#------------------------------------------------------------------------------
#$Date: 2020-10-10 04:31:56 +0300 (Sat, 10 Oct 2020) $
#$Revision: 258285 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/93/1559327.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_1559327
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         'C56 H75 N4 Nb S'
_chemical_formula_sum            'C56 H75 N4 Nb S'
_chemical_formula_weight         929.17
_chemical_melting_point          442
_chemical_name_common            (κ1-BDI)Nb(NtBu)(NHtBu)(SCPh3)
_chemical_name_systematic
(tert-butyl)amino-(tert-butyl)imino-(triphenylmethylthiolato)-(N-(4-((2,6-diisopropylphenyl)imino)pent-2-en-2-yl)-2,6-diisopropylanilido)-niobium(V)
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-05-17
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-17 deposited with the CCDC.	2020-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                101.7150(10)
_cell_angle_beta                 96.702(2)
_cell_angle_gamma                90.848(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4066(4)
_cell_length_b                   13.5108(4)
_cell_length_c                   14.4569(4)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.91
_cell_volume                     2544.57(13)
_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 0.996
_diffrn_measured_fraction_theta_max 0.993
_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  0.0478
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            57967
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.426
_diffrn_reflns_theta_min         1.449
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0897 before and 0.0529 after correction.
The Ratio of minimum to maximum transmission is 0.9457.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexamethyldisiloxane'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         9328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0289P)²+2.0561P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8059
_reflns_number_total             9328
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc03489d2.cif
_cod_data_source_block           bmkxr44
_cod_database_code               1559327
_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   0.984
_shelx_estimated_absorpt_t_min   0.975
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(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)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C40(H40),
 C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49),
  C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), N4(H4)
2.c 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), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.20463(15) 0.36415(14) 0.81618(14) 0.0165(4) Uani 1 1 d . . . . .
C2 C 0.12425(15) 0.40876(14) 0.77878(15) 0.0180(4) Uani 1 1 d . . . . .
H2 H 0.062162 0.396694 0.801016 0.022 Uiso 1 1 calc R . . . .
C3 C 0.12071(15) 0.47328(14) 0.70837(15) 0.0167(4) Uani 1 1 d . . . . .
C4 C 0.30952(15) 0.37708(15) 0.79189(16) 0.0200(5) Uani 1 1 d . . . . .
H4A H 0.306574 0.401559 0.732328 0.030 Uiso 1 1 calc GR . . . .
H4B H 0.342022 0.311909 0.784312 0.030 Uiso 1 1 calc GR . . . .
H4C H 0.348286 0.426180 0.843195 0.030 Uiso 1 1 calc GR . . . .
C5 C 0.02365(16) 0.46312(16) 0.64158(16) 0.0251(5) Uani 1 1 d . . . . .
H5A H 0.016561 0.523263 0.613552 0.038 Uiso 1 1 calc GR . . . .
H5B H -0.033230 0.456620 0.677084 0.038 Uiso 1 1 calc GR . . . .
H5C H 0.024787 0.402909 0.590862 0.038 Uiso 1 1 calc GR . . . .
C6 C 0.10436(15) 0.29105(15) 0.91858(16) 0.0198(5) Uani 1 1 d . . . . .
C7 C 0.09634(17) 0.34419(16) 1.01204(16) 0.0248(5) Uani 1 1 d . . . . .
C8 C 0.00766(19) 0.33106(19) 1.0501(2) 0.0351(6) Uani 1 1 d . . . . .
H8 H 0.000785 0.365856 1.112978 0.042 Uiso 1 1 calc R . . . .
C9 C -0.07041(19) 0.2687(2) 0.9987(2) 0.0393(7) Uani 1 1 d . . . . .
H9 H -0.130239 0.260819 1.026203 0.047 Uiso 1 1 calc R . . . .
C10 C -0.06200(17) 0.21760(18) 0.9073(2) 0.0332(6) Uani 1 1 d . . . . .
H10 H -0.116318 0.174653 0.872647 0.040 Uiso 1 1 calc R . . . .
C11 C 0.02526(16) 0.22786(16) 0.86464(17) 0.0235(5) Uani 1 1 d . . . . .
C12 C 0.18118(18) 0.41389(17) 1.06952(16) 0.0285(5) Uani 1 1 d . . . . .
