#------------------------------------------------------------------------------
#$Date: 2022-09-04 01:56:11 +0300 (Sun, 04 Sep 2022) $
#$Revision: 277615 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/11/7711141.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_7711141
loop_
_publ_author_name
'Griffin, Samuel E.'
'Adamczyk, Olivia V.'
'Schafer, Laurel L.'
_publ_section_title
;
 Vanadium Pyridonates: Dimerization, Redox Behaviour, and Metal-Ligand
 Cooperativity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02177C
_journal_year                    2022
_chemical_formula_moiety         'C45 H48 N3 O3 V'
_chemical_formula_sum            'C45 H48 N3 O3 V'
_chemical_formula_weight         729.80
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-01 deposited with the CCDC.	2022-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.0650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9174(3)
_cell_length_b                   12.5107(2)
_cell_length_c                   23.1488(5)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.18
_cell_measurement_theta_min      2.96
_cell_volume                     3990.72(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker-Nonius Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            50659
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.194
_diffrn_reflns_theta_min         1.854
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0450 before and 0.0428 after correction. The Ratio of minimum to maximum transmission is 0.9381. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       rod
_exptl_crystal_F_000             1544
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/hexanes'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         10770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0416
_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)+(0.0426P)²+2.2265P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7856
_reflns_number_total             10770
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt02177c3.cif
_cod_data_source_block           ls919
_cod_database_code               7711141
_shelx_shelxl_version_number     2018/1
_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   0.983
_shelx_estimated_absorpt_t_min   0.941
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C11(H11), C18(H18), C19(H19), C24(H24), C26(H26),
 C33(H33), C34(H34), C39(H39), C41(H41)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C36(H36A,
 H36B,H36C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_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
V1 V 0.23866(2) 0.53915(2) 0.47878(2) 0.01580(7) Uani 1 1 d . . . . .
O1 O 0.15998(8) 0.55112(9) 0.54487(5) 0.0203(2) Uani 1 1 d . . . . .
O2 O 0.30596(8) 0.58644(9) 0.41472(4) 0.0184(2) Uani 1 1 d . . . . .
O3 O 0.21842(8) 0.38489(9) 0.47102(4) 0.0191(2) Uani 1 1 d . . . . .
N1 N 0.26121(9) 0.68151(11) 0.53104(5) 0.0184(3) Uani 1 1 d . . . . .
N2 N 0.14714(9) 0.61302(10) 0.40911(5) 0.0163(3) Uani 1 1 d . . . . .
N3 N 0.34755(9) 0.44821(11) 0.52749(5) 0.0182(3) Uani 1 1 d . . . . .
C1 C 0.20204(11) 0.63811(13) 0.56661(6) 0.0181(3) Uani 1 1 d . . . . .
C2 C 0.19206(12) 0.68174(13) 0.62141(7) 0.0200(3) Uani 1 1 d . . . . .
C3 C 0.24685(13) 0.77133(14) 0.63759(7) 0.0247(4) Uani 1 1 d . . . . .
H3 H 0.243466 0.803144 0.674510 0.030 Uiso 1 1 calc R . . . .
C4 C 0.30742(13) 0.81645(14) 0.60070(7) 0.0252(4) Uani 1 1 d . . . . .
H4 H 0.343924 0.878871 0.612377 0.030 Uiso 1 1 calc R . . . .
C5 C 0.31394(12) 0.76991(13) 0.54725(7) 0.0209(3) Uani 1 1 d . . . . .
C6 C 0.37616(13) 0.81387(15) 0.50493(8) 0.0276(4) Uani 1 1 d . . . . .
H6A H 0.394044 0.756089 0.479914 0.041 Uiso 1 1 calc GR . . . .
H6B H 0.435036 0.845348 0.526463 0.041 Uiso 1 1 calc GR . . . .
H6C H 0.340036 0.868888 0.480774 0.041 Uiso 1 1 calc GR . . . .
