#------------------------------------------------------------------------------
#$Date: 2026-03-04 12:19:07 +0100 (Wed 04 de Mar de 2026) $
#$Revision: 304754 $
#$URL: svn://www.crystallography.net/cod/cif/7/72/04/7720469.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_7720469
loop_
_publ_author_name
'Gong, Yi'
'Shibata, Kaname'
'Michiue, Kenji'
'Gbertyo, Joseph'
'Rais, Zaid'
'Elsegood, Mark R. J.'
'Prior, Timothy J.'
'Redshaw, Carl'
_publ_section_title
;
 Phenoxybis(imine) complexes of vanadium: structure, ethylene
 polymerization, and ring opening polymerization of ε-caprolactone.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1866
_journal_page_last               1881
_journal_paper_doi               10.1039/d5dt02846a
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C66 H82 N4 O3 V'
_chemical_formula_sum            'C66 H82 N4 O3 V'
_chemical_formula_weight         1030.29
_chemical_properties_physical    Air-sensitive,Moisture-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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-01-20 deposited with the CCDC.	2025-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.6408(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2637(5)
_cell_length_b                   32.1121(19)
_cell_length_c                   10.5093(6)
_cell_measurement_reflns_used    7618
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      2.36
_cell_volume                     3024.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21757
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.101
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2004/1, Sheldrick, G.M., (2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1106
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.580
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         5329
_refine_ls_number_restraints     891
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.1135
_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)+(0.0422P)²+7.7250P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2462
_refine_ls_wR_factor_ref         0.2562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4315
_reflns_number_total             5329
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt02846a2.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7720469
_shelx_shelxl_version_number     2019/3
_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_min   0.884
_shelx_estimated_absorpt_t_max   0.963
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 0.05198(17) 0.50559(5) 0.52305(15) 0.0406(4) Uani 0.5 1 d . . P . .
O2 O 0.2077(7) 0.5235(2) 0.6004(6) 0.0495(16) Uani 0.5 1 d . . P . .
O1 O 0.0059(4) 0.53381(9) 0.3620(3) 0.0511(8) Uani 1 1 d . . . . .
C1 C 0.0665(5) 0.53075(15) 0.2601(4) 0.0453(11) Uani 1 1 d . . . . .
C2 C 0.1357(5) 0.49418(15) 0.2337(4) 0.0462(11) Uani 1 1 d . . . . .
C3 C 0.1963(6) 0.49187(18) 0.1233(5) 0.0600(14) Uani 1 1 d . . . . .
H3 H 0.238589 0.466399 0.104211 0.072 Uiso 1 1 calc R U . . .
C4 C 0.1954(6) 0.5257(2) 0.0432(5) 0.0618(14) Uani 1 1 d . . . . .
C5 C 0.1269(6) 0.56109(19) 0.0701(5) 0.0603(14) Uani 1 1 d . . . . .
H5 H 0.123567 0.584372 0.013671 0.072 Uiso 1 1 calc R U . . .
C6 C 0.0619(5) 0.56512(16) 0.1753(5) 0.0520(12) Uani 1 1 d . . . . .
C7 C 0.1489(6) 0.45771(15) 0.3147(5) 0.0508(12) Uani 1 1 d . . . . .
H7 H 0.194638 0.434253 0.286053 0.061 Uiso 1 1 calc R U . . .
N1 N 0.1067(5) 0.45278(11) 0.4213(4) 0.0492(10) Uani 1 1 d . . . . .
C8 C 0.2676(7) 0.5236(2) -0.0717(5) 0.084(2) Uani 1 1 d . . . . .
H8A H 0.373477 0.516624 -0.038968 0.126 Uiso 1 1 calc R U . . .
H8B H 0.257775 0.550650 -0.116139 0.126 Uiso 1 1 calc R U . . .
H8C H 0.217898 0.502160 -0.133878 0.126 Uiso 1 1 calc R U . . .
C9 C 0.1428(6) 0.41240(14) 0.4825(5) 0.0513(10) Uani 1 1 d . U . . .
C10 C 0.0440(7) 0.37999(16) 0.4438(6) 0.0674(13) Uani 1 1 d . U . . .
C11 C 0.0886(9) 0.34070(18) 0.5017(8) 0.0913(19) Uani 1 1 d . U . . .