H12 H 0.245869 0.381715 1.055273 0.034 Uiso 1 1 calc R . . . .
C13 C 0.1816(2) 0.51570(19) 1.03976(19) 0.0434(7) Uani 1 1 d . . . . .
H13A H 0.186609 0.505228 0.971393 0.065 Uiso 1 1 calc GR . . . .
H13B H 0.239210 0.557901 1.075220 0.065 Uiso 1 1 calc GR . . . .
H13C H 0.119229 0.549504 1.053509 0.065 Uiso 1 1 calc GR . . . .
C14 C 0.1802(2) 0.4335(2) 1.17706(18) 0.0449(7) Uani 1 1 d . . . . .
H14A H 0.123653 0.475602 1.194392 0.067 Uiso 1 1 calc GR . . . .
H14B H 0.243322 0.468538 1.208832 0.067 Uiso 1 1 calc GR . . . .
H14C H 0.172995 0.368932 1.197079 0.067 Uiso 1 1 calc GR . . . .
C15 C 0.03151(17) 0.17149(16) 0.76380(17) 0.0266(5) Uani 1 1 d . . . . .
H15 H 0.094307 0.196175 0.743146 0.032 Uiso 1 1 calc R . . . .
C16 C -0.0572(2) 0.19306(19) 0.6951(2) 0.0416(7) Uani 1 1 d . . . . .
H16A H -0.119684 0.166990 0.712083 0.062 Uiso 1 1 calc GR . . . .
H16B H -0.048097 0.159816 0.629986 0.062 Uiso 1 1 calc GR . . . .
H16C H -0.060638 0.266218 0.699326 0.062 Uiso 1 1 calc GR . . . .
C17 C 0.03857(19) 0.05765(17) 0.75773(19) 0.0327(6) Uani 1 1 d . . . . .
H17A H 0.097149 0.044633 0.800225 0.049 Uiso 1 1 calc GR . . . .
H17B H 0.045618 0.024122 0.692168 0.049 Uiso 1 1 calc GR . . . .
H17C H -0.022524 0.031172 0.776913 0.049 Uiso 1 1 calc GR . . . .
C18 C 0.18879(15) 0.59097(15) 0.63162(15) 0.0182(4) Uani 1 1 d . . . . .
C19 C 0.14985(15) 0.68823(15) 0.64945(16) 0.0213(5) Uani 1 1 d . . . . .
C20 C 0.15332(16) 0.74632(16) 0.57937(17) 0.0252(5) Uani 1 1 d . . . . .
H20 H 0.127526 0.812251 0.589547 0.030 Uiso 1 1 calc R . . . .
C21 C 0.19352(17) 0.70934(17) 0.49605(17) 0.0274(5) Uani 1 1 d . . . . .
H21 H 0.196638 0.750306 0.450185 0.033 Uiso 1 1 calc R . . . .
C22 C 0.22913(17) 0.61290(16) 0.47944(16) 0.0246(5) Uani 1 1 d . . . . .
H22 H 0.255449 0.587587 0.421370 0.029 Uiso 1 1 calc R . . . .
C23 C 0.22723(15) 0.55192(15) 0.54623(15) 0.0201(5) Uani 1 1 d . . . . .
C24 C 0.26997(16) 0.44784(16) 0.52945(16) 0.0230(5) Uani 1 1 d . . . . .
H24 H 0.235900 0.406958 0.567936 0.028 Uiso 1 1 calc R . . . .
C25 C 0.2514(2) 0.39188(19) 0.42505(18) 0.0396(6) Uani 1 1 d . . . . .
H25A H 0.180480 0.395464 0.400822 0.059 Uiso 1 1 calc GR . . . .
H25B H 0.268505 0.320914 0.420478 0.059 Uiso 1 1 calc GR . . . .
H25C H 0.293484 0.423530 0.387177 0.059 Uiso 1 1 calc GR . . . .
C26 C 0.38219(17) 0.45480(18) 0.56515(18) 0.0303(5) Uani 1 1 d . . . . .
H26A H 0.417851 0.493486 0.527815 0.045 Uiso 1 1 calc GR . . . .
H26B H 0.408095 0.386569 0.558145 0.045 Uiso 1 1 calc GR . . . .
H26C H 0.392625 0.488802 0.632379 0.045 Uiso 1 1 calc GR . . . .