C7 C 0.13126(12) 0.62698(13) 0.66068(6) 0.0197(3) Uani 1 1 d . . . . .
C8 C 0.03508(12) 0.65839(14) 0.66263(7) 0.0224(3) Uani 1 1 d . . . . .
C9 C -0.01583(12) 0.61094(15) 0.70400(7) 0.0253(4) Uani 1 1 d . . . . .
H9 H -0.080631 0.632887 0.705978 0.030 Uiso 1 1 calc R . . . .
C10 C 0.02547(13) 0.53307(15) 0.74205(7) 0.0250(4) Uani 1 1 d . . . . .
C11 C 0.11818(13) 0.49720(15) 0.73607(7) 0.0244(3) Uani 1 1 d . . . . .
H11 H 0.145747 0.440453 0.760169 0.029 Uiso 1 1 calc R . . . .
C12 C 0.17168(12) 0.54222(14) 0.69570(7) 0.0212(3) Uani 1 1 d . . . . .
C13 C -0.01443(14) 0.73907(16) 0.62012(8) 0.0324(4) Uani 1 1 d . . . . .
H13A H 0.030688 0.797415 0.615176 0.049 Uiso 1 1 calc GR . . . .
H13B H -0.071572 0.767814 0.635151 0.049 Uiso 1 1 calc GR . . . .
H13C H -0.034605 0.704442 0.582394 0.049 Uiso 1 1 calc GR . . . .
C14 C -0.02736(14) 0.48707(17) 0.78908(8) 0.0340(4) Uani 1 1 d . . . . .
H14A H -0.083671 0.531858 0.793426 0.051 Uiso 1 1 calc GR . . . .
H14B H 0.016486 0.485114 0.826093 0.051 Uiso 1 1 calc GR . . . .
H14C H -0.049168 0.414400 0.778230 0.051 Uiso 1 1 calc GR . . . .
C15 C 0.27109(13) 0.49953(16) 0.68920(8) 0.0282(4) Uani 1 1 d . . . . .
H15A H 0.270700 0.471870 0.649561 0.042 Uiso 1 1 calc GR . . . .
H15B H 0.288125 0.441842 0.717426 0.042 Uiso 1 1 calc GR . . . .
H15C H 0.318964 0.557159 0.696401 0.042 Uiso 1 1 calc GR . . . .
C16 C 0.22740(11) 0.62806(12) 0.38338(6) 0.0158(3) Uani 1 1 d . . . . .
C17 C 0.22610(11) 0.68327(13) 0.33073(6) 0.0168(3) Uani 1 1 d . . . . .
C18 C 0.13688(12) 0.72545(13) 0.30706(7) 0.0204(3) Uani 1 1 d . . . . .
H18 H 0.132072 0.765499 0.271902 0.024 Uiso 1 1 calc R . . . .
C19 C 0.05435(12) 0.71020(13) 0.33383(7) 0.0214(3) Uani 1 1 d . . . . .
H19 H -0.006075 0.739316 0.316782 0.026 Uiso 1 1 calc R . . . .
C20 C 0.06041(11) 0.65233(13) 0.38553(7) 0.0184(3) Uani 1 1 d . . . . .
C21 C -0.02395(12) 0.63142(15) 0.41739(8) 0.0248(4) Uani 1 1 d . . . . .
H21A H -0.007460 0.653274 0.458231 0.037 Uiso 1 1 calc GR . . . .
H21B H -0.039441 0.554977 0.415599 0.037 Uiso 1 1 calc GR . . . .
H21C H -0.080274 0.672313 0.399224 0.037 Uiso 1 1 calc GR . . . .
C22 C 0.31531(11) 0.69149(13) 0.30213(6) 0.0175(3) Uani 1 1 d . . . . .
C23 C 0.36459(12) 0.78896(13) 0.30036(7) 0.0198(3) Uani 1 1 d . . . . .
C24 C 0.44522(12) 0.79408(14) 0.27091(7) 0.0256(4) Uani 1 1 d . . . . .
