#------------------------------------------------------------------------------
#$Date: 2018-09-10 21:56:42 +0300 (Mon, 10 Sep 2018) $
#$Revision: 210787 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/27/7102791.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_7102791
loop_
_publ_author_name
'Tsai, Yi-Chou'
'Wang, Po-Yang'
'Lin, Kuan-Ming'
'Chen, Shin-An'
'Chen, Jin-Ming'
_publ_section_title
;
 Synthesis and reactions of β-diketiminato divanadium(I)
 inverted-sandwich complexes
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   2
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              205
_journal_page_last               207
_journal_paper_doi               10.1039/b711816c
_journal_year                    2008
_chemical_formula_moiety         'C64 H96 N4 O3 V2'
_chemical_formula_sum            'C64 H96 N4 O3 V2'
_chemical_formula_weight         1071.33
_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                 106.4620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7676(2)
_cell_length_b                   21.2023(4)
_cell_length_c                   23.5956(5)
_cell_measurement_reflns_used    29732
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     6605.3(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 19'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1059
_diffrn_reflns_av_sigmaI/netI    0.0741
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32107
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.325
_exptl_absorpt_correction_T_max  0.9752
_exptl_absorpt_correction_T_min  0.7099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
?
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.077
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       0.0135(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         11904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0721
_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)+(0.1087P)²+4.1296P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1911
_refine_ls_wR_factor_ref         0.2076
_reflns_number_gt                9165
_reflns_number_total             11904
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b711816c.txt
_cod_data_source_block           complex_2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7102791
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 0.1144(2) 0.09209(15) 0.10817(13) 0.0286(7) Uani 1 1 d . . .
C2 C 0.2124(3) 0.06638(16) 0.12137(14) 0.0321(7) Uani 1 1 d . . .
C3 C 0.2628(3) 0.03426(17) 0.17960(15) 0.0363(8) Uani 1 1 d . . .
H3 H 0.2396 0.0556 0.2103 0.044 Uiso 1 1 calc R . .
C4 C 0.2308(3) -0.03471(18) 0.17849(19) 0.0512(10) Uani 1 1 d . . .
H4A H 0.2628 -0.0538 0.2160 0.077 Uiso 1 1 calc R . .
H4B H 0.2508 -0.0566 0.1480 0.077 Uiso 1 1 calc R . .
H4C H 0.1585 -0.0371 0.1707 0.077 Uiso 1 1 calc R . .
C5 C 0.3784(3) 0.0382(2) 0.19757(17) 0.0476(10) Uani 1 1 d . . .
H5A H 0.4055 0.0178 0.2350 0.071 Uiso 1 1 calc R . .
H5B H 0.3988 0.0816 0.2007 0.071 Uiso 1 1 calc R . .
H5C H 0.4034 0.0176 0.1683 0.071 Uiso 1 1 calc R . .
C6 C 0.2614(3) 0.06825(19) 0.07688(16) 0.0424(9) Uani 1 1 d . . .
H6 H 0.3254 0.0503 0.0839 0.051 Uiso 1 1 calc R . .
C7 C 0.2173(3) 0.0960(2) 0.02330(17) 0.0495(10) Uani 1 1 d . . .
H7 H 0.2516 0.0967 -0.0055 0.059 Uiso 1 1 calc R . .
C8 C 0.1225(3) 0.1228(2) 0.01169(15) 0.0485(10) Uani 1 1 d . . .
H8 H 0.0938 0.1419 -0.0247 0.058 Uiso 1 1 calc R . .
C9 C 0.0696(3) 0.12140(17) 0.05348(14) 0.0378(8) Uani 1 1 d . . .
C10 C -0.0353(3) 0.1511(2) 0.03815(17) 0.0528(11) Uani 1 1 d . . .
H10 H -0.0619 0.1463 0.0723 0.063 Uiso 1 1 calc R . .
C11 C -0.0289(5) 0.2217(3) 0.0259(2) 0.0826(18) Uani 1 1 d . . .