C27 C 0.10662(17) 0.73116(16) 0.74071(17) 0.0263(5) Uani 1 1 d . . . . .
H27 H 0.103398 0.675842 0.777043 0.032 Uiso 1 1 calc R . . . .
C28 C 0.00060(18) 0.76740(19) 0.7228(2) 0.0397(6) Uani 1 1 d . . . . .
H28A H 0.001661 0.822726 0.688331 0.060 Uiso 1 1 calc GR . . . .
H28B H -0.025169 0.791469 0.783808 0.060 Uiso 1 1 calc GR . . . .
H28C H -0.043020 0.711343 0.684802 0.060 Uiso 1 1 calc GR . . . .
C29 C 0.17389(18) 0.81751(19) 0.80316(18) 0.0345(6) Uani 1 1 d . . . . .
H29A H 0.240656 0.792561 0.819127 0.052 Uiso 1 1 calc GR . . . .
H29B H 0.144167 0.843085 0.861785 0.052 Uiso 1 1 calc GR . . . .
H29C H 0.179942 0.872213 0.768582 0.052 Uiso 1 1 calc GR . . . .
C30 C 0.24025(16) 0.08826(16) 1.05872(16) 0.0232(5) Uani 1 1 d . . . . .
C31 C 0.30139(19) -0.00728(18) 1.0468(2) 0.0367(6) Uani 1 1 d . . . . .
H31A H 0.293040 -0.041750 0.979695 0.055 Uiso 1 1 calc GR . . . .
H31B H 0.277701 -0.052578 1.085375 0.055 Uiso 1 1 calc GR . . . .
H31C H 0.372597 0.011294 1.067727 0.055 Uiso 1 1 calc GR . . . .
C32 C 0.12884(17) 0.06052(18) 1.02515(18) 0.0295(5) Uani 1 1 d . . . . .
H32A H 0.091189 0.122456 1.027897 0.044 Uiso 1 1 calc GR . . . .
H32B H 0.102725 0.019790 1.066546 0.044 Uiso 1 1 calc GR . . . .
H32C H 0.121347 0.021554 0.959538 0.044 Uiso 1 1 calc GR . . . .
C33 C 0.2530(2) 0.1456(2) 1.16174(17) 0.0382(6) Uani 1 1 d . . . . .
H33A H 0.324226 0.164064 1.182503 0.057 Uiso 1 1 calc GR . . . .
H33B H 0.228621 0.102602 1.202076 0.057 Uiso 1 1 calc GR . . . .
H33C H 0.214282 0.207038 1.166992 0.057 Uiso 1 1 calc GR . . . .
C34 C 0.51069(16) 0.30956(17) 1.06732(16) 0.0261(5) Uani 1 1 d . . . . .
C35 C 0.60990(19) 0.3575(2) 1.05277(19) 0.0416(7) Uani 1 1 d . . . . .
H35A H 0.642687 0.310153 1.006049 0.062 Uiso 1 1 calc GR . . . .
H35B H 0.653824 0.373141 1.113403 0.062 Uiso 1 1 calc GR . . . .
H35C H 0.596920 0.419891 1.029517 0.062 Uiso 1 1 calc GR . . . .
C36 C 0.4630(2) 0.3776(2) 1.14543(18) 0.0430(7) Uani 1 1 d . . . . .
H36A H 0.449375 0.442678 1.127494 0.065 Uiso 1 1 calc GR . . . .
H36B H 0.508951 0.388635 1.204820 0.065 Uiso 1 1 calc GR . . . .
H36C H 0.399881 0.345479 1.154542 0.065 Uiso 1 1 calc GR . . . .
C37 C 0.52989(19) 0.20677(19) 1.09248(18) 0.0361(6) Uani 1 1 d . . . . .
H37A H 0.466005 0.174755 1.099785 0.054 Uiso 1 1 calc GR . . . .
H37B H 0.574920 0.215693 1.152288 0.054 Uiso 1 1 calc GR . . . .
H37C H 0.561078 0.163735 1.041540 0.054 Uiso 1 1 calc GR . . . .
C38 C 0.39871(15) 0.05700(15) 0.69233(15) 0.0175(4) Uani 1 1 d . . . . .
C39 C 0.31494(16) 0.06495(15) 0.61174(15) 0.0206(5) Uani 1 1 d . . . . .