H24 H 0.478155 0.860314 0.269409 0.031 Uiso 1 1 calc R . . . .
C25 C 0.47891(13) 0.70562(15) 0.24374(8) 0.0275(4) Uani 1 1 d . . . . .
C26 C 0.43112(13) 0.60914(14) 0.24767(7) 0.0247(4) Uani 1 1 d . . . . .
H26 H 0.454326 0.547391 0.230149 0.030 Uiso 1 1 calc R . . . .
C27 C 0.35009(12) 0.60004(13) 0.27655(6) 0.0201(3) Uani 1 1 d . . . . .
C28 C 0.33335(13) 0.88637(14) 0.33137(7) 0.0248(4) Uani 1 1 d . . . . .
H28A H 0.268980 0.909167 0.312821 0.037 Uiso 1 1 calc GR . . . .
H28B H 0.380060 0.944292 0.329031 0.037 Uiso 1 1 calc GR . . . .
H28C H 0.330735 0.868924 0.372389 0.037 Uiso 1 1 calc GR . . . .
C29 C 0.56385(18) 0.7141(2) 0.21025(12) 0.0442(6) Uani 1 1 d . . . . .
H29A H 0.5543(19) 0.761(2) 0.1801(12) 0.066 Uiso 1 1 d R . . . .
H29B H 0.620(2) 0.744(2) 0.2363(12) 0.066 Uiso 1 1 d R . . . .
C30 C 0.30122(13) 0.49328(14) 0.27954(7) 0.0254(4) Uani 1 1 d . . . . .
H30A H 0.315192 0.464889 0.319286 0.038 Uiso 1 1 calc GR . . . .
H30B H 0.325680 0.443593 0.252290 0.038 Uiso 1 1 calc GR . . . .
H30C H 0.230952 0.501826 0.268981 0.038 Uiso 1 1 calc GR . . . .
C31 C 0.29564(11) 0.35994(13) 0.50906(6) 0.0176(3) Uani 1 1 d . . . . .
C32 C 0.32268(11) 0.25755(13) 0.52997(6) 0.0187(3) Uani 1 1 d . . . . .
C33 C 0.40765(12) 0.25286(15) 0.56952(7) 0.0238(3) Uani 1 1 d . . . . .
H33 H 0.429714 0.185347 0.584807 0.029 Uiso 1 1 calc R . . . .
C34 C 0.46140(12) 0.34374(14) 0.58743(7) 0.0240(4) Uani 1 1 d . . . . .
H34 H 0.519637 0.337835 0.614072 0.029 Uiso 1 1 calc R . . . .
C35 C 0.42943(11) 0.44251(14) 0.56620(6) 0.0203(3) Uani 1 1 d . . . . .
C36 C 0.48003(12) 0.54501(15) 0.58408(7) 0.0260(4) Uani 1 1 d . . . . .
H36A H 0.486605 0.587550 0.549306 0.039 Uiso 1 1 calc GR . . . .
H36B H 0.544550 0.529612 0.605272 0.039 Uiso 1 1 calc GR . . . .
H36C H 0.442150 0.585137 0.609410 0.039 Uiso 1 1 calc GR . . . .
C37 C 0.26143(11) 0.16210(13) 0.51313(7) 0.0198(3) Uani 1 1 d . . . . .
C38 C 0.24712(12) 0.12523(14) 0.45518(7) 0.0242(3) Uani 1 1 d . . . . .
C39 C 0.18953(13) 0.03533(15) 0.44116(8) 0.0299(4) Uani 1 1 d . . . . .
H39 H 0.180005 0.010529 0.401982 0.036 Uiso 1 1 calc R . . . .
C40 C 0.14562(14) -0.01913(14) 0.48270(9) 0.0324(4) Uani 1 1 d . . . . .
C41 C 0.16030(14) 0.01858(15) 0.53952(9) 0.0319(4) Uani 1 1 d . . . . .
H41 H 0.130522 -0.017724 0.568392 0.038 Uiso 1 1 calc R . . . .
