0.029 Uiso 1 1 calc R . . . .
C75 C 0.89289(16) 0.29971(13) 0.33246(12) 0.0247(7) Uani 1 1 d . . . . .
H75 H 0.925421 0.336453 0.336685 0.030 Uiso 1 1 calc R . . . .
C76 C 0.81432(16) 0.30734(12) 0.31256(11) 0.0205(6) Uani 1 1 d . . . . .
C77 C 0.74693(16) 0.13239(13) 0.32496(12) 0.0258(7) Uani 1 1 d . . . . .
H77 H 0.692280 0.145891 0.311698 0.031 Uiso 1 1 calc R . . . .
C78 C 0.76678(19) 0.08039(14) 0.28676(13) 0.0357(8) Uani 1 1 d . . . . .
H78A H 0.757764 0.096905 0.249540 0.054 Uiso 1 1 calc GR . . . .
H78B H 0.734172 0.042627 0.288614 0.054 Uiso 1 1 calc GR . . . .
H78C H 0.821139 0.068282 0.297635 0.054 Uiso 1 1 calc GR . . . .
C79 C 0.75292(18) 0.10618(14) 0.38229(13) 0.0333(8) Uani 1 1 d . . . . .
H79A H 0.805728 0.091354 0.395739 0.050 Uiso 1 1 calc GR . . . .
H79B H 0.717044 0.070160 0.381925 0.050 Uiso 1 1 calc GR . . . .
H79C H 0.739848 0.140167 0.406070 0.050 Uiso 1 1 calc GR . . . .
C80 C 0.77918(16) 0.37283(12) 0.29728(12) 0.0250(7) Uani 1 1 d . . . . .
H80 H 0.734865 0.366418 0.266560 0.030 Uiso 1 1 calc R . . . .
C81 C 0.83459(18) 0.42055(13) 0.27826(13) 0.0312(7) Uani 1 1 d . . . . .
H81A H 0.878424 0.428430 0.307757 0.047 Uiso 1 1 calc GR . . . .
H81B H 0.807547 0.461070 0.267913 0.047 Uiso 1 1 calc GR . . . .
H81C H 0.853295 0.402696 0.246937 0.047 Uiso 1 1 calc GR . . . .
C82 C 0.74662(18) 0.40036(13) 0.34498(13) 0.0303(7) Uani 1 1 d . . . . .
H82A H 0.708380 0.370564 0.354726 0.045 Uiso 1 1 calc GR . . . .
H82B H 0.722054 0.441876 0.334584 0.045 Uiso 1 1 calc GR . . . .
H82C H 0.788588 0.406263 0.376152 0.045 Uiso 1 1 calc GR . . . .
C83 C 0.58179(16) 0.42145(13) 0.25034(12) 0.0245(7) Uani 1 1 d . . . . .
H83 H 0.608339 0.415187 0.221079 0.029 Uiso 1 1 calc R . . . .
C84 C 0.56702(17) 0.48338(13) 0.26517(13) 0.0284(7) Uani 1 1 d . . . . .
H84 H 0.583859 0.518842 0.246549 0.034 Uiso 1 1 calc R . . . .
C85 C 0.52785(19) 0.49365(14) 0.30699(13) 0.0332(8) Uani 1 1 d . . . . .
H85 H 0.517560 0.536056 0.317721 0.040 Uiso 1 1 calc R . . . .
C86 C 0.50381(18) 0.44117(14) 0.33303(13) 0.0323(7) Uani 1 1 d . . . . .
H86 H 0.476537 0.446735 0.361997 0.039 Uiso 1 1 calc R . . . .
C87 C 0.52018(17) 0.38024(13) 0.31616(12) 0.0255(7) Uani 1 1 d . . . . .
H87 H 0.502583 0.344302 0.333804 0.031 Uiso 1 1 calc R . . . .
C88 C 0.5966(5) 0.1279(5) 0.6172(3) 0.206(5) Uani 1 1 d . . . . .
