#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:55:19 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179769 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/65/7006598.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_7006598
loop_
_publ_author_name
'Pugh, David'
'Wright, Joseph A.'
'Freeman, Sandra'
'Danopoulos, Andreas A.'
_publ_section_title
;
 'Pincer' dicarbene complexes of some early transition metals and
 uranium.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              775
_journal_page_last               782
_journal_paper_doi               10.1039/b512133g
_journal_year                    2006
_chemical_formula_moiety         'C35 H41 Cl3 N5 Nb, C4 H8 O'
_chemical_formula_sum            'C39 H49 Cl3 N5 Nb O'
_chemical_formula_weight         803.09
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 92.61(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.803(7)
_cell_length_b                   18.707(11)
_cell_length_c                   18.838(17)
_cell_measurement_reflns_used    8081
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     3803(5)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
PLATON (Spek, 2003)
ENCIFER (Allen, 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1992)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1325
_diffrn_reflns_av_sigmaI/netI    0.1954
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26634
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         3.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  0.9944
_exptl_absorpt_correction_T_min  0.6249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8730
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1973
_refine_ls_R_factor_gt           0.0902
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0444P)²+5.6157P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                4281
_reflns_number_total             8730
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b512133g.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7006598
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4103(5) 0.1845(3) -0.0613(4) 0.0326(15) Uani 1 1 d . . .
C2 C 0.2707(5) 0.2503(3) 0.0075(3) 0.0272(14) Uani 1 1 d . . .
C3 C 0.1594(6) 0.3075(3) -0.0796(4) 0.0376(16) Uani 1 1 d . . .
H3 H 0.0986 0.3373 -0.1025 0.045 Uiso 1 1 calc R . .
C4 C 0.2439(6) 0.2688(3) -0.1114(4) 0.0350(16) Uani 1 1 d . . .
H4 H 0.2550 0.2657 -0.1611 0.042 Uiso 1 1 calc R . .
C5 C 0.1022(5) 0.3315(3) 0.0459(3) 0.0328(15) Uani 1 1 d . . .
C6 C -0.0102(5) 0.2993(3) 0.0619(3) 0.0376(16) Uani 1 1 d . . .
C7 C -0.0833(7) 0.3366(4) 0.1090(4) 0.053(2) Uani 1 1 d . . .
H7 H -0.1607 0.3172 0.1214 0.064 Uiso 1 1 calc R . .
C8 C -0.0447(7) 0.4006(4) 0.1375(4) 0.062(2) Uani 1 1 d . . .
H8 H -0.0954 0.4251 0.1694 0.074 Uiso 1 1 calc R . .
C9 C 0.0666(7) 0.4298(3) 0.1203(4) 0.053(2) Uani 1 1 d . . .
H9 H 0.0922 0.4737 0.1416 0.064 Uiso 1 1 calc R . .
C10 C 0.1428(6) 0.3970(3) 0.0725(4) 0.0427(17) Uani 1 1 d . . .
C11 C 0.2624(6) 0.4325(3) 0.0529(4) 0.0466(19) Uani 1 1 d . . .
H11 H 0.3097 0.3980 0.0241 0.056 Uiso 1 1 calc R . .
C12 C 0.3419(7) 0.4515(4) 0.1189(5) 0.062(2) Uani 1 1 d . . .
H12A H 0.3010 0.4891 0.1454 0.094 Uiso 1 1 calc R . .
H12B H 0.4230 0.4686 0.1048 0.094 Uiso 1 1 calc R . .
H12C H 0.3530 0.4090 0.1490 0.094 Uiso 1 1 calc R . .
C13 C 0.2348(7) 0.4990(3) 0.0073(4) 0.057(2) Uani 1 1 d . . .
H13A H 0.1885 0.4850 -0.0364 0.086 Uiso 1 1 calc R . .
H13B H 0.3129 0.5217 -0.0046 0.086 Uiso 1 1 calc R . .
H13C H 0.1853 0.5328 0.0339 0.086 Uiso 1 1 calc R . .
C14 C -0.0558(6) 0.2300(3) 0.0302(4) 0.0401(17) Uani 1 1 d . . .