H11 H 0.023585 0.317542 0.477645 0.110 Uiso 1 1 calc R U . . .
C12 C 0.2209(10) 0.3353(2) 0.5900(8) 0.102(2) Uani 1 1 d . U . . .
H12 H 0.248208 0.308637 0.627349 0.122 Uiso 1 1 calc R U . . .
C13 C 0.3142(8) 0.3678(2) 0.6250(7) 0.0901(18) Uani 1 1 d . U . . .
H13 H 0.407197 0.363502 0.687025 0.108 Uiso 1 1 calc R U . . .
C14 C 0.2794(7) 0.40758(18) 0.5736(6) 0.0660(12) Uani 1 1 d . U . . .
C15 C -0.1035(7) 0.3846(2) 0.3438(7) 0.0829(16) Uani 1 1 d D U . . .
H15 H -0.119656 0.414548 0.317844 0.099 Uiso 0.753(18) 1 calc R U P A 1
H15X H -0.072035 0.409987 0.302619 0.099 Uiso 0.247(18) 1 calc R U P A 2
C16 C -0.1206(11) 0.3583(2) 0.2222(7) 0.116(3) Uani 1 1 d D U . . .
H16A H -0.030768 0.360828 0.189647 0.174 Uiso 1 1 calc R U . . .
H16B H -0.207486 0.367829 0.154298 0.174 Uiso 1 1 calc R U . . .
H16C H -0.134680 0.329118 0.243609 0.174 Uiso 1 1 calc R U . . .
C17 C -0.2298(11) 0.3699(6) 0.4072(11) 0.119(5) Uani 0.753(18) 1 d D U P A 1
H17A H -0.224984 0.385920 0.487516 0.143 Uiso 0.753(18) 1 calc R U P A 1
H17B H -0.326989 0.374276 0.344978 0.143 Uiso 0.753(18) 1 calc R U P A 1
H17C H -0.216790 0.340227 0.428954 0.143 Uiso 0.753(18) 1 calc R U P A 1
C17X C -0.233(2) 0.4058(11) 0.378(3) 0.082(8) Uani 0.247(18) 1 d D U P A 2
H17D H -0.197341 0.421231 0.460061 0.098 Uiso 0.247(18) 1 calc R U P A 2
H17E H -0.278874 0.425189 0.306961 0.098 Uiso 0.247(18) 1 calc R U P A 2
H17F H -0.305965 0.384949 0.387738 0.098 Uiso 0.247(18) 1 calc R U P A 2
C18 C 0.3882(8) 0.4429(2) 0.6117(7) 0.0914(18) Uani 1 1 d D U . . .
H18 H 0.335263 0.469380 0.578563 0.110 Uiso 1 1 calc R U . . .
C19 C 0.4466(10) 0.4463(3) 0.7605(8) 0.134(3) Uani 1 1 d D U . . .
H19A H 0.362615 0.450015 0.800369 0.201 Uiso 1 1 calc R U . . .
H19B H 0.513893 0.470264 0.781970 0.201 Uiso 1 1 calc R U . . .
H19C H 0.500899 0.420827 0.794779 0.201 Uiso 1 1 calc R U . . .
C20 C 0.5194(10) 0.4380(4) 0.5495(10) 0.154(4) Uani 1 1 d D U . . .
H20A H 0.572967 0.412139 0.580936 0.231 Uiso 1 1 calc R U . . .
H20B H 0.587172 0.461708 0.574049 0.231 Uiso 1 1 calc R U . . .
H20C H 0.482185 0.436892 0.453594 0.231 Uiso 1 1 calc R U . . .
C21 C -0.0089(7) 0.60418(17) 0.1925(6) 0.0684(16) Uani 1 1 d . . . . .
H21 H -0.051516 0.607712 0.265114 0.082 Uiso 1 1 calc R U . . .
N2 N -0.0143(7) 0.63365(17) 0.1114(6) 0.0909(16) Uani 1 1 d D U . . .