H88A H 0.614720 0.086022 0.606903 0.310 Uiso 1 1 calc GR . . . .
H88B H 0.611473 0.133583 0.656556 0.310 Uiso 1 1 calc GR . . . .
H88C H 0.619859 0.162049 0.598673 0.310 Uiso 1 1 calc GR . . . .
C89 C 0.5121(5) 0.1311(4) 0.6016(4) 0.163(3) Uani 1 1 d . . . . .
H89A H 0.489916 0.106812 0.628929 0.196 Uiso 1 1 calc R . . . .
H89B H 0.496667 0.176547 0.604105 0.196 Uiso 1 1 calc R . . . .
C90 C 0.4072(5) 0.1050(5) 0.5295(5) 0.219(6) Uani 1 1 d . . . . .
H90A H 0.385590 0.148018 0.534465 0.263 Uiso 1 1 calc R . . . .
H90B H 0.384252 0.075701 0.553323 0.263 Uiso 1 1 calc R . . . .
C91 C 0.3731(5) 0.0867(5) 0.4763(3) 0.187(5) Uani 1 1 d . . . . .
H91A H 0.396136 0.111677 0.450185 0.281 Uiso 1 1 calc GR . . . .
H91B H 0.317511 0.095007 0.470391 0.281 Uiso 1 1 calc GR . . . .
H91C H 0.382123 0.040844 0.471228 0.281 Uiso 1 1 calc GR . . . .
N1 N 0.49143(12) 0.18248(9) 0.07793(9) 0.0164(5) Uani 1 1 d . . . . .
N2 N 0.50053(13) 0.32252(10) 0.07689(9) 0.0179(5) Uani 1 1 d . . . . .
N3 N 0.65723(13) 0.23994(10) 0.09526(10) 0.0178(5) Uani 1 1 d . . . . .
N4 N 0.52719(13) 0.22455(10) 0.30164(9) 0.0192(5) Uani 1 1 d . . . . .
N5 N 0.27873(13) 0.26734(11) 0.27403(10) 0.0238(5) Uani 1 1 d . . . . .
N6 N 0.68800(13) 0.25755(9) 0.28607(10) 0.0176(5) Uani 1 1 d . . . . .
N7 N 0.55984(13) 0.36925(10) 0.27593(9) 0.0202(5) Uani 1 1 d . . . . .
O1 O 0.59003(10) 0.31627(8) 0.18172(7) 0.0185(4) Uani 1 1 d . . . . .
O2 O 0.57857(10) 0.19700(8) 0.19112(7) 0.0179(4) Uani 1 1 d . . . . .
O3 O 0.4784(3) 0.1090(3) 0.5517(2) 0.148(2) Uani 1 1 d . . . . .
Nb1 Nb 0.57413(2) 0.24993(2) 0.12654(2) 0.01526(8) Uani 1 1 d . . . . .
Nb2 Nb 0.59281(2) 0.26363(2) 0.24778(2) 0.01624(8) 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'
Nb Nb -2.0727 0.6215 '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'
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
C2 C1 C4 115.5(2) . . ?
N1 C1 C2 124.1(2) . . ?
N1 C1 C4 120.4(2) . . ?
C1 C2 H2 115.7 . . ?
C3 C2 C1 128.6(3) . . ?
C3 C2 H2 115.7 . . ?
C2 C3 C5 115.5(2) . . ?
N2 C3 C2 124.0(2) . . ?
N2 C3 C5 120.4(2) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 119.3(2) . . ?
C11 C6 C7 121.6(2) . . ?
C11 C6 N1 118.9(2) . . ?
C6 C7 C12 123.0(2) . . ?
C8 C7 C6 117.1(3) . . ?
C8 C7 C12 120.0(2) . . ?
C7 C8 H8 119.0 . . ?
C9 C8 C7 122.0(3) . . ?
C9 C8 H8 119.0 . . ?
C8 C9 H9 120.2 . . ?