C42 C 0.21735(13) 0.10806(14) 0.55563(7) 0.0253(4) Uani 1 1 d . . . . .
C43 C 0.29420(14) 0.18077(17) 0.40863(8) 0.0329(4) Uani 1 1 d . . . . .
H43A H 0.266065 0.252222 0.401722 0.049 Uiso 1 1 calc GR . . . .
H43B H 0.283014 0.139148 0.372444 0.049 Uiso 1 1 calc GR . . . .
H43C H 0.364129 0.187051 0.421447 0.049 Uiso 1 1 calc GR . . . .
C44 C 0.08547(16) -0.11832(17) 0.46694(11) 0.0475(6) Uani 1 1 d . . . . .
H44A H 0.054359 -0.113255 0.426341 0.071 Uiso 1 1 calc GR . . . .
H44B H 0.035570 -0.124500 0.492706 0.071 Uiso 1 1 calc GR . . . .
H44C H 0.127510 -0.181473 0.471549 0.071 Uiso 1 1 calc GR . . . .
C45 C 0.22944(15) 0.14434(17) 0.61849(8) 0.0362(5) Uani 1 1 d . . . . .
H45A H 0.289572 0.114505 0.639402 0.054 Uiso 1 1 calc GR . . . .
H45B H 0.174145 0.119465 0.636810 0.054 Uiso 1 1 calc GR . . . .
H45C H 0.232432 0.222563 0.620028 0.054 Uiso 1 1 calc GR . . . .
H29C H 0.5825(19) 0.645(2) 0.1970(11) 0.060(8) Uiso 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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
O1 V1 N1 64.02(5) . . ?
O1 V1 N2 102.31(5) . . ?
O1 V1 N3 93.50(5) . . ?
O1 V1 C1 31.35(5) . . ?
O1 V1 C16 132.68(5) . . ?
O1 V1 C31 92.27(5) . . ?
O2 V1 O1 157.90(5) . . ?
O2 V1 O3 107.91(5) . . ?
O2 V1 N1 97.38(5) . . ?
O2 V1 N2 65.90(5) . . ?
O2 V1 N3 100.70(5) . . ?
O2 V1 C1 130.03(5) . . ?
O2 V1 C16 32.63(5) . . ?
O2 V1 C31 108.92(5) . . ?
O3 V1 O1 93.25(5) . . ?
O3 V1 N1 151.26(5) . . ?
O3 V1 N2 107.27(5) . . ?
O3 V1 N3 66.24(5) . . ?
O3 V1 C1 121.45(5) . . ?
O3 V1 C16 111.96(5) . . ?
O3 V1 C31 32.73(5) . . ?
N1 V1 C1 32.94(5) . . ?
N1 V1 C16 96.68(5) . . ?
N1 V1 C31 125.56(5) . . ?
N2 V1 N1 95.25(5) . . ?
N2 V1 C1 103.53(5) . . ?
N2 V1 C16 33.29(5) . . ?
N2 V1 C31 138.81(5) . . ?
N3 V1 N1 96.29(5) . . ?
N3 V1 N2 163.38(5) . . ?
N3 V1 C1 92.63(5) . . ?
N3 V1 C16 132.84(5) . . ?
N3 V1 C31 33.59(5) . . ?
C16 V1 C1 120.88(5) . . ?
C31 V1 C1 108.45(5) . . ?
C31 V1 C16 130.47(5) . . ?
C1 O1 V1 95.35(9) . . ?
C16 O2 V1 95.02(9) . . ?
C31 O3 V1 94.50(9) . . ?
C1 N1 V1 87.53(9) . . ?
C5 N1 V1 149.85(11) . . ?
C5 N1 C1 120.74(13) . . ?
C16 N2 V1 87.16(9) . . ?
C20 N2 V1 151.16(11) . . ?
C20 N2 C16 121.35(13) . . ?
C31 N3 V1 87.68(9) . . ?
C35 N3 V1 150.06(12) . . ?