H14 H 0.0137 0.2072 0.0051 0.048 Uiso 1 1 calc R . .
C15 C -0.0990(7) 0.1780(4) 0.0860(5) 0.065(2) Uani 1 1 d . . .
H15A H -0.0333 0.1719 0.1231 0.098 Uiso 1 1 calc R . .
H15B H -0.1180 0.1318 0.0637 0.098 Uiso 1 1 calc R . .
H15C H -0.1735 0.1970 0.1071 0.098 Uiso 1 1 calc R . .
C16 C -0.1604(7) 0.2454(4) -0.0241(4) 0.059(2) Uani 1 1 d . . .
H16A H -0.2284 0.2690 -0.0006 0.089 Uiso 1 1 calc R . .
H16B H -0.1902 0.2004 -0.0454 0.089 Uiso 1 1 calc R . .
H16C H -0.1303 0.2767 -0.0612 0.089 Uiso 1 1 calc R . .
C17 C 0.4630(6) 0.1661(3) -0.1245(4) 0.0386(17) Uani 1 1 d . . .
H17 H 0.4363 0.1867 -0.1687 0.046 Uiso 1 1 calc R . .
C18 C 0.5575(6) 0.1156(3) -0.1192(4) 0.0453(19) Uani 1 1 d . . .
H18 H 0.5981 0.1016 -0.1607 0.054 Uiso 1 1 calc R . .
C19 C 0.5931(6) 0.0858(3) -0.0551(4) 0.0408(18) Uani 1 1 d . . .
H19 H 0.6562 0.0504 -0.0517 0.049 Uiso 1 1 calc R . .
C20 C 0.5342(5) 0.1087(3) 0.0043(4) 0.0338(16) Uani 1 1 d . . .
C21 C 0.4999(5) 0.1156(3) 0.1275(4) 0.0307(15) Uani 1 1 d . . .
C22 C 0.6347(5) 0.0307(3) 0.1674(4) 0.0363(16) Uani 1 1 d . . .
H22 H 0.6802 0.0001 0.1993 0.044 Uiso 1 1 calc R . .
C23 C 0.6425(5) 0.0320(3) 0.0979(4) 0.0356(17) Uani 1 1 d . . .
H23 H 0.6944 0.0030 0.0704 0.043 Uiso 1 1 calc R . .
C24 C 0.5302(5) 0.1013(3) 0.2595(3) 0.0316(15) Uani 1 1 d . . .
C25 C 0.4281(5) 0.0743(3) 0.2946(4) 0.0339(16) Uani 1 1 d . . .
C26 C 0.4205(6) 0.0908(3) 0.3654(4) 0.0396(17) Uani 1 1 d . . .
H26 H 0.3533 0.0726 0.3907 0.048 Uiso 1 1 calc R . .
C27 C 0.5070(6) 0.1329(3) 0.4006(4) 0.0386(17) Uani 1 1 d . . .
H27 H 0.4993 0.1437 0.4495 0.046 Uiso 1 1 calc R . .
C28 C 0.6064(6) 0.1596(3) 0.3643(4) 0.0383(17) Uani 1 1 d . . .
H28 H 0.6664 0.1886 0.3889 0.046 Uiso 1 1 calc R . .
C29 C 0.6197(5) 0.1448(3) 0.2930(4) 0.0332(16) Uani 1 1 d . . .
C30 C 0.7298(6) 0.1740(3) 0.2549(4) 0.0411(17) Uani 1 1 d . . .
H30 H 0.7167 0.1639 0.2030 0.049 Uiso 1 1 calc R . .
C31 C 0.7407(6) 0.2551(3) 0.2651(4) 0.0495(19) Uani 1 1 d . . .
H31A H 0.6677 0.2786 0.2429 0.074 Uiso 1 1 calc R . .
H31B H 0.8155 0.2724 0.2430 0.074 Uiso 1 1 calc R . .
H31C H 0.7460 0.2663 0.3160 0.074 Uiso 1 1 calc R . .
C32 C 0.8498(6) 0.1364(4) 0.2819(4) 0.052(2) Uani 1 1 d . . .
H32A H 0.8588 0.1408 0.3337 0.078 Uiso 1 1 calc R . .