H11A H -0.0954 0.2398 0.0163 0.124 Uiso 1 1 calc R . .
H11B H -0.0009 0.2274 -0.0067 0.124 Uiso 1 1 calc R . .
H11C H 0.0138 0.2420 0.0604 0.124 Uiso 1 1 calc R . .
C12 C -0.1088(4) 0.1178(3) -0.0152(2) 0.0785(16) Uani 1 1 d . . .
H12A H -0.1743 0.1372 -0.0236 0.118 Uiso 1 1 calc R . .
H12B H -0.1140 0.0740 -0.0061 0.118 Uiso 1 1 calc R . .
H12C H -0.0836 0.1215 -0.0490 0.118 Uiso 1 1 calc R . .
C13 C -0.0261(3) -0.00561(19) 0.10203(18) 0.0483(10) Uani 1 1 d . . .
H13A H 0.0245 -0.0017 0.0814 0.072 Uiso 1 1 calc R . .
H13B H -0.0922 -0.0031 0.0743 0.072 Uiso 1 1 calc R . .
H13C H -0.0186 -0.0455 0.1220 0.072 Uiso 1 1 calc R . .
C14 C -0.0136(2) 0.04673(16) 0.14645(14) 0.0320(7) Uani 1 1 d . . .
C15 C -0.0824(3) 0.04713(17) 0.17995(16) 0.0366(8) Uani 1 1 d . . .
H15 H -0.1214 0.0109 0.1777 0.044 Uiso 1 1 calc R . .
C16 C -0.1001(2) 0.09497(17) 0.21642(14) 0.0333(7) Uani 1 1 d . . .
C17 C -0.1891(3) 0.0866(2) 0.2407(2) 0.0549(11) Uani 1 1 d . . .
H17A H -0.1941 0.1223 0.2647 0.082 Uiso 1 1 calc R . .
H17B H -0.1800 0.0490 0.2643 0.082 Uiso 1 1 calc R . .
H17C H -0.2500 0.0830 0.2087 0.082 Uiso 1 1 calc R . .
C18 C -0.0764(2) 0.19859(16) 0.25920(15) 0.0324(7) Uani 1 1 d . . .
C19 C -0.1386(3) 0.24558(18) 0.22479(16) 0.0398(8) Uani 1 1 d . . .
C20 C -0.1774(3) 0.2414(2) 0.15781(18) 0.0541(11) Uani 1 1 d . . .
H20 H -0.1461 0.2045 0.1450 0.065 Uiso 1 1 calc R . .
C21 C -0.1489(4) 0.3000(3) 0.1281(2) 0.0734(15) Uani 1 1 d . . .
H21A H -0.1742 0.2957 0.0860 0.110 Uiso 1 1 calc R . .
H21B H -0.0765 0.3042 0.1391 0.110 Uiso 1 1 calc R . .
H21C H -0.1781 0.3367 0.1406 0.110 Uiso 1 1 calc R . .
C22 C -0.2939(4) 0.2319(4) 0.1383(3) 0.094(2) Uani 1 1 d . . .
H22A H -0.3175 0.2292 0.0960 0.142 Uiso 1 1 calc R . .
H22B H -0.3259 0.2669 0.1516 0.142 Uiso 1 1 calc R . .
H22C H -0.3105 0.1936 0.1552 0.142 Uiso 1 1 calc R . .
C23 C -0.1665(3) 0.29665(19) 0.25339(18) 0.0449(9) Uani 1 1 d . . .
H23 H -0.2074 0.3279 0.2312 0.054 Uiso 1 1 calc R . .
C24 C -0.1349(3) 0.30192(19) 0.31378(18) 0.0457(9) Uani 1 1 d . . .
H24 H -0.1536 0.3368 0.3321 0.055 Uiso 1 1 calc R . .
C25 C -0.0758(3) 0.25567(19) 0.34704(17) 0.0441(9) Uani 1 1 d . . .
H25 H -0.0560 0.2593 0.3880 0.053 Uiso 1 1 calc R . .