C8 C9 C10 119.7(3) . . ?
C10 C9 H9 120.2 . . ?
C9 C10 H10 119.4 . . ?
C9 C10 C11 121.3(3) . . ?
C11 C10 H10 119.4 . . ?
C6 C11 C15 122.0(2) . . ?
C10 C11 C6 118.3(3) . . ?
C10 C11 C15 119.6(3) . . ?
C7 C12 H12 108.1 . . ?
C7 C12 C13 113.2(2) . . ?
C7 C12 C14 109.5(2) . . ?
C13 C12 H12 108.1 . . ?
C14 C12 H12 108.1 . . ?
C14 C12 C13 109.8(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15 107.5 . . ?
C11 C15 C16 112.1(2) . . ?
C11 C15 C17 112.7(2) . . ?
C16 C15 H15 107.5 . . ?
C16 C15 C17 109.4(2) . . ?
C17 C15 H15 107.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 N2 118.6(2) . . ?
C23 C18 C19 121.7(2) . . ?
C23 C18 N2 119.6(2) . . ?
C18 C19 C24 122.5(2) . . ?
C20 C19 C18 117.5(3) . . ?
C20 C19 C24 120.0(3) . . ?
C19 C20 H20 119.1 . . ?
C21 C20 C19 121.9(3) . . ?
C21 C20 H20 119.1 . . ?
C20 C21 H21 120.2 . . ?
C22 C21 C20 119.5(3) . . ?
C22 C21 H21 120.2 . . ?
C21 C22 H22 119.2 . . ?
C21 C22 C23 121.6(3) . . ?
C23 C22 H22 119.2 . . ?
C18 C23 C27 123.8(2) . . ?
C22 C23 C18 117.7(3) . . ?
C22 C23 C27 118.5(2) . . ?
C19 C24 H24 107.4 . . ?
C19 C24 C25 113.5(2) . . ?
C19 C24 C26 112.6(2) . . ?
C25 C24 H24 107.4 . . ?
C26 C24 H24 107.4 . . ?
C26 C24 C25 108.3(2) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 H27 107.5 . . ?
C23 C27 C28 112.6(2) . . ?
C23 C27 C29 111.3(2) . . ?
C28 C27 H27 107.5 . . ?
C29 C27 H27 107.5 . . ?
C29 C27 C28 110.1(2) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C35 C30 C31 118.6(3) . . ?
N3 C30 C31 119.6(3) . . ?
N3 C30 C35 121.7(3) . . ?
C30 C31 C36 121.4(3) . . ?
C32 C31 C30 119.5(3) . . ?
C32 C31 C36 119.1(3) . . ?
C31 C32 H32 119.3 . . ?
C33 C32 C31 121.3(3) . . ?
C33 C32 H32 119.3 . . ?
C32 C33 H33 120.3 . . ?
C34 C33 C32 119.3(3) . . ?
C34 C33 H33 120.3 . . ?
C33 C34 H34 119.1 . . ?
C33 C34 C35 121.9(3) . . ?
C35 C34 H34 119.1 . . ?
C30 C35 C39 122.0(3) . . ?
C34 C35 C30 119.3(3) . . ?
C34 C35 C39 118.6(3) . . ?
C31 C36 H36 107.3 . . ?
C31 C36 C37 110.9(2) . . ?
C31 C36 C38 113.8(2) . . ?
C37 C36 H36 107.3 . . ?
C37 C36 C38 109.9(2) . . ?
C38 C36 H36 107.3 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35 C39 H39 108.4 . . ?
C35 C39 C40 112.5(3) . . ?
C40 C39 H39 108.4 . . ?
C41 C39 C35 109.7(3) . . ?
C41 C39 H39 108.4 . . ?
C41 C39 C40 109.4(3) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C45 123.0(3) . . ?
C43 C42 N4 123.7(3) . . ?
N4 C42 C45 113.3(2) . . ?