C22 C -0.0998(14) 0.6706(3) 0.1121(15) 0.093(3) Uani 0.658(8) 1 d D U P B 1
C23 C -0.2458(17) 0.6757(4) 0.0310(17) 0.114(3) Uani 0.658(8) 1 d D U P B 1
C24 C -0.3177(17) 0.7130(4) 0.0388(17) 0.130(4) Uani 0.658(8) 1 d D U P B 1
H24 H -0.418864 0.716467 -0.008385 0.156 Uiso 0.658(8) 1 calc R U P B 1
C25 C -0.2411(19) 0.7459(4) 0.1169(18) 0.128(4) Uani 0.658(8) 1 d D U P B 1
H25 H -0.289240 0.771876 0.119647 0.153 Uiso 0.658(8) 1 calc R U P B 1
C26 C -0.1010(19) 0.7402(4) 0.1863(17) 0.114(3) Uani 0.658(8) 1 d D U P B 1
H26 H -0.049840 0.762512 0.237969 0.137 Uiso 0.658(8) 1 calc R U P B 1
C27 C -0.0280(17) 0.7027(3) 0.1854(13) 0.097(3) Uani 0.658(8) 1 d D U P B 1
C28 C -0.310(2) 0.6393(5) -0.066(2) 0.138(4) Uani 0.658(8) 1 d D U P B 1
H28 H -0.229580 0.617853 -0.055461 0.166 Uiso 0.658(8) 1 calc R U P B 1
C29 C -0.435(2) 0.6196(7) -0.0249(18) 0.198(7) Uani 0.658(8) 1 d D U P B 1
H29A H -0.402950 0.612155 0.068413 0.297 Uiso 0.658(8) 1 calc R U P B 1
H29B H -0.518853 0.639141 -0.038761 0.297 Uiso 0.658(8) 1 calc R U P B 1
H29C H -0.466453 0.594429 -0.077348 0.297 Uiso 0.658(8) 1 calc R U P B 1
C30 C -0.354(2) 0.6508(5) -0.2045(17) 0.148(5) Uani 0.658(8) 1 d D U P B 1
H30A H -0.268939 0.663801 -0.229061 0.221 Uiso 0.658(8) 1 calc R U P B 1
H30B H -0.384619 0.625853 -0.258057 0.221 Uiso 0.658(8) 1 calc R U P B 1
H30C H -0.437019 0.670565 -0.219471 0.221 Uiso 0.658(8) 1 calc R U P B 1
C31 C 0.1310(18) 0.6988(4) 0.2676(13) 0.107(3) Uani 0.658(8) 1 d D U P B 1
H31 H 0.139141 0.671190 0.312884 0.128 Uiso 0.658(8) 1 calc R U P B 1
C32 C 0.189(2) 0.7312(4) 0.3731(13) 0.136(5) Uani 0.658(8) 1 d D U P B 1
H32A H 0.292990 0.724780 0.418178 0.204 Uiso 0.658(8) 1 calc R U P B 1
H32B H 0.184141 0.758802 0.332578 0.204 Uiso 0.658(8) 1 calc R U P B 1
H32C H 0.128137 0.730896 0.436875 0.204 Uiso 0.658(8) 1 calc R U P B 1
C33 C 0.2395(19) 0.6977(9) 0.1765(19) 0.143(6) Uani 0.658(8) 1 d D U P B 1
H33A H 0.342380 0.695176 0.230101 0.215 Uiso 0.658(8) 1 calc R U P B 1
H33B H 0.215540 0.673757 0.116972 0.215 Uiso 0.658(8) 1 calc R U P B 1
H33C H 0.229124 0.723423 0.124812 0.215 Uiso 0.658(8) 1 calc R U P B 1
C22X C -0.052(2) 0.6746(6) 0.156(3) 0.100(4) Uani 0.342(8) 1 d D U P B 2
C23X C -0.204(3) 0.6879(6) 0.100(3) 0.114(4) Uani 0.342(8) 1 d D U P B 2
C24X C -0.240(3) 0.7286(7) 0.127(4) 0.124(4) Uani 0.342(8) 1 d D U P B 2
H24X H -0.334037 0.740001 0.083144 0.149 Uiso 0.342(8) 1 calc R U P B 2
C25X C -0.136(3) 0.7528(7) 0.218(3) 0.123(5) Uani 0.342(8) 1 d D U P B 2
H25X H -0.169107 0.777961 0.249141 0.148 Uiso 0.342(8) 1 calc R U P B 2