C40 C 0.24619(17) 0.14030(17) 0.62355(17) 0.0281(5) Uani 1 1 d . . . . .
H40 H 0.248707 0.185498 0.683483 0.034 Uiso 1 1 calc R . . . .
C41 C 0.17356(18) 0.15176(19) 0.55024(18) 0.0352(6) Uani 1 1 d . . . . .
H41 H 0.127803 0.204823 0.560007 0.042 Uiso 1 1 calc R . . . .
C42 C 0.16793(18) 0.08587(19) 0.46304(18) 0.0353(6) Uani 1 1 d . . . . .
H42 H 0.117741 0.092624 0.412841 0.042 Uiso 1 1 calc R . . . .
C43 C 0.23558(18) 0.01052(18) 0.44964(17) 0.0323(6) Uani 1 1 d . . . . .
H43 H 0.232257 -0.034687 0.389639 0.039 Uiso 1 1 calc R . . . .
C44 C 0.30904(17) -0.00041(17) 0.52298(16) 0.0257(5) Uani 1 1 d . . . . .
H44 H 0.355468 -0.052776 0.512496 0.031 Uiso 1 1 calc R . . . .
C45 C 0.44446(16) -0.04798(15) 0.67192(14) 0.0191(4) Uani 1 1 d . . . . .
C46 C 0.38390(17) -0.13371(15) 0.66865(16) 0.0234(5) Uani 1 1 d . . . . .
H46 H 0.316269 -0.125836 0.681548 0.028 Uiso 1 1 calc R . . . .
C47 C 0.42009(17) -0.23000(16) 0.64704(16) 0.0253(5) Uani 1 1 d . . . . .
H47 H 0.377512 -0.287329 0.645378 0.030 Uiso 1 1 calc R . . . .
C48 C 0.51789(17) -0.24266(16) 0.62795(16) 0.0263(5) Uani 1 1 d . . . . .
H48 H 0.543227 -0.308618 0.613816 0.032 Uiso 1 1 calc R . . . .
C49 C 0.57887(17) -0.15911(17) 0.62944(16) 0.0262(5) Uani 1 1 d . . . . .
H49 H 0.646091 -0.167688 0.615476 0.031 Uiso 1 1 calc R . . . .
C50 C 0.54230(16) -0.06188(16) 0.65140(15) 0.0220(5) Uani 1 1 d . . . . .
H50 H 0.584908 -0.004810 0.652261 0.026 Uiso 1 1 calc R . . . .
C51 C 0.48090(15) 0.14032(15) 0.70397(15) 0.0183(4) Uani 1 1 d . . . . .
C52 C 0.55251(15) 0.16009(15) 0.78480(15) 0.0206(5) Uani 1 1 d . . . . .
H52 H 0.545288 0.127580 0.836201 0.025 Uiso 1 1 calc R . . . .
C53 C 0.63356(16) 0.22640(17) 0.79055(17) 0.0267(5) Uani 1 1 d . . . . .
H53 H 0.681565 0.238822 0.845785 0.032 Uiso 1 1 calc R . . . .
C54 C 0.64555(17) 0.27489(17) 0.71677(17) 0.0288(5) Uani 1 1 d . . . . .
H54 H 0.701572 0.320156 0.720959 0.035 Uiso 1 1 calc R . . . .
C55 C 0.57510(17) 0.25673(17) 0.63694(18) 0.0302(5) Uani 1 1 d . . . . .
H55 H 0.582464 0.290160 0.586178 0.036 Uiso 1 1 calc R . . . .
C56 C 0.49356(16) 0.18993(16) 0.63032(16) 0.0240(5) Uani 1 1 d . . . . .
H56 H 0.445849 0.177929 0.574875 0.029 Uiso 1 1 calc R . . . .
N1 N 0.19807(12) 0.29943(12) 0.87964(12) 0.0157(4) Uani 1 1 d . . . . .
N2 N 0.19490(12) 0.53287(12) 0.70452(12) 0.0181(4) Uani 1 1 d . . . . .
N3 N 0.27691(13) 0.15275(12) 0.99878(12) 0.0186(4) Uani 1 1 d . . . . .
N4 N 0.44183(13) 0.29440(13) 0.97694(12) 0.0204(4) Uani 1 1 d . . . . .
H4 H 0.462281 0.332488 0.939610 0.024 Uiso 1 1 calc R . . . .