C42 C43 H43 115.7 . . ?
C42 C43 C44 128.6(3) . . ?
C44 C43 H43 115.7 . . ?
C43 C44 C46 113.1(3) . . ?
N5 C44 C43 123.2(3) . . ?
N5 C44 C46 123.6(3) . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 N4 117.4(2) . . ?
C52 C47 C48 120.6(3) . . ?
C52 C47 N4 121.9(2) . . ?
C47 C48 C53 123.2(3) . . ?
C49 C48 C47 118.1(3) . . ?
C49 C48 C53 118.7(2) . . ?
C48 C49 H49 119.1 . . ?
C50 C49 C48 121.9(3) . . ?
C50 C49 H49 119.1 . . ?
C49 C50 H50 120.6 . . ?
C51 C50 C49 118.9(3) . . ?
C51 C50 H50 120.6 . . ?
C50 C51 H51 119.0 . . ?
C50 C51 C52 122.0(3) . . ?
C52 C51 H51 119.0 . . ?
C47 C52 C56 122.9(3) . . ?
C51 C52 C47 118.4(3) . . ?
C51 C52 C56 118.6(3) . . ?
C48 C53 H53 107.6 . . ?
C48 C53 C54 111.4(2) . . ?
C48 C53 C55 111.8(3) . . ?
C54 C53 H53 107.6 . . ?
C55 C53 H53 107.6 . . ?
C55 C53 C54 110.5(2) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C52 C56 H56 107.7 . . ?
C52 C56 C57 111.9(3) . . ?
C52 C56 C58 110.9(3) . . ?
C57 C56 H56 107.7 . . ?
C58 C56 H56 107.7 . . ?
C58 C56 C57 110.8(3) . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C64 C59 C60 120.2(3) . . ?
C64 C59 N5 123.5(3) . . ?
N5 C59 C60 116.1(3) . . ?
C59 C60 C65 119.2(2) . . ?
C61 C60 C59 118.6(3) . . ?
C61 C60 C65 122.1(3) . . ?
C60 C61 H61 119.4 . . ?
C62 C61 C60 121.2(3) . . ?
C62 C61 H61 119.4 . . ?
C61 C62 H62 120.0 . . ?
C61 C62 C63 120.1(3) . . ?
C63 C62 H62 120.0 . . ?
C62 C63 H63 119.3 . . ?
C62 C63 C64 121.4(3) . . ?
C64 C63 H63 119.3 . . ?
C59 C64 C68 121.9(3) . . ?
C63 C64 C59 118.5(3) . . ?
C63 C64 C68 119.6(3) . . ?
C60 C65 H65 107.3 . . ?
C66 C65 C60 110.5(2) . . ?
C66 C65 H65 107.3 . . ?
C66 C65 C67 110.5(3) . . ?
C67 C65 C60 113.7(3) . . ?
C67 C65 H65 107.3 . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C65 C67 H67A 109.5 . . ?
C65 C67 H67B 109.5 . . ?
C65 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C64 C68 H68 107.9 . . ?
C64 C68 C69 111.8(3) . . ?
C64 C68 C70 110.8(3) . . ?
C69 C68 H68 107.9 . . ?
C70 C68 H68 107.9 . . ?
C70 C68 C69 110.3(3) . . ?
C68 C69 H69A 109.5 . . ?
C68 C69 H69B 109.5 . . ?
C68 C69 H69C 109.5 . . ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C68 C70 H70A 109.5 . . ?
C68 C70 H70B 109.5 . . ?
C68 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C72 C71 C76 120.7(3) . . ?
N6 C71 C72 120.0(2) . . ?
N6 C71 C76 119.3(2) . . ?
C71 C72 C77 121.4(2) . . ?
C73 C72 C71 118.3(2) . . ?
C73 C72 C77 120.2(2) . . ?
C72 C73 H73 119.3 . . ?
C74 C73 C72 121.4(3) . . ?
C74 C73 H73 119.3 . . ?