C26 C -0.0444(3) 0.20329(17) 0.32104(15) 0.0363(8) Uani 1 1 d . . .
C27 C 0.0191(3) 0.15267(18) 0.36082(16) 0.0398(8) Uani 1 1 d . . .
H27 H 0.0357 0.1201 0.3356 0.048 Uiso 1 1 calc R . .
C28 C -0.0404(4) 0.1215(2) 0.3995(2) 0.0599(12) Uani 1 1 d . . .
H28A H 0.0009 0.0898 0.4239 0.090 Uiso 1 1 calc R . .
H28B H -0.1007 0.1024 0.3747 0.090 Uiso 1 1 calc R . .
H28C H -0.0585 0.1528 0.4241 0.090 Uiso 1 1 calc R . .
C29 C 0.1180(3) 0.1792(2) 0.40047(17) 0.0460(9) Uani 1 1 d . . .
H29A H 0.1558 0.1461 0.4246 0.069 Uiso 1 1 calc R . .
H29B H 0.1033 0.2116 0.4253 0.069 Uiso 1 1 calc R . .
H29C H 0.1571 0.1968 0.3765 0.069 Uiso 1 1 calc R . .
C30 C 0.3991(3) 0.05117(16) 0.37085(14) 0.0317(7) Uani 1 1 d . . .
C31 C 0.3211(3) 0.00619(16) 0.36009(15) 0.0347(7) Uani 1 1 d . . .
C32 C 0.2144(3) 0.02152(18) 0.36239(16) 0.0383(8) Uani 1 1 d . . .
H32 H 0.2091 0.0675 0.3651 0.046 Uiso 1 1 calc R . .
C33 C 0.1933(3) -0.0072(3) 0.41738(19) 0.0603(12) Uani 1 1 d . . .
H33A H 0.1257 0.0032 0.4178 0.090 Uiso 1 1 calc R . .
H33B H 0.2407 0.0094 0.4522 0.090 Uiso 1 1 calc R . .
H33C H 0.2005 -0.0522 0.4166 0.090 Uiso 1 1 calc R . .
C34 C 0.1333(3) -0.0003(2) 0.30674(17) 0.0453(9) Uani 1 1 d . . .
H34A H 0.0674 0.0104 0.3101 0.068 Uiso 1 1 calc R . .
H34B H 0.1379 -0.0451 0.3026 0.068 Uiso 1 1 calc R . .
H34C H 0.1438 0.0203 0.2727 0.068 Uiso 1 1 calc R . .
C35 C 0.3453(3) -0.05563(18) 0.34902(17) 0.0446(9) Uani 1 1 d . . .
H35 H 0.2951 -0.0864 0.3419 0.054 Uiso 1 1 calc R . .
C36 C 0.4413(3) -0.07223(18) 0.34839(18) 0.0485(10) Uani 1 1 d . . .
H36 H 0.4557 -0.1140 0.3417 0.058 Uiso 1 1 calc R . .
C37 C 0.5167(3) -0.02737(19) 0.35764(16) 0.0451(9) Uani 1 1 d . . .
H37 H 0.5811 -0.0391 0.3564 0.054 Uiso 1 1 calc R . .
C38 C 0.4975(3) 0.03530(17) 0.36886(15) 0.0358(8) Uani 1 1 d . . .
C39 C 0.5823(3) 0.0838(2) 0.37864(17) 0.0433(9) Uani 1 1 d . . .
H39 H 0.5519 0.1256 0.3790 0.052 Uiso 1 1 calc R . .
C40 C 0.6322(3) 0.0833(3) 0.3293(2) 0.0614(12) Uani 1 1 d . . .
H40A H 0.6848 0.1145 0.3369 0.092 Uiso 1 1 calc R . .
H40B H 0.5827 0.0926 0.2925 0.092 Uiso 1 1 calc R . .
H40C H 0.6609 0.0424 0.3270 0.092 Uiso 1 1 calc R . .
C41 C 0.6605(4) 0.0743(3) 0.4387(2) 0.0687(14) Uani 1 1 d . . .