C26X C 0.007(3) 0.7416(6) 0.264(3) 0.117(4) Uani 0.342(8) 1 d D U P B 2
H26X H 0.078591 0.759830 0.316291 0.140 Uiso 0.342(8) 1 calc R U P B 2
C27X C 0.047(3) 0.7016(6) 0.230(3) 0.103(4) Uani 0.342(8) 1 d D U P B 2
C28X C -0.308(2) 0.6567(9) 0.009(3) 0.123(5) Uani 0.342(8) 1 d D U P B 2
H28X H -0.286176 0.629182 0.054995 0.148 Uiso 0.342(8) 1 calc R U P B 2
C29X C -0.471(2) 0.6632(10) -0.010(3) 0.152(7) Uani 0.342(8) 1 d D U P B 2
H29D H -0.492733 0.666813 0.076166 0.227 Uiso 0.342(8) 1 calc R U P B 2
H29E H -0.501768 0.688177 -0.063208 0.227 Uiso 0.342(8) 1 calc R U P B 2
H29F H -0.525059 0.638982 -0.054310 0.227 Uiso 0.342(8) 1 calc R U P B 2
C30X C -0.269(4) 0.6511(12) -0.117(3) 0.144(8) Uani 0.342(8) 1 d D U P B 2
H30D H -0.160928 0.646862 -0.101386 0.215 Uiso 0.342(8) 1 calc R U P B 2
H30E H -0.321486 0.626752 -0.162890 0.215 Uiso 0.342(8) 1 calc R U P B 2
H30F H -0.298195 0.675947 -0.171788 0.215 Uiso 0.342(8) 1 calc R U P B 2
C31X C 0.212(3) 0.6904(7) 0.284(2) 0.111(5) Uani 0.342(8) 1 d D U P B 2
H31X H 0.212615 0.660484 0.310390 0.133 Uiso 0.342(8) 1 calc R U P B 2
C32X C 0.304(3) 0.7130(9) 0.404(3) 0.144(8) Uani 0.342(8) 1 d D U P B 2
H32D H 0.406246 0.702218 0.425561 0.217 Uiso 0.342(8) 1 calc R U P B 2
H32E H 0.305250 0.742890 0.385045 0.217 Uiso 0.342(8) 1 calc R U P B 2
H32F H 0.260257 0.708565 0.478535 0.217 Uiso 0.342(8) 1 calc R U P B 2
C33X C 0.292(4) 0.6920(17) 0.172(3) 0.139(8) Uani 0.342(8) 1 d D U P B 2
H33D H 0.232043 0.677350 0.095229 0.208 Uiso 0.342(8) 1 calc R U P B 2
H33E H 0.305467 0.721044 0.149556 0.208 Uiso 0.342(8) 1 calc R U P B 2
H33F H 0.389739 0.678487 0.201696 0.208 Uiso 0.342(8) 1 calc R U P B 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'
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
V1 V1 O2 176.8(3) 3_566 . ?
V1 V1 O1 76.7(2) 3_566 . ?
O2 V1 O1 105.0(3) . . ?
V1 V1 O1 71.9(2) 3_566 3_566 ?
O2 V1 O1 106.4(3) . 3_566 ?
O1 V1 O1 148.57(10) . 3_566 ?
V1 V1 N1 78.4(2) 3_566 . ?
O2 V1 N1 104.3(3) . . ?
O1 V1 N1 87.73(15) . . ?
O1 V1 N1 86.04(15) 3_566 . ?
V1 V1 N1 74.0(2) 3_566 3_566 ?
O2 V1 N1 103.3(3) . 3_566 ?
O1 V1 N1 86.00(15) . 3_566 ?
O1 V1 N1 85.44(15) 3_566 3_566 ?
N1 V1 N1 152.42(9) . 3_566 ?
C1 O1 V1 130.2(3) . . ?
C1 O1 V1 134.4(3) . 3_566 ?
O1 C1 C2 121.9(4) . . ?
O1 C1 C6 119.8(4) . . ?
C2 C1 C6 118.3(4) . . ?
C1 C2 C3 120.3(5) . . ?
C1 C2 C7 122.8(4) . . ?
C3 C2 C7 116.9(4) . . ?
C4 C3 C2 121.4(5) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 117.5(5) . . ?
C5 C4 C8 121.4(5) . . ?
C3 C4 C8 121.1(6) . . ?