C73 C74 H74 120.1 . . ?
C73 C74 C75 119.8(3) . . ?
C75 C74 H74 120.1 . . ?
C74 C75 H75 119.3 . . ?
C74 C75 C76 121.5(3) . . ?
C76 C75 H75 119.3 . . ?
C71 C76 C80 120.2(2) . . ?
C75 C76 C71 118.0(2) . . ?
C75 C76 C80 121.7(2) . . ?
C72 C77 H77 108.0 . . ?
C72 C77 C78 111.3(2) . . ?
C72 C77 C79 110.7(2) . . ?
C78 C77 H77 108.0 . . ?
C79 C77 H77 108.0 . . ?
C79 C77 C78 110.8(2) . . ?
C77 C78 H78A 109.5 . . ?
C77 C78 H78B 109.5 . . ?
C77 C78 H78C 109.5 . . ?
H78A C78 H78B 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C77 C79 H79A 109.5 . . ?
C77 C79 H79B 109.5 . . ?
C77 C79 H79C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C76 C80 H80 107.4 . . ?
C76 C80 C81 114.0(2) . . ?
C76 C80 C82 109.5(2) . . ?
C81 C80 H80 107.4 . . ?
C81 C80 C82 110.8(2) . . ?
C82 C80 H80 107.4 . . ?
C80 C81 H81A 109.5 . . ?
C80 C81 H81B 109.5 . . ?
C80 C81 H81C 109.5 . . ?
H81A C81 H81B 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C80 C82 H82A 109.5 . . ?
C80 C82 H82B 109.5 . . ?
C80 C82 H82C 109.5 . . ?
H82A C82 H82B 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C84 C83 H83 118.8 . . ?
N7 C83 H83 118.8 . . ?
N7 C83 C84 122.5(3) . . ?
C83 C84 H84 120.1 . . ?
C85 C84 C83 119.8(3) . . ?
C85 C84 H84 120.1 . . ?
C84 C85 H85 120.7 . . ?
C84 C85 C86 118.7(3) . . ?
C86 C85 H85 120.7 . . ?
C85 C86 H86 120.6 . . ?
C85 C86 C87 118.7(3) . . ?
C87 C86 H86 120.6 . . ?
C86 C87 H87 118.3 . . ?
N7 C87 C86 123.4(3) . . ?
N7 C87 H87 118.3 . . ?
H88A C88 H88B 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C89 C88 H88A 109.5 . . ?
C89 C88 H88B 109.5 . . ?
C89 C88 H88C 109.5 . . ?
C88 C89 H89A 107.7 . . ?
C88 C89 H89B 107.7 . . ?
H89A C89 H89B 107.1 . . ?
O3 C89 C88 118.6(7) . . ?
O3 C89 H89A 107.7 . . ?
O3 C89 H89B 107.7 . . ?
H90A C90 H90B 105.8 . . ?
C91 C90 H90A 104.8 . . ?
C91 C90 H90B 104.8 . . ?
O3 C90 H90A 104.8 . . ?
O3 C90 H90B 104.8 . . ?
O3 C90 C91 129.8(10) . . ?
C90 C91 H91A 109.5 . . ?
C90 C91 H91B 109.5 . . ?
C90 C91 H91C 109.5 . . ?
H91A C91 H91B 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
C1 N1 C6 114.6(2) . . ?
C1 N1 Nb1 122.92(16) . . ?
C6 N1 Nb1 121.34(16) . . ?
C3 N2 C18 114.8(2) . . ?
C3 N2 Nb1 122.80(16) . . ?
C18 N2 Nb1 121.29(16) . . ?
C30 N3 Nb1 173.33(18) . . ?
C42 N4 C47 114.8(2) . . ?
C42 N4 Nb2 115.23(18) . . ?
C47 N4 Nb2 129.52(17) . . ?
C44 N5 C59 122.9(3) . . ?
C71 N6 Nb2 170.3(2) . . ?