H41A H 0.7126 0.1057 0.4439 0.103 Uiso 1 1 calc R . .
H41B H 0.6899 0.0331 0.4402 0.103 Uiso 1 1 calc R . .
H41C H 0.6280 0.0783 0.4695 0.103 Uiso 1 1 calc R . .
C42 C 0.4249(3) 0.0877(2) 0.48981(16) 0.0515(10) Uani 1 1 d . . .
H42A H 0.4226 0.0458 0.4740 0.077 Uiso 1 1 calc R . .
H42B H 0.3766 0.0911 0.5121 0.077 Uiso 1 1 calc R . .
H42C H 0.4916 0.0961 0.5151 0.077 Uiso 1 1 calc R . .
C43 C 0.3990(3) 0.13527(18) 0.43924(14) 0.0357(8) Uani 1 1 d . . .
C44 C 0.3996(3) 0.19886(18) 0.45551(15) 0.0392(8) Uani 1 1 d . . .
H44 H 0.4064 0.2067 0.4952 0.047 Uiso 1 1 calc R . .
C45 C 0.3913(3) 0.25146(17) 0.41954(15) 0.0357(8) Uani 1 1 d . . .
C46 C 0.4179(4) 0.3131(2) 0.45186(18) 0.0537(11) Uani 1 1 d . . .
H46A H 0.4104 0.3468 0.4238 0.081 Uiso 1 1 calc R . .
H46B H 0.4868 0.3117 0.4763 0.081 Uiso 1 1 calc R . .
H46C H 0.3736 0.3202 0.4761 0.081 Uiso 1 1 calc R . .
C47 C 0.3752(3) 0.30586(16) 0.32901(15) 0.0341(7) Uani 1 1 d . . .
C48 C 0.2909(3) 0.34427(16) 0.30459(15) 0.0341(8) Uani 1 1 d . . .
C49 C 0.1850(3) 0.32685(17) 0.30778(16) 0.0376(8) Uani 1 1 d . . .
H49 H 0.1800 0.2808 0.3057 0.045 Uiso 1 1 calc R . .
C50 C 0.1688(3) 0.3468(2) 0.36696(19) 0.0530(10) Uani 1 1 d . . .
H50A H 0.1020 0.3347 0.3678 0.079 Uiso 1 1 calc R . .
H50B H 0.1761 0.3917 0.3713 0.079 Uiso 1 1 calc R . .
H50C H 0.2182 0.3264 0.3987 0.079 Uiso 1 1 calc R . .
C51 C 0.1006(3) 0.3527(2) 0.25717(19) 0.0509(10) Uani 1 1 d . . .
H51A H 0.0364 0.3397 0.2618 0.076 Uiso 1 1 calc R . .
H51B H 0.1076 0.3368 0.2205 0.076 Uiso 1 1 calc R . .
H51C H 0.1041 0.3979 0.2572 0.076 Uiso 1 1 calc R . .
C52 C 0.3064(3) 0.40066(18) 0.27846(17) 0.0460(9) Uani 1 1 d . . .
H52 H 0.2517 0.4272 0.2627 0.055 Uiso 1 1 calc R . .
C53 C 0.4010(4) 0.4181(2) 0.2753(2) 0.0566(11) Uani 1 1 d . . .
H53 H 0.4100 0.4566 0.2587 0.068 Uiso 1 1 calc R . .
C54 C 0.4818(3) 0.3785(2) 0.2967(2) 0.0523(10) Uani 1 1 d . . .
H54 H 0.5451 0.3903 0.2934 0.063 Uiso 1 1 calc R . .
C55 C 0.4718(3) 0.32152(18) 0.32302(18) 0.0436(9) Uani 1 1 d . . .
C56 C 0.5639(3) 0.2782(2) 0.3434(2) 0.0541(11) Uani 1 1 d . . .
H56 H 0.5418 0.2395 0.3588 0.065 Uiso 1 1 calc R . .
C57 C 0.6026(4) 0.2601(3) 0.2915(3) 0.0774(15) Uani 1 1 d . . .