C4 C5 C6 123.9(5) . . ?
C4 C5 H5 118.0 . . ?
C6 C5 H5 118.0 . . ?
C5 C6 C1 118.6(5) . . ?
C5 C6 C21 118.7(5) . . ?
C1 C6 C21 122.7(4) . . ?
N1 C7 C2 128.2(4) . . ?
N1 C7 H7 115.9 . . ?
C2 C7 H7 115.9 . . ?
C7 N1 C9 114.2(4) . . ?
C7 N1 V1 120.1(3) . . ?
C9 N1 V1 123.2(3) . . ?
C7 N1 V1 122.2(3) . 3_566 ?
C9 N1 V1 121.9(3) . 3_566 ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C14 122.7(5) . . ?
C10 C9 N1 118.9(5) . . ?
C14 C9 N1 118.3(5) . . ?
C9 C10 C11 116.5(6) . . ?
C9 C10 C15 123.3(5) . . ?
C11 C10 C15 120.1(6) . . ?
C12 C11 C10 121.7(7) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C13 C12 C11 119.9(7) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 122.4(7) . . ?
C12 C13 H13 118.8 . . ?
C14 C13 H13 118.8 . . ?
C9 C14 C13 116.8(6) . . ?
C9 C14 C18 122.2(5) . . ?
C13 C14 C18 120.9(6) . . ?
C17X C15 C16 122.6(12) . . ?
C17X C15 C10 121.2(11) . . ?
C16 C15 C10 114.8(6) . . ?
C16 C15 C17 105.3(8) . . ?
C10 C15 C17 108.6(7) . . ?
C16 C15 H15 109.4 . . ?
C10 C15 H15 109.4 . . ?
C17 C15 H15 109.4 . . ?
C17X C15 H15X 94.0 . . ?
C16 C15 H15X 94.0 . . ?
C10 C15 H15X 94.0 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C17X H17D 109.5 . . ?
C15 C17X H17E 109.5 . . ?
H17D C17X H17E 109.5 . . ?
C15 C17X H17F 109.5 . . ?
H17D C17X H17F 109.5 . . ?
H17E C17X H17F 109.5 . . ?
C14 C18 C19 111.6(7) . . ?
C14 C18 C20 111.1(6) . . ?
C19 C18 C20 109.4(7) . . ?
C14 C18 H18 108.2 . . ?
C19 C18 H18 108.2 . . ?
C20 C18 H18 108.2 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 C6 120.4(6) . . ?
N2 C21 H21 119.8 . . ?
C6 C21 H21 119.8 . . ?
C21 N2 C22 123.1(8) . . ?
C21 N2 C22X 115.1(14) . . ?
C27 C22 C23 120.8(11) . . ?
C27 C22 N2 116.2(10) . . ?
C23 C22 N2 122.7(11) . . ?
C24 C23 C22 117.7(14) . . ?
C24 C23 C28 125.1(14) . . ?
C22 C23 C28 117.1(11) . . ?
C23 C24 C25 120.2(14) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C26 C25 C24 119.5(13) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C25 C26 C27 121.8(15) . . ?
C25 C26 H26 119.1 . . ?
C27 C26 H26 119.1 . . ?
C22 C27 C26 119.7(14) . . ?
C22 C27 C31 122.0(10) . . ?
C26 C27 C31 118.4(13) . . ?
C30 C28 C29 111.1(15) . . ?
C30 C28 C23 115.0(13) . . ?
C29 C28 C23 109.2(18) . . ?
C30 C28 H28 107.0 . . ?
C29 C28 H28 107.0 . . ?
C23 C28 H28 107.0 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C27 C31 C32 118.4(13) . . ?
C27 C31 C33 109.7(11) . . ?
C32 C31 C33 107.5(13) . . ?
C27 C31 H31 106.9 . . ?
C32 C31 H31 106.9 . . ?
C33 C31 H31 106.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C27X C22X C23X 119.3(16) . . ?
C27X C22X N2 125.0(16) . . ?
C23X C22X N2 115.1(15) . . ?
C24X C23X C22X 117(2) . . ?
C24X C23X C28X 126(2) . . ?
C22X C23X C28X 116.6(16) . . ?
C23X C24X C25X 120(2) . . ?
C23X C24X H24X 120.1 . . ?
C25X C24X H24X 120.1 . . ?