H32B H 0.9211 0.1587 0.2604 0.078 Uiso 1 1 calc R . .
H32C H 0.8460 0.0857 0.2689 0.078 Uiso 1 1 calc R . .
C33 C 0.3312(5) 0.0259(3) 0.2590(4) 0.0326(16) Uani 1 1 d . . .
H33 H 0.3455 0.0246 0.2069 0.039 Uiso 1 1 calc R . .
C34 C 0.3459(6) -0.0498(3) 0.2884(4) 0.0391(17) Uani 1 1 d . . .
H34A H 0.4294 -0.0674 0.2799 0.059 Uiso 1 1 calc R . .
H34B H 0.2845 -0.0812 0.2645 0.059 Uiso 1 1 calc R . .
H34C H 0.3332 -0.0494 0.3395 0.059 Uiso 1 1 calc R . .
C35 C 0.1991(5) 0.0536(3) 0.2691(4) 0.0424(18) Uani 1 1 d . . .
H35A H 0.1831 0.0546 0.3199 0.064 Uiso 1 1 calc R . .
H35B H 0.1392 0.0219 0.2444 0.064 Uiso 1 1 calc R . .
H35C H 0.1908 0.1020 0.2495 0.064 Uiso 1 1 calc R . .
C36A C 0.104(2) 0.404(2) 0.3054(14) 0.047(4) Uani 0.363(6) 1 d PD A 1
H36A H 0.1540 0.3724 0.2756 0.056 Uiso 0.363(6) 1 calc PR A 1
H36B H 0.0791 0.4480 0.2794 0.056 Uiso 0.363(6) 1 calc PR A 1
C37A C -0.0018(9) 0.3661(4) 0.3390(6) 0.098(4) Uani 0.363(6) 1 d PD A 1
H37A H -0.0643 0.3496 0.3026 0.117 Uiso 0.363(6) 1 calc PR A 1
H37B H 0.0280 0.3247 0.3677 0.117 Uiso 0.363(6) 1 calc PR A 1
C38A C -0.0535(7) 0.4229(4) 0.3849(5) 0.070(3) Uani 0.363(6) 1 d PD A 1
H38A H -0.0983 0.4601 0.3565 0.084 Uiso 0.363(6) 1 calc PR A 1
H38B H -0.1086 0.4028 0.4204 0.084 Uiso 0.363(6) 1 calc PR A 1
C39A C 0.0645(14) 0.4501(11) 0.4182(13) 0.062(4) Uani 0.363(6) 1 d PD A 1
H39A H 0.0684 0.5029 0.4151 0.074 Uiso 0.363(6) 1 calc PR A 1
H39B H 0.0732 0.4358 0.4687 0.074 Uiso 0.363(6) 1 calc PR A 1
C36B C 0.1246(12) 0.3894(8) 0.3207(9) 0.047(4) Uani 0.637(6) 1 d PD A 2
H36C H 0.1865 0.3790 0.3597 0.056 Uiso 0.637(6) 1 calc PR A 2
H36D H 0.1506 0.3663 0.2765 0.056 Uiso 0.637(6) 1 calc PR A 2
C37B C -0.0018(9) 0.3661(4) 0.3390(6) 0.098(4) Uani 0.637(6) 1 d PD A 2
H37C H 0.0024 0.3200 0.3648 0.117 Uiso 0.637(6) 1 calc PR A 2
H37D H -0.0551 0.3599 0.2953 0.117 Uiso 0.637(6) 1 calc PR A 2
C38B C -0.0535(7) 0.4229(4) 0.3849(5) 0.070(3) Uani 0.637(6) 1 d PD A 2
H38C H -0.0504 0.4084 0.4355 0.084 Uiso 0.637(6) 1 calc PR A 2
H38D H -0.1400 0.4348 0.3696 0.084 Uiso 0.637(6) 1 calc PR A 2
C39B C 0.0358(10) 0.4862(6) 0.3718(7) 0.062(4) Uani 0.637(6) 1 d PD A 2
H39C H -0.0116 0.5305 0.3612 0.074 Uiso 0.637(6) 1 calc PR A 2
H39D H 0.0916 0.4945 0.4141 0.074 Uiso 0.637(6) 1 calc PR A 2
Cl1 Cl 0.21143(14) 0.09663(9) 0.08219(11) 0.0529(5) Uani 1 1 d . . .