S1 S 0.34126(4) 0.05881(4) 0.80552(4) 0.01887(12) Uani 1 1 d . . . . .
Nb1 Nb 0.31864(2) 0.21520(2) 0.91483(2) 0.01563(6) 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'
S S 0.1246 0.1234 '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
C2 C1 C4 123.47(18) . . ?
C2 C1 N1 123.31(18) . . ?
N1 C1 C4 113.20(16) . . ?
C1 C2 H2 115.8 . . ?
C1 C2 C3 128.32(19) . . ?
C3 C2 H2 115.8 . . ?
C2 C3 C5 114.61(17) . . ?
N2 C3 C2 121.85(18) . . ?
N2 C3 C5 123.54(18) . . ?
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 118.70(19) . . ?
C11 C6 C7 121.5(2) . . ?
C11 C6 N1 119.72(19) . . ?
C6 C7 C12 121.4(2) . . ?
C8 C7 C6 117.9(2) . . ?
C8 C7 C12 120.7(2) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 C7 121.4(2) . . ?
C9 C8 H8 119.3 . . ?
C8 C9 H9 119.9 . . ?
C8 C9 C10 120.2(2) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 119.4 . . ?
C9 C10 C11 121.2(2) . . ?
C11 C10 H10 119.4 . . ?
C6 C11 C15 122.47(19) . . ?
C10 C11 C6 117.7(2) . . ?
C10 C11 C15 119.8(2) . . ?
C7 C12 H12 107.5 . . ?
C7 C12 C13 111.00(19) . . ?
C7 C12 C14 114.9(2) . . ?
C13 C12 H12 107.5 . . ?
C13 C12 C14 108.0(2) . . ?
C14 C12 H12 107.5 . . ?
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 107.7 . . ?
C11 C15 C16 111.6(2) . . ?
C11 C15 C17 111.79(19) . . ?
C16 C15 H15 107.7 . . ?
C17 C15 H15 107.7 . . ?
C17 C15 C16 110.22(19) . . ?
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 119.37(19) . . ?
C23 C18 C19 121.47(19) . . ?
C23 C18 N2 119.05(18) . . ?
C18 C19 C27 122.24(19) . . ?
C20 C19 C18 117.6(2) . . ?
C20 C19 C27 120.15(19) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 C19 121.2(2) . . ?
C21 C20 H20 119.4 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.0(2) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 119.4 . . ?
C21 C22 C23 121.2(2) . . ?
C23 C22 H22 119.4 . . ?
C18 C23 C24 120.41(19) . . ?
C22 C23 C18 118.46(19) . . ?
C22 C23 C24 121.1(2) . . ?
C23 C24 H24 107.6 . . ?
C23 C24 C25 113.22(18) . . ?
C23 C24 C26 110.15(18) . . ?
C25 C24 H24 107.6 . . ?
C26 C24 H24 107.6 . . ?
C26 C24 C25 110.44(19) . . ?
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 . . ?
C19 C27 H27 107.7 . . ?
C19 C27 C28 112.6(2) . . ?
C19 C27 C29 111.56(19) . . ?
C28 C27 H27 107.7 . . ?
C28 C27 C29 109.52(19) . . ?
C29 C27 H27 107.7 . . ?
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 . . ?
C31 C30 C32 110.07(19) . . ?
C33 C30 C31 111.3(2) . . ?
C33 C30 C32 109.8(2) . . ?
N3 C30 C31 107.59(18) . . ?
N3 C30 C32 108.76(17) . . ?
N3 C30 C33 109.26(18) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C36 C34 C35 110.4(2) . . ?
C36 C34 C37 110.4(2) . . ?
C37 C34 C35 109.2(2) . . ?
N4 C34 C35 108.79(19) . . ?
N4 C34 C36 109.43(18) . . ?
N4 C34 C37 108.60(18) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 S1 109.23(14) . . ?
C45 C38 C39 109.84(16) . . ?
C45 C38 S1 103.49(13) . . ?
C51 C38 C39 111.34(16) . . ?
C51 C38 C45 110.20(16) . . ?
C51 C38 S1 112.45(14) . . ?
C40 C39 C38 121.02(19) . . ?
C40 C39 C44 117.7(2) . . ?
C44 C39 C38 121.19(19) . . ?
C39 C40 H40 119.1 . . ?