C26X C25X C24X 123(2) . . ?
C26X C25X H25X 118.7 . . ?
C24X C25X H25X 118.7 . . ?
C25X C26X C27X 117(2) . . ?
C25X C26X H26X 121.5 . . ?
C27X C26X H26X 121.5 . . ?
C22X C27X C26X 123(2) . . ?
C22X C27X C31X 122.0(16) . . ?
C26X C27X C31X 114.8(18) . . ?
C30X C28X C29X 112(2) . . ?
C30X C28X C23X 112(2) . . ?
C29X C28X C23X 116(2) . . ?
C30X C28X H28X 105.1 . . ?
C29X C28X H28X 105.1 . . ?
C23X C28X H28X 105.1 . . ?
C28X C29X H29D 109.5 . . ?
C28X C29X H29E 109.5 . . ?
H29D C29X H29E 109.5 . . ?
C28X C29X H29F 109.5 . . ?
H29D C29X H29F 109.5 . . ?
H29E C29X H29F 109.5 . . ?
C28X C30X H30D 109.5 . . ?
C28X C30X H30E 109.5 . . ?
H30D C30X H30E 109.5 . . ?
C28X C30X H30F 109.5 . . ?
H30D C30X H30F 109.5 . . ?
H30E C30X H30F 109.5 . . ?
C32X C31X C27X 120(2) . . ?
C32X C31X C33X 109.7(19) . . ?
C27X C31X C33X 109.7(18) . . ?
C32X C31X H31X 105.5 . . ?
C27X C31X H31X 105.5 . . ?
C33X C31X H31X 105.5 . . ?
C31X C32X H32D 109.5 . . ?
C31X C32X H32E 109.5 . . ?
H32D C32X H32E 109.5 . . ?
C31X C32X H32F 109.5 . . ?
H32D C32X H32F 109.5 . . ?
H32E C32X H32F 109.5 . . ?
C31X C33X H33D 109.5 . . ?
C31X C33X H33E 109.5 . . ?
H33D C33X H33E 109.5 . . ?
C31X C33X H33F 109.5 . . ?
H33D C33X H33F 109.5 . . ?
H33E C33X H33F 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 V1 1.027(3) 3_566 ?
V1 O2 1.575(7) . ?
V1 O1 1.872(3) . ?
V1 O1 1.917(3) 3_566 ?
V1 N1 2.133(4) . ?
V1 N1 2.173(4) 3_566 ?
O1 C1 1.332(5) . ?
C1 C2 1.399(6) . ?
C1 C6 1.412(6) . ?
C2 C3 1.413(6) . ?
C2 C7 1.435(7) . ?
C3 C4 1.372(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.367(8) . ?
C4 C8 1.522(7) . ?
C5 C6 1.393(7) . ?
C5 H5 0.9500 . ?
C6 C21 1.448(7) . ?
C7 N1 1.286(6) . ?
C7 H7 0.9500 . ?
N1 C9 1.448(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.378(7) . ?
C9 C14 1.389(7) . ?
C10 C11 1.416(8) . ?
C10 C15 1.506(9) . ?
C11 C12 1.349(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.346(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(8) . ?
C13 H13 0.9500 . ?
C14 C18 1.503(9) . ?
C15 C17X 1.494(17) . ?
C15 C16 1.506(9) . ?
C15 C17 1.559(11) . ?
C15 H15 1.0000 . ?
C15 H15X 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17X H17D 0.9800 . ?
C17X H17E 0.9800 . ?
C17X H17F 0.9800 . ?
C18 C19 1.523(9) . ?
C18 C20 1.527(10) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 N2 1.266(7) . ?
C21 H21 0.9500 . ?
N2 C22 1.428(11) . ?
N2 C22X 1.468(15) . ?
C22 C27 1.355(15) . ?
C22 C23 1.414(16) . ?
C23 C24 1.383(16) . ?
C23 C28 1.56(2) . ?
C24 C25 1.41(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.33(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.383(15) . ?
C26 H26 0.9500 . ?
C27 C31 1.513(16) . ?
C28 C30 1.46(2) . ?
C28 C29 1.474(19) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.516(13) . ?
C31 C33 1.555(14) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C22X C27X 1.356(19) . ?
C22X C23X 1.44(2) . ?