Cl2 Cl 0.52601(15) 0.29054(8) 0.10871(11) 0.0487(5) Uani 1 1 d . . .
Cl3 Cl 0.2635(2) 0.24579(11) 0.20005(12) 0.0814(8) Uani 1 1 d . . .
N1 N 0.4454(4) 0.1592(2) 0.0023(3) 0.0302(12) Uani 1 1 d . . .
N2 N 0.3126(4) 0.2340(2) -0.0580(3) 0.0312(12) Uani 1 1 d . . .
N3 N 0.1759(4) 0.2965(2) -0.0070(3) 0.0305(12) Uani 1 1 d . . .
N4 N 0.5596(4) 0.0844(2) 0.0725(3) 0.0325(13) Uani 1 1 d . . .
N5 N 0.5478(4) 0.0821(2) 0.1865(3) 0.0307(13) Uani 1 1 d . . .
Nb1 Nb 0.36084(5) 0.19892(3) 0.10177(3) 0.03293(19) Uani 1 1 d . . .
O1A O 0.1608(12) 0.4171(7) 0.3771(10) 0.066(2) Uani 0.363(6) 1 d PD A 1
O1B O 0.1064(7) 0.4653(4) 0.3113(5) 0.066(2) Uani 0.637(6) 1 d PD A 2
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'
Cl Cl 0.1484 0.1585 '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
N1 C1 C17 125.1(6) . . ?
N1 C1 N2 112.2(5) . . ?
C17 C1 N2 122.7(6) . . ?
N3 C2 N2 103.8(5) . . ?
N3 C2 Nb1 137.8(4) . . ?
N2 C2 Nb1 118.4(4) . . ?
C4 C3 N3 107.8(6) . . ?
C4 C3 H3 126.1 . . ?
N3 C3 H3 126.1 . . ?
C3 C4 N2 106.5(6) . . ?
C3 C4 H4 126.7 . . ?
N2 C4 H4 126.7 . . ?
C10 C5 C6 124.4(6) . . ?
C10 C5 N3 118.0(5) . . ?
C6 C5 N3 117.4(5) . . ?
C5 C6 C7 116.2(6) . . ?
C5 C6 C14 123.9(5) . . ?
C7 C6 C14 119.9(6) . . ?
C8 C7 C6 120.8(7) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C7 C8 C9 120.7(6) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C8 C9 C10 121.9(7) . . ?
C8 C9 H9 119.1 . . ?
C10 C9 H9 119.1 . . ?
C5 C10 C9 116.0(6) . . ?
C5 C10 C11 124.0(6) . . ?
C9 C10 C11 120.0(6) . . ?
C10 C11 C12 111.1(6) . . ?
C10 C11 C13 110.3(6) . . ?
C12 C11 C13 110.9(6) . . ?
C10 C11 H11 108.1 . . ?
C12 C11 H11 108.1 . . ?
C13 C11 H11 108.1 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C6 C14 C16 109.0(5) . . ?
C6 C14 C15 112.4(6) . . ?
C16 C14 C15 110.2(6) . . ?
C6 C14 H14 108.4 . . ?
C16 C14 H14 108.4 . . ?
C15 C14 H14 108.4 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C1 C17 C18 115.9(7) . . ?
C1 C17 H17 122.1 . . ?
C18 C17 H17 122.1 . . ?
C19 C18 C17 121.0(6) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C18 C19 C20 117.9(6) . . ?
C18 C19 H19 121.1 . . ?
C20 C19 H19 121.1 . . ?
N1 C20 N4 111.7(5) . . ?
N1 C20 C19 123.3(7) . . ?
N4 C20 C19 125.0(6) . . ?
N5 C21 N4 104.3(5) . . ?
N5 C21 Nb1 137.5(4) . . ?
N4 C21 Nb1 118.2(5) . . ?
C23 C22 N5 108.5(6) . . ?
C23 C22 H22 125.8 . . ?