H57A H 0.6599 0.2326 0.3049 0.116 Uiso 1 1 calc R . .
H57B H 0.6223 0.2974 0.2746 0.116 Uiso 1 1 calc R . .
H57C H 0.5499 0.2388 0.2623 0.116 Uiso 1 1 calc R . .
C58 C 0.6485(4) 0.3073(3) 0.3930(2) 0.0762(15) Uani 1 1 d . . .
H58A H 0.7042 0.2783 0.4045 0.114 Uiso 1 1 calc R . .
H58B H 0.6237 0.3160 0.4263 0.114 Uiso 1 1 calc R . .
H58C H 0.6707 0.3458 0.3793 0.114 Uiso 1 1 calc R . .
C59 C 0.4141(9) 0.2228(6) 0.1280(4) 0.163(4) Uani 1 1 d . . .
H59A H 0.4317 0.1906 0.1579 0.245 Uiso 1 1 calc R . .
H59B H 0.4723 0.2486 0.1303 0.245 Uiso 1 1 calc R . .
H59C H 0.3919 0.2034 0.0897 0.245 Uiso 1 1 calc R . .
C60 C 0.3348(10) 0.2607(8) 0.1373(7) 0.218(7) Uani 1 1 d . . .
H60A H 0.2800 0.2322 0.1379 0.262 Uiso 1 1 calc R . .
H60B H 0.3597 0.2778 0.1770 0.262 Uiso 1 1 calc R . .
C61 C 0.2924(8) 0.3095(6) 0.1018(4) 0.128(3) Uani 1 1 d . . .
H61A H 0.3487 0.3360 0.0998 0.154 Uiso 1 1 calc R . .
H61B H 0.2661 0.2912 0.0628 0.154 Uiso 1 1 calc R . .
C62 C 0.2195(10) 0.3502(6) 0.1075(5) 0.149(4) Uani 1 1 d . . .
H62A H 0.1684 0.3229 0.1156 0.179 Uiso 1 1 calc R . .
H62B H 0.2506 0.3718 0.1444 0.179 Uiso 1 1 calc R . .
C63 C 0.1667(10) 0.3943(7) 0.0739(6) 0.170(4) Uani 1 1 d . . .
H63A H 0.1319 0.3728 0.0375 0.204 Uiso 1 1 calc R . .
H63B H 0.2168 0.4210 0.0641 0.204 Uiso 1 1 calc R . .
C64 C 0.0956(13) 0.4357(6) 0.0837(6) 0.209(6) Uani 1 1 d . . .
H64A H 0.0706 0.4621 0.0496 0.313 Uiso 1 1 calc R . .
H64B H 0.1265 0.4615 0.1175 0.313 Uiso 1 1 calc R . .
H64C H 0.0406 0.4124 0.0909 0.313 Uiso 1 1 calc R . .
V1 V 0.08694(4) 0.16277(2) 0.20994(2) 0.02444(17) Uani 1 1 d . . .
V2 V 0.32841(4) 0.17040(3) 0.31136(2) 0.02557(18) Uani 1 1 d . . .
N1 N 0.05966(19) 0.09037(12) 0.15222(11) 0.0269(6) Uani 1 1 d . . .
N2 N -0.0434(2) 0.14664(13) 0.22940(12) 0.0295(6) Uani 1 1 d . . .
N3 N 0.37893(19) 0.11646(13) 0.38307(11) 0.0290(6) Uani 1 1 d . . .
N4 N 0.3651(2) 0.24895(13) 0.36079(11) 0.0308(6) Uani 1 1 d . . .
O1 O 0.07224(19) 0.22477(11) 0.17031(10) 0.0377(6) Uani 1 1 d . . .
O2 O 0.40931(18) 0.16574(12) 0.27500(10) 0.0389(6) Uani 1 1 d . . .
O3 O 0.19627(17) 0.15662(11) 0.27324(10) 0.0335(5) 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'
V V 0.3005 0.5294 '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'
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 C9 121.2(3) . . ?