C23X C24X 1.39(2) . ?
C23X C28X 1.54(2) . ?
C24X C25X 1.41(3) . ?
C24X H24X 0.9500 . ?
C25X C26X 1.34(3) . ?
C25X H25X 0.9500 . ?
C26X C27X 1.404(19) . ?
C26X H26X 0.9500 . ?
C27X C31X 1.53(2) . ?
C28X C30X 1.48(3) . ?
C28X C29X 1.49(2) . ?
C28X H28X 1.0000 . ?
C29X H29D 0.9800 . ?
C29X H29E 0.9800 . ?
C29X H29F 0.9800 . ?
C30X H30D 0.9800 . ?
C30X H30E 0.9800 . ?
C30X H30F 0.9800 . ?
C31X C32X 1.516(16) . ?
C31X C33X 1.542(18) . ?
C31X H31X 1.0000 . ?
C32X H32D 0.9800 . ?
C32X H32E 0.9800 . ?
C32X H32F 0.9800 . ?
C33X H33D 0.9800 . ?
C33X H33E 0.9800 . ?
C33X H33F 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 V1 O1 C1 -112.0(4) 3_566 . . . ?
O2 V1 O1 C1 70.8(5) . . . . ?
O1 V1 O1 C1 -112.0(4) 3_566 . . . ?
N1 V1 O1 C1 -33.4(4) . . . . ?
N1 V1 O1 C1 173.5(4) 3_566 . . . ?
O2 V1 O1 V1 -177.2(3) . . . 3_566 ?
O1 V1 O1 V1 -0.002(1) 3_566 . . 3_566 ?
N1 V1 O1 V1 78.62(19) . . . 3_566 ?
N1 V1 O1 V1 -74.50(19) 3_566 . . 3_566 ?
V1 O1 C1 C2 26.8(7) . . . . ?
V1 O1 C1 C2 -15.8(7) 3_566 . . . ?
V1 O1 C1 C6 -153.2(4) . . . . ?
V1 O1 C1 C6 164.2(4) 3_566 . . . ?
O1 C1 C2 C3 178.9(4) . . . . ?
C6 C1 C2 C3 -1.2(7) . . . . ?
O1 C1 C2 C7 -1.1(7) . . . . ?
C6 C1 C2 C7 178.9(5) . . . . ?
C1 C2 C3 C4 3.1(8) . . . . ?
C7 C2 C3 C4 -177.0(5) . . . . ?
C2 C3 C4 C5 -3.2(8) . . . . ?
C2 C3 C4 C8 177.0(5) . . . . ?
C3 C4 C5 C6 1.6(8) . . . . ?
C8 C4 C5 C6 -178.6(5) . . . . ?
C4 C5 C6 C1 0.1(8) . . . . ?
C4 C5 C6 C21 -179.3(5) . . . . ?
O1 C1 C6 C5 179.6(4) . . . . ?
C2 C1 C6 C5 -0.3(7) . . . . ?
O1 C1 C6 C21 -1.0(8) . . . . ?
C2 C1 C6 C21 179.1(5) . . . . ?
C1 C2 C7 N1 -2.3(8) . . . . ?
C3 C2 C7 N1 177.8(5) . . . . ?
C2 C7 N1 C9 -177.4(5) . . . . ?
C2 C7 N1 V1 -14.9(7) . . . . ?
C2 C7 N1 V1 17.3(7) . . . 3_566 ?
C7 N1 C9 C10 -87.4(6) . . . . ?
V1 N1 C9 C10 110.7(5) . . . . ?
V1 N1 C9 C10 77.9(5) 3_566 . . . ?
C7 N1 C9 C14 89.7(6) . . . . ?
V1 N1 C9 C14 -72.1(5) . . . . ?
V1 N1 C9 C14 -104.9(5) 3_566 . . . ?
C14 C9 C10 C11 -0.3(8) . . . . ?
N1 C9 C10 C11 176.7(5) . . . . ?
C14 C9 C10 C15 -179.2(5) . . . . ?
N1 C9 C10 C15 -2.1(8) . . . . ?
C9 C10 C11 C12 0.0(10) . . . . ?
C15 C10 C11 C12 178.9(7) . . . . ?
C10 C11 C12 C13 0.0(12) . . . . ?