N5 C22 H22 125.8 . . ?
C22 C23 N4 106.5(5) . . ?
C22 C23 H23 126.7 . . ?
N4 C23 H23 126.7 . . ?
C29 C24 C25 122.6(6) . . ?
C29 C24 N5 117.4(5) . . ?
C25 C24 N5 120.0(6) . . ?
C26 C25 C24 117.3(6) . . ?
C26 C25 C33 119.6(5) . . ?
C24 C25 C33 123.1(6) . . ?
C27 C26 C25 122.0(6) . . ?
C27 C26 H26 119.0 . . ?
C25 C26 H26 119.0 . . ?
C26 C27 C28 119.5(7) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C29 C28 C27 121.5(6) . . ?
C29 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
C28 C29 C24 117.1(5) . . ?
C28 C29 C30 120.4(6) . . ?
C24 C29 C30 122.5(6) . . ?
C29 C30 C31 110.7(5) . . ?
C29 C30 C32 110.2(5) . . ?
C31 C30 C32 110.6(6) . . ?
C29 C30 H30 108.4 . . ?
C31 C30 H30 108.4 . . ?
C32 C30 H30 108.4 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C25 C33 C34 109.6(5) . . ?
C25 C33 C35 111.7(5) . . ?
C34 C33 C35 110.4(5) . . ?
C25 C33 H33 108.4 . . ?
C34 C33 H33 108.4 . . ?
C35 C33 H33 108.4 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O1A C36A C37A 89.2(14) . . ?
O1A C36A H36A 113.8 . . ?
C37A C36A H36A 113.8 . . ?
O1A C36A H36B 113.8 . . ?
C37A C36A H36B 113.8 . . ?
H36A C36A H36B 111.0 . . ?
C38A C37A C36A 102.8(16) . . ?
C38A C37A H37A 111.2 . . ?
C36A C37A H37A 111.2 . . ?
C38A C37A H37B 111.2 . . ?
C36A C37A H37B 111.2 . . ?
H37A C37A H37B 109.1 . . ?
C39A C38A C37A 98.7(9) . . ?
C39A C38A H38A 112.0 . . ?
C37A C38A H38A 112.0 . . ?
C39A C38A H38B 112.0 . . ?
C37A C38A H38B 112.0 . . ?
H38A C38A H38B 109.7 . . ?
O1A C39A C38A 104.4(13) . . ?
O1A C39A H39A 110.9 . . ?
C38A C39A H39A 110.9 . . ?
O1A C39A H39B 110.9 . . ?
C38A C39A H39B 110.9 . . ?
H39A C39A H39B 108.9 . . ?
O1B C36B H36C 111.5 . . ?
O1B C36B H36D 111.5 . . ?
H36C C36B H36D 109.3 . . ?
O1B C39B H39C 110.6 . . ?
O1B C39B H39D 110.6 . . ?
H39C C39B H39D 108.7 . . ?
C1 N1 C20 116.7(5) . . ?
C1 N1 Nb1 121.6(4) . . ?
C20 N1 Nb1 121.7(5) . . ?
C2 N2 C4 111.2(5) . . ?
C2 N2 C1 117.8(5) . . ?
C4 N2 C1 131.0(5) . . ?
C2 N3 C3 110.7(5) . . ?
C2 N3 C5 125.3(5) . . ?
C3 N3 C5 124.0(5) . . ?
C21 N4 C20 118.8(5) . . ?
C21 N4 C23 110.7(6) . . ?
C20 N4 C23 130.4(5) . . ?
C21 N5 C22 110.0(5) . . ?
C21 N5 C24 127.1(5) . . ?
C22 N5 C24 122.3(6) . . ?
C21 Nb1 C2 139.2(2) . . ?
C21 Nb1 N1 69.5(2) . . ?
C2 Nb1 N1 69.8(2) . . ?
C21 Nb1 Cl3 114.66(18) . . ?
C2 Nb1 Cl3 105.98(16) . . ?
N1 Nb1 Cl3 175.79(15) . . ?
C21 Nb1 Cl2 89.73(15) . . ?
C2 Nb1 Cl2 91.79(15) . . ?