C39 C40 C41 121.8(2) . . ?
C41 C40 H40 119.1 . . ?
C40 C41 H41 120.1 . . ?
C42 C41 C40 119.9(2) . . ?
C42 C41 H41 120.1 . . ?
C41 C42 H42 120.3 . . ?
C43 C42 C41 119.3(2) . . ?
C43 C42 H42 120.3 . . ?
C42 C43 H43 119.6 . . ?
C42 C43 C44 120.8(2) . . ?
C44 C43 H43 119.6 . . ?
C39 C44 H44 119.7 . . ?
C43 C44 C39 120.5(2) . . ?
C43 C44 H44 119.7 . . ?
C46 C45 C38 119.10(18) . . ?
C50 C45 C38 122.85(18) . . ?
C50 C45 C46 117.95(19) . . ?
C45 C46 H46 119.3 . . ?
C47 C46 C45 121.5(2) . . ?
C47 C46 H46 119.3 . . ?
C46 C47 H47 120.0 . . ?
C48 C47 C46 119.9(2) . . ?
C48 C47 H47 120.0 . . ?
C47 C48 H48 120.2 . . ?
C47 C48 C49 119.7(2) . . ?
C49 C48 H48 120.2 . . ?
C48 C49 H49 119.8 . . ?
C48 C49 C50 120.3(2) . . ?
C50 C49 H49 119.8 . . ?
C45 C50 C49 120.6(2) . . ?
C45 C50 H50 119.7 . . ?
C49 C50 H50 119.7 . . ?
C52 C51 C38 120.47(19) . . ?
C56 C51 C38 121.07(18) . . ?
C56 C51 C52 118.04(19) . . ?
C51 C52 H52 119.7 . . ?
C53 C52 C51 120.7(2) . . ?
C53 C52 H52 119.7 . . ?
C52 C53 H53 119.6 . . ?
C52 C53 C54 120.7(2) . . ?
C54 C53 H53 119.6 . . ?
C53 C54 H54 120.4 . . ?
C55 C54 C53 119.2(2) . . ?
C55 C54 H54 120.4 . . ?
C54 C55 H55 119.8 . . ?
C54 C55 C56 120.5(2) . . ?
C56 C55 H55 119.8 . . ?
C51 C56 H56 119.6 . . ?
C55 C56 C51 120.8(2) . . ?
C55 C56 H56 119.6 . . ?
C1 N1 C6 118.66(15) . . ?
C1 N1 Nb1 120.68(13) . . ?
C6 N1 Nb1 120.66(12) . . ?
C3 N2 C18 119.36(17) . . ?
C30 N3 Nb1 172.25(15) . . ?
C34 N4 H4 110.2 . . ?
C34 N4 Nb1 139.51(15) . . ?
Nb1 N4 H4 110.2 . . ?
C38 S1 Nb1 121.63(6) . . ?
N1 Nb1 S1 117.21(5) . . ?
N3 Nb1 N1 103.71(7) . . ?
N3 Nb1 N4 106.73(8) . . ?
N3 Nb1 S1 92.92(6) . . ?
N4 Nb1 N1 115.29(7) . . ?
N4 Nb1 S1 116.58(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 1.354(3) . ?
C1 C4 1.505(3) . ?
C1 N1 1.399(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.466(3) . ?
C3 C5 1.514(3) . ?
C3 N2 1.284(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 1.413(3) . ?
C6 C11 1.404(3) . ?
C6 N1 1.447(3) . ?
C7 C8 1.391(3) . ?
C7 C12 1.517(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.377(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.378(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.403(3) . ?
C11 C15 1.514(3) . ?
C12 H12 1.0000 . ?
C12 C13 1.522(3) . ?
C12 C14 1.525(3) . ?
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 1.529(3) . ?
C15 C17 1.528(3) . ?
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 1.407(3) . ?
C18 C23 1.400(3) . ?
C18 N2 1.432(3) . ?
C19 C20 1.406(3) . ?
C19 C27 1.513(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.381(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.379(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.393(3) . ?
C23 C24 1.511(3) . ?
C24 H24 1.0000 . ?
C24 C25 1.535(3) . ?
C24 C26 1.528(3) . ?
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 1.521(3) . ?
C27 C29 1.530(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 C31 1.530(3) . ?
C30 C32 1.532(3) . ?