C35 N3 C31 121.96(14) . . ?
O1 C1 V1 53.30(7) . . ?
O1 C1 N1 112.20(13) . . ?
O1 C1 C2 125.24(14) . . ?
N1 C1 V1 59.53(8) . . ?
N1 C1 C2 122.52(14) . . ?
C2 C1 V1 170.42(12) . . ?
C1 C2 C7 120.51(14) . . ?
C3 C2 C1 116.11(15) . . ?
C3 C2 C7 123.20(14) . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.33(15) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 H4 120.1 . . ?
C5 C4 C3 119.80(16) . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C4 119.49(15) . . ?
N1 C5 C6 117.36(14) . . ?
C4 C5 C6 123.14(15) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C2 121.10(15) . . ?
C8 C7 C12 120.01(15) . . ?
C12 C7 C2 118.88(14) . . ?
C7 C8 C13 121.18(15) . . ?
C9 C8 C7 118.70(16) . . ?
C9 C8 C13 120.10(16) . . ?
C8 C9 H9 119.0 . . ?
C10 C9 C8 121.95(16) . . ?
C10 C9 H9 119.0 . . ?
C9 C10 C11 118.16(16) . . ?
C9 C10 C14 121.77(17) . . ?
C11 C10 C14 120.06(17) . . ?
C10 C11 H11 119.1 . . ?
C10 C11 C12 121.80(16) . . ?
C12 C11 H11 119.1 . . ?
C7 C12 C15 120.54(15) . . ?
C11 C12 C7 118.97(15) . . ?
C11 C12 C15 120.49(15) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O2 C16 V1 52.35(7) . . ?
O2 C16 N2 111.86(13) . . ?
O2 C16 C17 125.27(14) . . ?
N2 C16 V1 59.55(8) . . ?
N2 C16 C17 122.86(14) . . ?
C17 C16 V1 176.10(12) . . ?
C16 C17 C22 120.76(13) . . ?
C18 C17 C16 115.65(14) . . ?
C18 C17 C22 123.56(14) . . ?
C17 C18 H18 119.3 . . ?
C17 C18 C19 121.32(14) . . ?
C19 C18 H18 119.3 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 119.99(14) . . ?
C20 C19 H19 120.0 . . ?
N2 C20 C19 118.79(14) . . ?
N2 C20 C21 117.24(14) . . ?
C19 C20 C21 123.96(14) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C17 120.95(14) . . ?
C23 C22 C27 119.79(14) . . ?
C27 C22 C17 119.26(14) . . ?
C22 C23 C28 120.91(14) . . ?
C24 C23 C22 119.00(15) . . ?
C24 C23 C28 120.06(15) . . ?
C23 C24 H24 118.9 . . ?
C25 C24 C23 122.13(17) . . ?
C25 C24 H24 118.9 . . ?
C24 C25 C26 117.96(16) . . ?
C24 C25 C29 121.14(18) . . ?
C26 C25 C29 120.90(18) . . ?
C25 C26 H26 119.0 . . ?
C25 C26 C27 122.01(16) . . ?
C27 C26 H26 119.0 . . ?
C22 C27 C30 121.24(15) . . ?
C26 C27 C22 119.03(16) . . ?
C26 C27 C30 119.72(15) . . ?
C23 C28 H28A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
C23 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C29 H29A 113.7(17) . . ?
C25 C29 H29B 108.9(16) . . ?
C25 C29 H29C 111.6(16) . . ?
H29A C29 H29B 104(2) . . ?
H29A C29 H29C 111(2) . . ?
H29B C29 H29C 108(2) . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O3 C31 V1 52.77(7) . . ?
O3 C31 N3 111.31(14) . . ?
O3 C31 C32 126.65(14) . . ?
N3 C31 V1 58.72(8) . . ?
N3 C31 C32 122.03(14) . . ?
C32 C31 V1 175.04(11) . . ?
C31 C32 C37 121.80(14) . . ?