N1 Nb1 Cl2 87.35(13) . . ?
Cl3 Nb1 Cl2 92.73(9) . . ?
C21 Nb1 Cl1 85.47(15) . . ?
C2 Nb1 Cl1 87.54(15) . . ?
N1 Nb1 Cl1 84.75(13) . . ?
Cl3 Nb1 Cl1 95.30(9) . . ?
Cl2 Nb1 Cl1 171.81(6) . . ?
C39A O1A C36A 106.2(19) . . ?
C36B O1B C39B 104.0(10) . . ?
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 N1 1.329(8) . ?
C1 C17 1.386(8) . ?
C1 N2 1.406(7) . ?
C2 N3 1.359(7) . ?
C2 N2 1.370(7) . ?
C2 Nb1 2.206(6) . ?
C3 C4 1.329(8) . ?
C3 N3 1.387(8) . ?
C3 H3 0.9500 . ?
C4 N2 1.386(8) . ?
C4 H4 0.9500 . ?
C5 C10 1.387(8) . ?
C5 C6 1.401(8) . ?
C5 N3 1.458(7) . ?
C6 C7 1.401(8) . ?
C6 C14 1.501(9) . ?
C7 C8 1.370(10) . ?
C7 H7 0.9500 . ?
C8 C9 1.372(10) . ?
C8 H8 0.9500 . ?
C9 C10 1.390(9) . ?
C9 H9 0.9500 . ?
C10 C11 1.514(9) . ?
C11 C12 1.520(11) . ?
C11 C13 1.532(10) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C16 1.516(10) . ?
C14 C15 1.521(9) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.391(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.369(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.381(8) . ?
C19 H19 0.9500 . ?
C20 N1 1.345(7) . ?
C20 N4 1.378(8) . ?
C21 N5 1.358(8) . ?
C21 N4 1.376(7) . ?
C21 Nb1 2.203(6) . ?
C22 C23 1.316(9) . ?
C22 N5 1.402(7) . ?
C22 H22 0.9500 . ?
C23 N4 1.398(7) . ?
C23 H23 0.9500 . ?
C24 C29 1.394(8) . ?
C24 C25 1.406(8) . ?
C24 N5 1.442(8) . ?
C25 C26 1.375(9) . ?
C25 C33 1.517(9) . ?
C26 C27 1.370(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.392(8) . ?
C27 H27 0.9500 . ?
C28 C29 1.384(9) . ?
C28 H28 0.9500 . ?
C29 C30 1.518(8) . ?
C30 C31 1.535(8) . ?
C30 C32 1.541(9) . ?
C30 H30 1.0000 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.527(8) . ?
C33 C35 1.539(8) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36A O1A 1.48(2) . ?
C36A C37A 1.508(19) . ?
C36A H36A 0.9900 . ?
C36A H36B 0.9900 . ?
C37A C38A 1.493(11) . ?
C37A H37A 0.9900 . ?
C37A H37B 0.9900 . ?
C38A C39A 1.485(15) . ?
C38A H38A 0.9900 . ?
C38A H38B 0.9900 . ?
C39A O1A 1.462(16) . ?
C39A H39A 0.9900 . ?
C39A H39B 0.9900 . ?
C36B O1B 1.444(15) . ?
C36B H36C 0.9900 . ?
C36B H36D 0.9900 . ?
C39B O1B 1.454(11) . ?
C39B H39C 0.9900 . ?
C39B H39D 0.9900 . ?
Cl1 Nb1 2.520(2) . ?
Cl2 Nb1 2.473(2) . ?
Cl3 Nb1 2.341(3) . ?
N1 Nb1 2.248(5) . ?
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
N3 C3 C4 N2 0.0(7) . . . . ?
C10 C5 C6 C7 -1.2(10) . . . . ?
N3 C5 C6 C7 -175.5(6) . . . . ?
C10 C5 C6 C14 177.0(6) . . . . ?
N3 C5 C6 C14 2.7(9) . . . . ?
C5 C6 C7 C8 -0.4(10) . . . . ?
C14 C6 C7 C8 -178.7(7) . . . . ?
C6 C7 C8 C9 0.2(12) . . . . ?