C2 C1 N1 119.6(3) . . ?
C9 C1 N1 119.2(3) . . ?
C6 C2 C1 117.3(3) . . ?
C6 C2 C3 119.9(3) . . ?
C1 C2 C3 122.7(3) . . ?
C2 C3 C4 111.1(3) . . ?
C2 C3 C5 113.6(3) . . ?
C4 C3 C5 109.3(3) . . ?
C2 C3 H3 107.5 . . ?
C4 C3 H3 107.5 . . ?
C5 C3 H3 107.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C2 121.4(3) . . ?
C7 C6 H6 119.3 . . ?
C2 C6 H6 119.3 . . ?
C6 C7 C8 120.5(3) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C7 C8 C9 120.7(3) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C8 C9 C1 118.7(3) . . ?
C8 C9 C10 118.6(3) . . ?
C1 C9 C10 122.7(3) . . ?
C9 C10 C11 110.3(4) . . ?
C9 C10 C12 111.3(4) . . ?
C11 C10 C12 110.6(4) . . ?
C9 C10 H10 108.2 . . ?
C11 C10 H10 108.2 . . ?
C12 C10 H10 108.2 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N1 C14 C15 123.2(3) . . ?
N1 C14 C13 120.8(3) . . ?
C15 C14 C13 115.9(3) . . ?
C14 C15 C16 128.3(3) . . ?
C14 C15 H15 115.9 . . ?
C16 C15 H15 115.9 . . ?
N2 C16 C15 123.1(3) . . ?
N2 C16 C17 119.9(3) . . ?
C15 C16 C17 116.9(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C26 C18 C19 120.6(3) . . ?
C26 C18 N2 120.7(3) . . ?
C19 C18 N2 118.7(3) . . ?
C23 C19 C18 118.6(3) . . ?
C23 C19 C20 119.2(3) . . ?
C18 C19 C20 122.2(3) . . ?
C19 C20 C21 111.6(4) . . ?
C19 C20 C22 110.2(4) . . ?
C21 C20 C22 110.3(4) . . ?
C19 C20 H20 108.2 . . ?
C21 C20 H20 108.2 . . ?
C22 C20 H20 108.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C19 121.3(4) . . ?
C24 C23 H23 119.4 . . ?
C19 C23 H23 119.4 . . ?
C25 C24 C23 119.9(4) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C25 C26 121.7(4) . . ?
C24 C25 H25 119.1 . . ?
C26 C25 H25 119.1 . . ?
C25 C26 C18 118.0(3) . . ?
C25 C26 C27 118.9(3) . . ?
C18 C26 C27 123.1(3) . . ?
C29 C27 C26 111.9(3) . . ?
C29 C27 C28 109.1(3) . . ?
C26 C27 C28 111.0(3) . . ?
C29 C27 H27 108.2 . . ?
C26 C27 H27 108.2 . . ?
C28 C27 H27 108.2 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C38 121.7(3) . . ?
C31 C30 N3 120.1(3) . . ?
C38 C30 N3 118.2(3) . . ?
C35 C31 C30 117.4(3) . . ?
C35 C31 C32 119.5(3) . . ?
C30 C31 C32 123.1(3) . . ?
C31 C32 C33 111.2(3) . . ?
C31 C32 C34 112.4(3) . . ?
C33 C32 C34 109.7(3) . . ?
C31 C32 H32 107.8 . . ?
C33 C32 H32 107.8 . . ?
C34 C32 H32 107.8 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C31 121.6(4) . . ?
C36 C35 H35 119.2 . . ?
C31 C35 H35 119.2 . . ?
C35 C36 C37 120.4(4) . . ?
C35 C36 H36 119.8 . . ?
C37 C36 H36 119.8 . . ?
C36 C37 C38 120.9(4) . . ?
C36 C37 H37 119.6 . . ?
C38 C37 H37 119.6 . . ?
C37 C38 C30 118.0(3) . . ?
C37 C38 C39 119.6(3) . . ?
C30 C38 C39 122.4(3) . . ?