C33 C32 C31 115.33(15) . . ?
C33 C32 C37 122.79(15) . . ?
C32 C33 H33 118.9 . . ?
C32 C33 C34 122.22(16) . . ?
C34 C33 H33 118.9 . . ?
C33 C34 H34 120.3 . . ?
C35 C34 C33 119.49(15) . . ?
C35 C34 H34 120.3 . . ?
N3 C35 C34 118.93(15) . . ?
N3 C35 C36 117.41(15) . . ?
C34 C35 C36 123.65(14) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 C32 120.85(14) . . ?
C42 C37 C32 119.59(14) . . ?
C42 C37 C38 119.56(16) . . ?
C37 C38 C43 120.89(16) . . ?
C39 C38 C37 119.16(16) . . ?
C39 C38 C43 119.95(16) . . ?
C38 C39 H39 119.0 . . ?
C40 C39 C38 121.99(17) . . ?
C40 C39 H39 119.0 . . ?
C39 C40 C44 121.20(19) . . ?
C41 C40 C39 118.03(17) . . ?
C41 C40 C44 120.75(19) . . ?
C40 C41 H41 119.0 . . ?
C40 C41 C42 122.05(18) . . ?
C42 C41 H41 119.0 . . ?
C37 C42 C45 121.99(16) . . ?
C41 C42 C37 119.22(16) . . ?
C41 C42 C45 118.79(16) . . ?
C38 C43 H43A 109.5 . . ?
C38 C43 H43B 109.5 . . ?
C38 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C40 C44 H44A 109.5 . . ?
C40 C44 H44B 109.5 . . ?
C40 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
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 . . ?
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
V1 O1 2.0081(11) . ?
V1 O2 1.9536(11) . ?
V1 O3 1.9550(12) . ?
V1 N1 2.1512(14) . ?
V1 N2 2.1215(13) . ?
V1 N3 2.0936(13) . ?
V1 C1 2.4935(16) . ?
V1 C16 2.4579(15) . ?
V1 C31 2.4476(16) . ?
O1 C1 1.3029(19) . ?
O2 C16 1.3304(18) . ?
O3 C31 1.3275(18) . ?
N1 C1 1.357(2) . ?
N1 C5 1.351(2) . ?
N2 C16 1.3508(19) . ?
N2 C20 1.346(2) . ?
N3 C31 1.355(2) . ?
N3 C35 1.3490(19) . ?
C1 C2 1.406(2) . ?
C2 C3 1.378(2) . ?
C2 C7 1.492(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.400(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.382(2) . ?
C5 C6 1.500(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.402(2) . ?
C7 C12 1.404(2) . ?
C8 C9 1.401(2) . ?
C8 C13 1.507(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.383(3) . ?
C10 C11 1.391(2) . ?
C10 C14 1.510(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.393(2) . ?
C12 C15 1.510(2) . ?
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 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.399(2) . ?
C17 C18 1.389(2) . ?
C17 C22 1.490(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.393(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.391(2) . ?
C20 C21 1.495(2) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.402(2) . ?
C22 C27 1.405(2) . ?
C23 C24 1.394(2) . ?
C23 C28 1.509(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.387(3) . ?
C25 C26 1.387(3) . ?
C25 C29 1.506(3) . ?
C26 H26 0.9500 . ?
C26 C27 1.394(2) . ?
C27 C30 1.505(2) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.91(3) . ?
C29 H29B 0.99(3) . ?
C29 H29C 0.96(3) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.402(2) . ?
C32 C33 1.391(2) . ?
C32 C37 1.487(2) . ?
C33 H33 0.9500 . ?
C33 C34 1.392(2) . ?
C34 H34 0.9500 . ?
C34 C35 1.380(2) . ?
C35 C36 1.493(2) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.406(2) . ?
C37 C42 1.404(2) . ?
C38 C39 1.393(3) . ?
C38 C43 1.507(3) . ?
C39 H39 0.9500 . ?
C39 C40 1.388(3) . ?