C30 C33 1.522(3) . ?
C30 N3 1.465(3) . ?
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 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.526(3) . ?
C34 C36 1.514(3) . ?
C34 C37 1.524(3) . ?
C34 N4 1.485(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.543(3) . ?
C38 C45 1.540(3) . ?
C38 C51 1.534(3) . ?
C38 S1 1.884(2) . ?
C39 C40 1.382(3) . ?
C39 C44 1.395(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.388(3) . ?
C41 H41 0.9500 . ?
C41 C42 1.381(4) . ?
C42 H42 0.9500 . ?
C42 C43 1.373(3) . ?
C43 H43 0.9500 . ?
C43 C44 1.393(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.394(3) . ?
C45 C50 1.385(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.384(3) . ?
C47 H47 0.9500 . ?
C47 C48 1.377(3) . ?
C48 H48 0.9500 . ?
C48 C49 1.379(3) . ?
C49 H49 0.9500 . ?
C49 C50 1.397(3) . ?
C50 H50 0.9500 . ?
C51 C52 1.401(3) . ?
C51 C56 1.393(3) . ?
C52 H52 0.9500 . ?
C52 C53 1.382(3) . ?
C53 H53 0.9500 . ?
C53 C54 1.383(3) . ?
C54 H54 0.9500 . ?
C54 C55 1.381(3) . ?
C55 H55 0.9500 . ?
C55 C56 1.389(3) . ?
C56 H56 0.9500 . ?
N1 Nb1 2.0651(16) . ?
N3 Nb1 1.7486(17) . ?
N4 H4 0.8800 . ?
N4 Nb1 1.9724(17) . ?
S1 Nb1 2.4143(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
C1 C2 C3 C5 146.7(2) . . . . ?
C1 C2 C3 N2 -33.1(3) . . . . ?
C2 C1 N1 C6 -9.5(3) . . . . ?
C2 C1 N1 Nb1 169.17(15) . . . . ?
C2 C3 N2 C18 177.37(18) . . . . ?
C4 C1 C2 C3 1.9(3) . . . . ?
C4 C1 N1 C6 171.90(17) . . . . ?
C4 C1 N1 Nb1 -9.4(2) . . . . ?
C5 C3 N2 C18 -2.4(3) . . . . ?
C6 C7 C8 C9 -0.3(3) . . . . ?
C6 C7 C12 C13 79.4(3) . . . . ?
C6 C7 C12 C14 -157.7(2) . . . . ?
C6 C11 C15 C16 -126.2(2) . . . . ?
C6 C11 C15 C17 109.8(2) . . . . ?
C7 C6 C11 C10 -1.1(3) . . . . ?
C7 C6 C11 C15 179.00(18) . . . . ?
C7 C6 N1 C1 -101.3(2) . . . . ?
C7 C6 N1 Nb1 80.0(2) . . . . ?
C7 C8 C9 C10 -0.1(4) . . . . ?
C8 C7 C12 C13 -100.4(3) . . . . ?
C8 C7 C12 C14 22.6(3) . . . . ?
C8 C9 C10 C11 -0.2(3) . . . . ?
C9 C10 C11 C6 0.8(3) . . . . ?
C9 C10 C11 C15 -179.4(2) . . . . ?
C10 C11 C15 C16 53.9(3) . . . . ?
C10 C11 C15 C17 -70.1(2) . . . . ?
C11 C6 C7 C8 0.9(3) . . . . ?
C11 C6 C7 C12 -178.88(18) . . . . ?
C11 C6 N1 C1 81.1(2) . . . . ?
C11 C6 N1 Nb1 -97.58(19) . . . . ?
C12 C7 C8 C9 179.5(2) . . . . ?
C18 C19 C20 C21 0.0(3) . . . . ?
C18 C19 C27 C28 -126.0(2) . . . . ?
C18 C19 C27 C29 110.4(2) . . . . ?
C18 C23 C24 C25 146.1(2) . . . . ?
C18 C23 C24 C26 -89.7(2) . . . . ?
C19 C18 C23 C22 1.9(3) . . . . ?
C19 C18 C23 C24 179.12(19) . . . . ?
C19 C18 N2 C3 90.7(2) . . . . ?
C19 C20 C21 C22 1.5(3) . . . . ?
C20 C19 C27 C28 54.8(3) . . . . ?