C7 C8 C9 C10 1.5(13) . . . . ?
C6 C5 C10 C9 2.7(10) . . . . ?
N3 C5 C10 C9 177.1(6) . . . . ?
C6 C5 C10 C11 -177.8(7) . . . . ?
N3 C5 C10 C11 -3.5(10) . . . . ?
C8 C9 C10 C5 -2.9(11) . . . . ?
C8 C9 C10 C11 177.6(7) . . . . ?
C5 C10 C11 C12 -126.2(7) . . . . ?
C9 C10 C11 C12 53.2(9) . . . . ?
C5 C10 C11 C13 110.4(7) . . . . ?
C9 C10 C11 C13 -70.2(9) . . . . ?
C5 C6 C14 C16 -106.2(7) . . . . ?
C7 C6 C14 C16 71.9(8) . . . . ?
C5 C6 C14 C15 131.3(7) . . . . ?
C7 C6 C14 C15 -50.5(8) . . . . ?
N1 C1 C17 C18 1.8(9) . . . . ?
N2 C1 C17 C18 -179.0(5) . . . . ?
C1 C17 C18 C19 1.1(9) . . . . ?
C17 C18 C19 C20 -1.6(9) . . . . ?
C18 C19 C20 N1 -0.7(9) . . . . ?
C18 C19 C20 N4 -179.6(6) . . . . ?
N5 C22 C23 N4 -0.2(6) . . . . ?
C29 C24 C25 C26 -1.8(9) . . . . ?
N5 C24 C25 C26 176.0(5) . . . . ?
C29 C24 C25 C33 -179.0(5) . . . . ?
N5 C24 C25 C33 -1.2(8) . . . . ?
C24 C25 C26 C27 1.1(9) . . . . ?
C33 C25 C26 C27 178.4(5) . . . . ?
C25 C26 C27 C28 -0.4(9) . . . . ?
C26 C27 C28 C29 0.2(9) . . . . ?
C27 C28 C29 C24 -0.8(9) . . . . ?
C27 C28 C29 C30 -179.3(6) . . . . ?
C25 C24 C29 C28 1.6(9) . . . . ?
N5 C24 C29 C28 -176.2(5) . . . . ?
C25 C24 C29 C30 -179.9(5) . . . . ?
N5 C24 C29 C30 2.3(8) . . . . ?
C28 C29 C30 C31 -52.9(8) . . . . ?
C24 C29 C30 C31 128.7(6) . . . . ?
C28 C29 C30 C32 69.7(7) . . . . ?
C24 C29 C30 C32 -108.7(7) . . . . ?
C26 C25 C33 C34 -68.6(7) . . . . ?
C24 C25 C33 C34 108.5(6) . . . . ?
C26 C25 C33 C35 54.0(7) . . . . ?
C24 C25 C33 C35 -128.8(6) . . . . ?
O1A C36A C37A C38A 60(2) . . . . ?
C36A C37A C38A C39A -46.0(17) . . . . ?
C37A C38A C39A O1A 11.3(17) . . . . ?
C17 C1 N1 C20 -4.0(8) . . . . ?
N2 C1 N1 C20 176.8(4) . . . . ?
C17 C1 N1 Nb1 175.8(4) . . . . ?
N2 C1 N1 Nb1 -3.5(6) . . . . ?
N4 C20 N1 C1 -177.6(5) . . . . ?
C19 C20 N1 C1 3.4(8) . . . . ?
N4 C20 N1 Nb1 2.7(6) . . . . ?
C19 C20 N1 Nb1 -176.4(4) . . . . ?
N3 C2 N2 C4 -0.6(6) . . . . ?
Nb1 C2 N2 C4 178.1(4) . . . . ?
N3 C2 N2 C1 -178.1(4) . . . . ?
Nb1 C2 N2 C1 0.6(6) . . . . ?
C3 C4 N2 C2 0.4(7) . . . . ?
C3 C4 N2 C1 177.4(5) . . . . ?
N1 C1 N2 C2 1.8(7) . . . . ?
C17 C1 N2 C2 -177.5(5) . . . . ?
N1 C1 N2 C4 -175.1(5) . . . . ?