C40 C41 1.385(3) . ?
C40 C44 1.513(3) . ?
C41 H41 0.9500 . ?
C41 C42 1.393(3) . ?
C42 C45 1.511(3) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
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
V1 O1 C1 N1 9.22(13) . . . . ?
V1 O1 C1 C2 -168.29(14) . . . . ?
V1 O2 C16 N2 -2.45(13) . . . . ?
V1 O2 C16 C17 176.17(14) . . . . ?
V1 O3 C31 N3 -4.95(13) . . . . ?
V1 O3 C31 C32 173.84(14) . . . . ?
V1 N1 C1 O1 -8.57(12) . . . . ?
V1 N1 C1 C2 169.02(14) . . . . ?
V1 N1 C5 C4 -157.50(17) . . . . ?
V1 N1 C5 C6 23.5(3) . . . . ?
V1 N2 C16 O2 2.25(12) . . . . ?
V1 N2 C16 C17 -176.40(14) . . . . ?
V1 N2 C20 C19 169.94(16) . . . . ?
V1 N2 C20 C21 -9.5(3) . . . . ?
V1 N3 C31 O3 4.61(12) . . . . ?
V1 N3 C31 C32 -174.24(13) . . . . ?
V1 N3 C35 C34 171.43(16) . . . . ?
V1 N3 C35 C36 -8.0(3) . . . . ?
O1 C1 C2 C3 176.66(15) . . . . ?
O1 C1 C2 C7 1.4(2) . . . . ?
O2 C16 C17 C18 -176.37(14) . . . . ?
O2 C16 C17 C22 5.6(2) . . . . ?
O3 C31 C32 C33 179.60(14) . . . . ?
O3 C31 C32 C37 -3.5(2) . . . . ?
N1 C1 C2 C3 -0.6(2) . . . . ?
N1 C1 C2 C7 -175.85(14) . . . . ?
N2 C16 C17 C18 2.1(2) . . . . ?
N2 C16 C17 C22 -175.92(14) . . . . ?
N3 C31 C32 C33 -1.7(2) . . . . ?
N3 C31 C32 C37 175.17(14) . . . . ?
C1 N1 C5 C4 0.0(2) . . . . ?
C1 N1 C5 C6 -178.94(15) . . . . ?
C1 C2 C3 C4 1.0(2) . . . . ?
C1 C2 C7 C8 -97.11(19) . . . . ?
C1 C2 C7 C12 82.41(19) . . . . ?
C2 C3 C4 C5 -0.9(3) . . . . ?
C2 C7 C8 C9 -174.27(14) . . . . ?
C2 C7 C8 C13 7.6(2) . . . . ?
C2 C7 C12 C11 174.41(14) . . . . ?
C2 C7 C12 C15 -6.4(2) . . . . ?
C3 C2 C7 C8 88.0(2) . . . . ?
C3 C2 C7 C12 -92.5(2) . . . . ?
C3 C4 C5 N1 0.4(3) . . . . ?
C3 C4 C5 C6 179.28(16) . . . . ?
C5 N1 C1 V1 -168.92(16) . . . . ?
C5 N1 C1 O1 -177.49(14) . . . . ?
C5 N1 C1 C2 0.1(2) . . . . ?
C7 C2 C3 C4 176.11(16) . . . . ?
C7 C8 C9 C10 -1.1(2) . . . . ?
C8 C7 C12 C11 -6.1(2) . . . . ?
C8 C7 C12 C15 173.16(15) . . . . ?
C8 C9 C10 C11 -4.0(2) . . . . ?
C8 C9 C10 C14 176.09(16) . . . . ?
C9 C10 C11 C12 4.1(2) . . . . ?
C10 C11 C12 C7 0.8(2) . . . . ?
C10 C11 C12 C15 -178.40(16) . . . . ?
C12 C7 C8 C9 6.2(2) . . . . ?
C12 C7 C8 C13 -171.95(15) . . . . ?