C83 N7 Nb2 119.11(18) . . ?
C87 N7 C83 116.9(2) . . ?
C87 N7 Nb2 124.04(17) . . ?
Nb1 O1 Nb2 100.46(8) . . ?
Nb1 O2 Nb2 100.51(7) . . ?
C90 O3 C89 130.4(8) . . ?
N1 Nb1 Nb2 123.55(6) . . ?
N2 Nb1 N1 82.26(8) . . ?
N2 Nb1 Nb2 116.48(6) . . ?
N3 Nb1 N1 101.14(9) . . ?
N3 Nb1 N2 105.86(9) . . ?
N3 Nb1 O1 111.84(9) . . ?
N3 Nb1 O2 112.77(9) . . ?
N3 Nb1 Nb2 120.40(8) . . ?
O1 Nb1 N1 146.75(8) . . ?
O1 Nb1 N2 84.73(8) . . ?
O1 Nb1 O2 80.24(7) . . ?
O1 Nb1 Nb2 40.27(5) . . ?
O2 Nb1 N1 91.18(7) . . ?
O2 Nb1 N2 141.36(8) . . ?
O2 Nb1 Nb2 39.98(5) . . ?
N4 Nb2 N7 88.45(8) . . ?
N4 Nb2 Nb1 130.03(6) . . ?
N6 Nb2 N4 101.70(10) . . ?
N6 Nb2 N7 99.28(8) . . ?
N6 Nb2 O1 111.48(9) . . ?
N6 Nb2 O2 108.77(8) . . ?
N6 Nb2 Nb1 117.05(8) . . ?
N7 Nb2 Nb1 113.24(5) . . ?
O1 Nb2 N4 145.30(8) . . ?
O1 Nb2 N7 76.75(7) . . ?
O1 Nb2 Nb1 39.27(5) . . ?
O2 Nb2 N4 100.38(8) . . ?
O2 Nb2 N7 147.97(7) . . ?
O2 Nb2 O1 78.77(7) . . ?
O2 Nb2 Nb1 39.51(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
C1 C2 1.401(3) . ?
C1 C4 1.519(3) . ?
C1 N1 1.339(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.396(4) . ?
C3 C5 1.517(4) . ?
C3 N2 1.337(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.417(4) . ?
C6 C11 1.396(4) . ?
C6 N1 1.464(3) . ?
C7 C8 1.398(4) . ?
C7 C12 1.517(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.371(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.383(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.393(4) . ?
C11 C15 1.530(4) . ?
C12 H12 1.0000 . ?
C12 C13 1.541(4) . ?
C12 C14 1.537(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C16 1.535(4) . ?
C15 C17 1.537(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.406(4) . ?
C18 C23 1.406(4) . ?
C18 N2 1.463(3) . ?
C19 C20 1.394(4) . ?
C19 C24 1.518(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.383(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.374(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.401(4) . ?
C23 C27 1.518(4) . ?
C24 H24 1.0000 . ?
C24 C25 1.541(4) . ?
C24 C26 1.535(4) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27 1.0000 . ?
C27 C28 1.538(4) . ?
C27 C29 1.538(4) . ?
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 C31 1.420(4) . ?
C30 C35 1.417(4) . ?
C30 N3 1.401(4) . ?
C31 C32 1.393(4) . ?
C31 C36 1.512(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.381(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.375(5) . ?
C34 H34 0.9500 . ?
C34 C35 1.390(4) . ?
C35 C39 1.525(4) . ?
C36 H36 1.0000 . ?
C36 C37 1.535(4) . ?
C36 C38 1.537(4) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39 1.0000 . ?
C39 C40 1.528(4) . ?
C39 C41 1.515(5) . ?
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 C43 1.365(4) . ?
C42 C45 1.510(4) . ?
C42 N4 1.395(3) . ?
C43 H43 0.9500 . ?
C43 C44 1.464(4) . ?
C44 C46 1.518(4) . ?