C40 C39 C38 112.0(3) . . ?
C40 C39 C41 111.0(4) . . ?
C38 C39 C41 111.1(3) . . ?
C40 C39 H39 107.5 . . ?
C38 C39 H39 107.5 . . ?
C41 C39 H39 107.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 H42A 109.5 . . ?
C43 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C43 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N3 C43 C44 122.9(3) . . ?
N3 C43 C42 121.0(3) . . ?
C44 C43 C42 116.1(3) . . ?
C45 C44 C43 127.8(3) . . ?
C45 C44 H44 116.1 . . ?
C43 C44 H44 116.1 . . ?
N4 C45 C44 123.8(3) . . ?
N4 C45 C46 121.2(3) . . ?
C44 C45 C46 115.0(3) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 C55 120.9(3) . . ?
C48 C47 N4 120.6(3) . . ?
C55 C47 N4 118.5(3) . . ?
C52 C48 C47 118.0(3) . . ?
C52 C48 C49 119.9(3) . . ?
C47 C48 C49 122.0(3) . . ?
C51 C49 C48 113.9(3) . . ?
C51 C49 C50 109.9(3) . . ?
C48 C49 C50 111.4(3) . . ?
C51 C49 H49 107.1 . . ?
C48 C49 H49 107.1 . . ?
C50 C49 H49 107.1 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49 C51 H51A 109.5 . . ?
C49 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C49 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C53 C52 C48 121.4(4) . . ?
C53 C52 H52 119.3 . . ?
C48 C52 H52 119.3 . . ?
C54 C53 C52 119.9(4) . . ?
C54 C53 H53 120.0 . . ?
C52 C53 H53 120.0 . . ?
C53 C54 C55 121.7(4) . . ?
C53 C54 H54 119.2 . . ?
C55 C54 H54 119.2 . . ?
C54 C55 C47 117.8(4) . . ?
C54 C55 C56 119.1(4) . . ?
C47 C55 C56 123.1(3) . . ?
C57 C56 C58 110.7(4) . . ?
C57 C56 C55 110.3(4) . . ?
C58 C56 C55 112.6(4) . . ?
C57 C56 H56 107.7 . . ?
C58 C56 H56 107.7 . . ?
C55 C56 H56 107.7 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C60 C59 H59A 109.5 . . ?
C60 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C60 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C61 C60 C59 123.5(12) . . ?
C61 C60 H60A 106.5 . . ?
C59 C60 H60A 106.5 . . ?
C61 C60 H60B 106.5 . . ?
C59 C60 H60B 106.5 . . ?
H60A C60 H60B 106.5 . . ?
C62 C61 C60 128.7(10) . . ?
C62 C61 H61A 105.1 . . ?
C60 C61 H61A 105.1 . . ?
C62 C61 H61B 105.1 . . ?
C60 C61 H61B 105.1 . . ?
H61A C61 H61B 105.9 . . ?
C63 C62 C61 134.0(12) . . ?
C63 C62 H62A 103.7 . . ?
C61 C62 H62A 103.7 . . ?
C63 C62 H62B 103.7 . . ?
C61 C62 H62B 103.7 . . ?
H62A C62 H62B 105.3 . . ?
C62 C63 C64 130.6(13) . . ?
C62 C63 H63A 104.6 . . ?
C64 C63 H63A 104.6 . . ?
C62 C63 H63B 104.6 . . ?
C64 C63 H63B 104.6 . . ?
H63A C63 H63B 105.7 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
O1 V1 O3 118.96(12) . . ?
O1 V1 N2 107.60(12) . . ?
O3 V1 N2 112.96(11) . . ?
O1 V1 N1 105.29(11) . . ?
O3 V1 N1 117.22(11) . . ?
N2 V1 N1 90.99(11) . . ?
O2 V2 O3 118.75(12) . . ?
O2 V2 N3 107.01(12) . . ?
O3 V2 N3 112.85(11) . . ?
O2 V2 N4 105.34(12) . . ?