C13 C8 C9 C10 177.04(16) . . . . ?
C14 C10 C11 C12 -175.92(16) . . . . ?
C16 N2 C20 C19 -0.5(2) . . . . ?
C16 N2 C20 C21 -179.95(14) . . . . ?
C16 C17 C18 C19 -1.8(2) . . . . ?
C16 C17 C22 C23 -109.42(17) . . . . ?
C16 C17 C22 C27 70.69(19) . . . . ?
C17 C18 C19 C20 0.4(3) . . . . ?
C17 C22 C23 C24 -177.18(14) . . . . ?
C17 C22 C23 C28 4.8(2) . . . . ?
C17 C22 C27 C26 177.27(14) . . . . ?
C17 C22 C27 C30 -2.4(2) . . . . ?
C18 C17 C22 C23 72.7(2) . . . . ?
C18 C17 C22 C27 -107.18(18) . . . . ?
C18 C19 C20 N2 0.8(2) . . . . ?
C18 C19 C20 C21 -179.81(16) . . . . ?
C20 N2 C16 V1 175.40(16) . . . . ?
C20 N2 C16 O2 177.65(13) . . . . ?
C20 N2 C16 C17 -1.0(2) . . . . ?
C22 C17 C18 C19 176.18(15) . . . . ?
C22 C23 C24 C25 -0.6(2) . . . . ?
C23 C22 C27 C26 -2.6(2) . . . . ?
C23 C22 C27 C30 177.72(14) . . . . ?
C23 C24 C25 C26 -1.5(3) . . . . ?
C23 C24 C25 C29 177.64(18) . . . . ?
C24 C25 C26 C27 1.6(3) . . . . ?
C25 C26 C27 C22 0.4(2) . . . . ?
C25 C26 C27 C30 -179.90(15) . . . . ?
C27 C22 C23 C24 2.7(2) . . . . ?
C27 C22 C23 C28 -175.33(14) . . . . ?
C28 C23 C24 C25 177.43(16) . . . . ?
C29 C25 C26 C27 -177.56(18) . . . . ?
C31 N3 C35 C34 0.3(2) . . . . ?
C31 N3 C35 C36 -179.16(14) . . . . ?
C31 C32 C33 C34 0.6(2) . . . . ?
C31 C32 C37 C38 66.1(2) . . . . ?
C31 C32 C37 C42 -113.88(17) . . . . ?
C32 C33 C34 C35 0.9(3) . . . . ?
C32 C37 C38 C39 179.78(15) . . . . ?
C32 C37 C38 C43 0.6(2) . . . . ?
C32 C37 C42 C41 -179.84(15) . . . . ?
C32 C37 C42 C45 0.5(2) . . . . ?
C33 C32 C37 C38 -117.19(18) . . . . ?
C33 C32 C37 C42 62.8(2) . . . . ?
C33 C34 C35 N3 -1.4(2) . . . . ?
C33 C34 C35 C36 178.02(15) . . . . ?
C35 N3 C31 V1 175.60(16) . . . . ?
C35 N3 C31 O3 -179.79(13) . . . . ?
C35 N3 C31 C32 1.4(2) . . . . ?
C37 C32 C33 C34 -176.27(15) . . . . ?
C37 C38 C39 C40 0.1(3) . . . . ?
C38 C37 C42 C41 0.1(2) . . . . ?
C38 C37 C42 C45 -179.54(16) . . . . ?
C38 C39 C40 C41 0.2(3) . . . . ?
C38 C39 C40 C44 -178.38(17) . . . . ?
C39 C40 C41 C42 -0.2(3) . . . . ?
C40 C41 C42 C37 0.1(3) . . . . ?
C40 C41 C42 C45 179.77(18) . . . . ?
C42 C37 C38 C39 -0.2(2) . . . . ?
C42 C37 C38 C43 -179.40(16) . . . . ?
C43 C38 C39 C40 179.26(17) . . . . ?
C44 C40 C41 C42 178.32(18) . . . . ?