C20 C19 C27 C29 -68.8(3) . . . . ?
C20 C21 C22 C23 -1.2(3) . . . . ?
C21 C22 C23 C18 -0.4(3) . . . . ?
C21 C22 C23 C24 -177.6(2) . . . . ?
C22 C23 C24 C25 -36.8(3) . . . . ?
C22 C23 C24 C26 87.4(2) . . . . ?
C23 C18 C19 C20 -1.7(3) . . . . ?
C23 C18 C19 C27 179.11(19) . . . . ?
C23 C18 N2 C3 -93.0(2) . . . . ?
C27 C19 C20 C21 179.2(2) . . . . ?
C35 C34 N4 Nb1 161.62(18) . . . . ?
C36 C34 N4 Nb1 -77.7(3) . . . . ?
C37 C34 N4 Nb1 42.8(3) . . . . ?
C38 C39 C40 C41 176.6(2) . . . . ?
C38 C39 C44 C43 -177.2(2) . . . . ?
C38 C45 C46 C47 177.51(19) . . . . ?
C38 C45 C50 C49 -177.28(19) . . . . ?
C38 C51 C52 C53 172.23(19) . . . . ?
C38 C51 C56 C55 -172.4(2) . . . . ?
C39 C38 C45 C46 -63.5(2) . . . . ?
C39 C38 C45 C50 112.9(2) . . . . ?
C39 C38 C51 C52 166.66(18) . . . . ?
C39 C38 C51 C56 -20.9(3) . . . . ?
C39 C38 S1 Nb1 -89.30(13) . . . . ?
C39 C40 C41 C42 0.9(4) . . . . ?
C40 C39 C44 C43 -0.3(3) . . . . ?
C40 C41 C42 C43 -1.0(4) . . . . ?
C41 C42 C43 C44 0.4(4) . . . . ?
C42 C43 C44 C39 0.3(4) . . . . ?
C44 C39 C40 C41 -0.2(3) . . . . ?
C45 C38 C39 C40 164.1(2) . . . . ?
C45 C38 C39 C44 -19.2(3) . . . . ?
C45 C38 C51 C52 -71.2(2) . . . . ?
C45 C38 C51 C56 101.3(2) . . . . ?
C45 C38 S1 Nb1 153.74(10) . . . . ?
C45 C46 C47 C48 -0.2(3) . . . . ?
C46 C45 C50 C49 -0.9(3) . . . . ?
C46 C47 C48 C49 -0.7(3) . . . . ?
C47 C48 C49 C50 0.8(3) . . . . ?
C48 C49 C50 C45 0.0(3) . . . . ?
C50 C45 C46 C47 0.9(3) . . . . ?
C51 C38 C39 C40 -73.6(3) . . . . ?
C51 C38 C39 C44 103.2(2) . . . . ?
C51 C38 C45 C46 173.52(19) . . . . ?
C51 C38 C45 C50 -10.1(3) . . . . ?
C51 C38 S1 Nb1 34.84(16) . . . . ?
C51 C52 C53 C54 0.2(3) . . . . ?
C52 C51 C56 C55 0.2(3) . . . . ?
C52 C53 C54 C55 0.3(3) . . . . ?
C53 C54 C55 C56 -0.5(4) . . . . ?
C54 C55 C56 C51 0.3(4) . . . . ?
C56 C51 C52 C53 -0.5(3) . . . . ?
N1 C1 C2 C3 -176.52(19) . . . . ?
N1 C6 C7 C8 -176.68(18) . . . . ?
N1 C6 C7 C12 3.6(3) . . . . ?
N1 C6 C11 C10 176.42(17) . . . . ?
N1 C6 C11 C15 -3.5(3) . . . . ?
N2 C18 C19 C20 174.49(18) . . . . ?
N2 C18 C19 C27 -4.7(3) . . . . ?
N2 C18 C23 C22 -174.27(18) . . . . ?
N2 C18 C23 C24 2.9(3) . . . . ?
S1 C38 C39 C40 51.2(2) . . . . ?
S1 C38 C39 C44 -132.06(18) . . . . ?
S1 C38 C45 C46 53.1(2) . . . . ?
S1 C38 C45 C50 -130.53(18) . . . . ?
S1 C38 C51 C52 43.7(2) . . . . ?
S1 C38 C51 C56 -143.84(17) . . . . ?