O3 V2 N4 118.24(11) . . ?
N3 V2 N4 90.74(11) . . ?
C14 N1 C1 118.2(3) . . ?
C14 N1 V1 125.6(2) . . ?
C1 N1 V1 115.53(19) . . ?
C16 N2 C18 119.7(3) . . ?
C16 N2 V1 126.4(2) . . ?
C18 N2 V1 113.9(2) . . ?
C43 N3 C30 118.9(3) . . ?
C43 N3 V2 126.5(2) . . ?
C30 N3 V2 114.63(19) . . ?
C45 N4 C47 118.0(3) . . ?
C45 N4 V2 125.9(2) . . ?
C47 N4 V2 115.8(2) . . ?
V1 O3 V2 152.51(15) . . ?
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 1.405(5) . ?
C1 C9 1.407(5) . ?
C1 N1 1.447(4) . ?
C2 C6 1.401(5) . ?
C2 C3 1.514(5) . ?
C3 C4 1.526(5) . ?
C3 C5 1.528(5) . ?
C3 H3 0.9800 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.370(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.378(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.382(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.523(5) . ?
C10 C11 1.532(7) . ?
C10 C12 1.543(6) . ?
C10 H10 0.9800 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.503(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 N1 1.347(4) . ?
C14 C15 1.395(5) . ?
C15 C16 1.396(5) . ?
C15 H15 0.9300 . ?
C16 N2 1.329(4) . ?
C16 C17 1.503(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C26 1.403(5) . ?
C18 C19 1.412(5) . ?
C18 N2 1.447(4) . ?
C19 C23 1.386(5) . ?
C19 C20 1.521(5) . ?
C20 C21 1.531(7) . ?
C20 C22 1.552(7) . ?
C20 H20 0.9800 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.371(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.371(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.395(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.527(5) . ?
C27 C29 1.524(5) . ?
C27 C28 1.539(6) . ?
C27 H27 0.9800 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.405(5) . ?
C30 C38 1.410(5) . ?
C30 N3 1.457(4) . ?
C31 C35 1.395(5) . ?
C31 C32 1.520(5) . ?
C32 C33 1.534(5) . ?
C32 C34 1.534(5) . ?
C32 H32 0.9800 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.373(6) . ?
C35 H35 0.9300 . ?
C36 C37 1.378(6) . ?
C36 H36 0.9300 . ?
C37 C38 1.395(5) . ?
C37 H37 0.9300 . ?
C38 C39 1.523(5) . ?
C39 C40 1.511(6) . ?
C39 C41 1.530(5) . ?
C39 H39 0.9800 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 C43 1.526(5) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 N3 1.336(4) . ?
C43 C44 1.401(5) . ?
C44 C45 1.386(5) . ?
C44 H44 0.9300 . ?
C45 N4 1.331(4) . ?
C45 C46 1.506(5) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 C48 1.400(5) . ?
C47 C55 1.417(5) . ?
C47 N4 1.448(4) . ?
C48 C52 1.389(5) . ?
C48 C49 1.526(5) . ?
C49 C51 1.514(5) . ?
C49 C50 1.535(5) . ?
C49 H49 0.9800 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 C53 1.375(6) . ?
C52 H52 0.9300 . ?
C53 C54 1.371(6) . ?
C53 H53 0.9300 . ?
C54 C55 1.384(6) . ?
C54 H54 0.9300 . ?
C55 C56 1.528(6) . ?
C56 C57 1.518(7) . ?
C56 C58 1.527(6) . ?
C56 H56 0.9800 . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C59 C60 1.423(15) . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C60 C61 1.355(14) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C61 C62 1.358(13) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C62 C63 1.305(13) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C63 C64 1.383(15) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
V1 O1 1.592(2) . ?
V1 O3 1.800(2) . ?
V1 N2 2.004(3) . ?
V1 N1 2.015(3) . ?
V2 O2 1.590(2) . ?
V2 O3 1.810(2) . ?
V2 N3 1.997(3) . ?
V2 N4 2.014(3) . ?