C17 C1 N2 C4 5.6(9) . . . . ?
N2 C2 N3 C3 0.6(6) . . . . ?
Nb1 C2 N3 C3 -177.7(4) . . . . ?
N2 C2 N3 C5 -178.1(5) . . . . ?
Nb1 C2 N3 C5 3.5(8) . . . . ?
C4 C3 N3 C2 -0.4(7) . . . . ?
C4 C3 N3 C5 178.4(5) . . . . ?
C10 C5 N3 C2 89.6(7) . . . . ?
C6 C5 N3 C2 -95.7(7) . . . . ?
C10 C5 N3 C3 -89.0(7) . . . . ?
C6 C5 N3 C3 85.7(7) . . . . ?
N5 C21 N4 C20 -177.9(5) . . . . ?
Nb1 C21 N4 C20 3.0(7) . . . . ?
N5 C21 N4 C23 0.3(6) . . . . ?
Nb1 C21 N4 C23 -178.8(4) . . . . ?
N1 C20 N4 C21 -3.6(7) . . . . ?
C19 C20 N4 C21 175.4(5) . . . . ?
N1 C20 N4 C23 178.6(5) . . . . ?
C19 C20 N4 C23 -2.3(10) . . . . ?
C22 C23 N4 C21 -0.1(6) . . . . ?
C22 C23 N4 C20 177.9(6) . . . . ?
N4 C21 N5 C22 -0.5(6) . . . . ?
Nb1 C21 N5 C22 178.4(4) . . . . ?
N4 C21 N5 C24 170.5(5) . . . . ?
Nb1 C21 N5 C24 -10.6(9) . . . . ?
C23 C22 N5 C21 0.5(7) . . . . ?
C23 C22 N5 C24 -171.0(5) . . . . ?
C29 C24 N5 C21 -94.4(7) . . . . ?
C25 C24 N5 C21 87.7(7) . . . . ?
C29 C24 N5 C22 75.5(7) . . . . ?
C25 C24 N5 C22 -102.3(6) . . . . ?
N5 C21 Nb1 C2 -174.7(5) . . . . ?
N4 C21 Nb1 C2 4.1(6) . . . . ?
N5 C21 Nb1 N1 -179.9(6) . . . . ?
N4 C21 Nb1 N1 -1.1(4) . . . . ?
N5 C21 Nb1 Cl3 0.0(6) . . . . ?
N4 C21 Nb1 Cl3 178.8(3) . . . . ?
N5 C21 Nb1 Cl2 92.9(6) . . . . ?
N4 C21 Nb1 Cl2 -88.4(4) . . . . ?
N5 C21 Nb1 Cl1 -93.8(6) . . . . ?
N4 C21 Nb1 Cl1 85.0(4) . . . . ?
N3 C2 Nb1 C21 171.3(5) . . . . ?
N2 C2 Nb1 C21 -6.9(6) . . . . ?
N3 C2 Nb1 N1 176.4(6) . . . . ?
N2 C2 Nb1 N1 -1.7(4) . . . . ?
N3 C2 Nb1 Cl3 -3.7(6) . . . . ?
N2 C2 Nb1 Cl3 178.2(4) . . . . ?
N3 C2 Nb1 Cl2 -97.1(5) . . . . ?
N2 C2 Nb1 Cl2 84.8(4) . . . . ?
N3 C2 Nb1 Cl1 91.1(5) . . . . ?
N2 C2 Nb1 Cl1 -87.0(4) . . . . ?
C1 N1 Nb1 C21 179.3(5) . . . . ?
C20 N1 Nb1 C21 -0.9(4) . . . . ?
C1 N1 Nb1 C2 2.9(4) . . . . ?
C20 N1 Nb1 C2 -177.3(5) . . . . ?
C1 N1 Nb1 Cl2 -90.0(4) . . . . ?
C20 N1 Nb1 Cl2 89.8(4) . . . . ?
C1 N1 Nb1 Cl1 92.2(4) . . . . ?
C20 N1 Nb1 Cl1 -88.0(4) . . . . ?
C38A C39A O1A C36A 27(2) . . . . ?
C37A C36A O1A C39A -52(2) . . . . ?