C44 N5 1.274(4) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.414(4) . ?
C47 C52 1.404(4) . ?
C47 N4 1.457(3) . ?
C48 C49 1.394(4) . ?
C48 C53 1.514(4) . ?
C49 H49 0.9500 . ?
C49 C50 1.387(4) . ?
C50 H50 0.9500 . ?
C50 C51 1.377(4) . ?
C51 H51 0.9500 . ?
C51 C52 1.393(4) . ?
C52 C56 1.514(4) . ?
C53 H53 1.0000 . ?
C53 C54 1.530(4) . ?
C53 C55 1.529(4) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56 1.0000 . ?
C56 C57 1.538(5) . ?
C56 C58 1.529(4) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C60 1.419(4) . ?
C59 C64 1.408(4) . ?
C59 N5 1.419(4) . ?
C60 C61 1.392(4) . ?
C60 C65 1.530(4) . ?
C61 H61 0.9500 . ?
C61 C62 1.374(4) . ?
C62 H62 0.9500 . ?
C62 C63 1.379(4) . ?
C63 H63 0.9500 . ?
C63 C64 1.395(4) . ?
C64 C68 1.526(4) . ?
C65 H65 1.0000 . ?
C65 C66 1.526(4) . ?
C65 C67 1.528(4) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68 1.0000 . ?
C68 C69 1.538(4) . ?
C68 C70 1.528(5) . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 C72 1.411(4) . ?
C71 C76 1.422(4) . ?
C71 N6 1.400(4) . ?
C72 C73 1.399(4) . ?
C72 C77 1.519(4) . ?
C73 H73 0.9500 . ?
C73 C74 1.377(4) . ?
C74 H74 0.9500 . ?
C74 C75 1.389(4) . ?
C75 H75 0.9500 . ?
C75 C76 1.393(4) . ?
C76 C80 1.517(4) . ?
C77 H77 1.0000 . ?
C77 C78 1.529(4) . ?
C77 C79 1.523(4) . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 H80 1.0000 . ?
C80 C81 1.530(4) . ?
C80 C82 1.531(4) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 H83 0.9500 . ?
C83 C84 1.380(4) . ?
C83 N7 1.354(3) . ?
C84 H84 0.9500 . ?
C84 C85 1.376(4) . ?
C85 H85 0.9500 . ?
C85 C86 1.379(4) . ?
C86 H86 0.9500 . ?
C86 C87 1.384(4) . ?
C87 H87 0.9500 . ?
C87 N7 1.350(4) . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C88 C89 1.470(10) . ?
C89 H89A 0.9900 . ?
C89 H89B 0.9900 . ?
C89 O3 1.363(8) . ?
C90 H90A 0.9900 . ?
C90 H90B 0.9900 . ?
C90 C91 1.412(12) . ?
C90 O3 1.279(9) . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
N1 Nb1 2.220(2) . ?
N2 Nb1 2.218(2) . ?
N3 Nb1 1.798(2) . ?
N4 Nb2 2.099(2) . ?
N6 Nb2 1.778(2) . ?
N7 Nb2 2.413(2) . ?
O1 Nb1 1.9385(17) . ?
O1 Nb2 1.9798(18) . ?
O2 Nb1 1.9487(17) . ?
O2 Nb2 1.9682(17) . ?
Nb1 Nb2 3.0118(4) . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 372.9 35.1 ?
2 0.122 0.569 0.848 8.5 0.0 ?
3 0.254 0.034 0.394 58.5 0.9 ?
4 0.246 0.534 0.106 58.5 0.9 ?
5 0.500 0.500 0.500 372.9 35.1 ?
6 0.378 0.069 0.652 8.5 0.0 ?
7 0.622 0.931 0.348 8.5 0.0 ?
8 0.746 -0.034 0.606 58.5 0.9 ?
9 0.754 0.466 0.894 58.5 0.9 ?
10 0.878 0.431 0.152 8.5 0.0 ?