C11 C12 C13 C14 0.3(12) . . . . ?
C10 C9 C14 C13 0.5(8) . . . . ?
N1 C9 C14 C13 -176.5(5) . . . . ?
C10 C9 C14 C18 178.1(5) . . . . ?
N1 C9 C14 C18 1.0(7) . . . . ?
C12 C13 C14 C9 -0.5(10) . . . . ?
C12 C13 C14 C18 -178.1(7) . . . . ?
C9 C10 C15 C17X -74.8(19) . . . . ?
C11 C10 C15 C17X 106.3(19) . . . . ?
C9 C10 C15 C16 118.6(7) . . . . ?
C11 C10 C15 C16 -60.3(9) . . . . ?
C9 C10 C15 C17 -124.0(9) . . . . ?
C11 C10 C15 C17 57.2(10) . . . . ?
C9 C14 C18 C19 132.2(7) . . . . ?
C13 C14 C18 C19 -50.3(9) . . . . ?
C9 C14 C18 C20 -105.3(8) . . . . ?
C13 C14 C18 C20 72.1(9) . . . . ?
C5 C6 C21 N2 1.7(9) . . . . ?
C1 C6 C21 N2 -177.7(6) . . . . ?
C6 C21 N2 C22 171.0(8) . . . . ?
C6 C21 N2 C22X -164.8(11) . . . . ?
C21 N2 C22 C27 91.1(14) . . . . ?
C21 N2 C22 C23 -95.4(15) . . . . ?
C27 C22 C23 C24 -6(2) . . . . ?
N2 C22 C23 C24 -179.4(13) . . . . ?
C27 C22 C23 C28 170.9(15) . . . . ?
N2 C22 C23 C28 -2(2) . . . . ?
C22 C23 C24 C25 6(2) . . . . ?
C28 C23 C24 C25 -171.3(16) . . . . ?
C23 C24 C25 C26 -2(3) . . . . ?
C24 C25 C26 C27 -1(3) . . . . ?
C23 C22 C27 C26 3(2) . . . . ?
N2 C22 C27 C26 177.1(13) . . . . ?
C23 C22 C27 C31 -176.8(14) . . . . ?
N2 C22 C27 C31 -3.2(19) . . . . ?
C25 C26 C27 C22 0(3) . . . . ?
C25 C26 C27 C31 -179.8(15) . . . . ?
C24 C23 C28 C30 55(3) . . . . ?
C22 C23 C28 C30 -121.4(17) . . . . ?
C24 C23 C28 C29 -70(2) . . . . ?
C22 C23 C28 C29 112.9(18) . . . . ?
C22 C27 C31 C32 -164.0(14) . . . . ?
C26 C27 C31 C32 15.8(18) . . . . ?
C22 C27 C31 C33 72.1(18) . . . . ?
C26 C27 C31 C33 -108.1(17) . . . . ?
C21 N2 C22X C27X 86(3) . . . . ?
C21 N2 C22X C23X -103(2) . . . . ?
C27X C22X C23X C24X 0(4) . . . . ?
N2 C22X C23X C24X -172(3) . . . . ?
C27X C22X C23X C28X 176(3) . . . . ?
N2 C22X C23X C28X 4(4) . . . . ?
C22X C23X C24X C25X -8(5) . . . . ?
C28X C23X C24X C25X 176(3) . . . . ?
C23X C24X C25X C26X 13(5) . . . . ?
C24X C25X C26X C27X -8(5) . . . . ?
C23X C22X C27X C26X 5(5) . . . . ?
N2 C22X C27X C26X 176(2) . . . . ?
C23X C22X C27X C31X -176(3) . . . . ?
N2 C22X C27X C31X -5(5) . . . . ?
C25X C26X C27X C22X -1(4) . . . . ?
C25X C26X C27X C31X 180(3) . . . . ?
C24X C23X C28X C30X 105(4) . . . . ?
C22X C23X C28X C30X -71(3) . . . . ?
C24X C23X C28X C29X -25(4) . . . . ?
C22X C23X C28X C29X 159(3) . . . . ?
C22X C27X C31X C32X -157(3) . . . . ?
C26X C27X C31X C32X 23(4) . . . . ?
C22X C27X C31X C33X 75(4) . . . . ?
C26X C27X C31X C33X -106(3) . . . . ?
