#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:32:58 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179850 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/46/7014690.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_7014690
loop_
_publ_author_name
'Chang, Kai-Chieh'
'Lu, Chia-Fu'
'Wang, Po-Yang'
'Lu, Duan-Yen'
'Chen, Hong-Zhang'
'Kuo, Ting-Shen'
'Tsai, Yi-Chou'
_publ_section_title
;
 Ligand-controlled synthesis of vanadium(i) β-diketiminates and their
 catalysis in cyclotrimerization of alkynes.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2324
_journal_page_last               2331
_journal_paper_doi               10.1039/c0dt01061h
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C72 H64 N4 V2'
_chemical_formula_sum            'C72 H64 N4 V2'
_chemical_formula_weight         1087.15
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ya'
_symmetry_space_group_name_H-M   'P 1 2/a 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                 112.559(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.8878(12)
_cell_length_b                   9.5634(5)
_cell_length_c                   25.2169(12)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     5542.7(5)
_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    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1006
_diffrn_reflns_av_sigmaI/netI    0.1227
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37278
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_T_max  0.9847
_exptl_absorpt_correction_T_min  0.8997
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         9846
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1683
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0886P)²+6.9017P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.2118
_reflns_number_gt                4872
_reflns_number_total             9846
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT01061H.TXT
_cod_data_source_block           a8935
_cod_original_sg_symbol_H-M      'P 2/a'
_cod_database_code               7014690
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'-x, -y, -z'
'x-1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1252(2) 0.9085(7) 0.6273(2) 0.0257(14) Uani 1 1 d . . .
C2 C 0.0953(2) 0.7834(6) 0.6092(2) 0.0254(14) Uani 1 1 d . . .
C3 C 0.1204(3) 0.6644(7) 0.5940(2) 0.0375(16) Uani 1 1 d . . .
H3 H 0.1588 0.6699 0.5948 0.045 Uiso 1 1 calc R . .
C4 C 0.0904(3) 0.5441(8) 0.5783(3) 0.0450(18) Uani 1 1 d . . .
H4 H 0.1086 0.4652 0.5693 0.054 Uiso 1 1 calc R . .
C5 C 0.0322(3) 0.5323(8) 0.5748(2) 0.0433(18) Uani 1 1 d . . .
H5 H 0.0116 0.4467 0.5633 0.052 Uiso 1 1 calc R . .
C6 C 0.0068(2) 0.6432(7) 0.5879(2) 0.0374(16) Uani 1 1 d . . .
H6 H -0.0323 0.6354 0.5851 0.045 Uiso 1 1 calc R . .
C7 C 0.0367(2) 0.7727(7) 0.6060(2) 0.0291(14) Uani 1 1 d . . .
C8 C 0.0108(2) 0.8884(7) 0.6198(2) 0.0328(16) Uani 1 1 d . . .
H8 H -0.0283 0.8814 0.6168 0.039 Uiso 1 1 calc R . .
C9 C 0.0404(2) 1.0144(7) 0.6378(2) 0.0328(15) Uani 1 1 d . . .
C10 C 0.0141(3) 1.1344(8) 0.6514(3) 0.0439(18) Uani 1 1 d . . .
H10 H -0.0249 1.1281 0.6489 0.053 Uiso 1 1 calc R . .
C11 C 0.0426(3) 1.2556(8) 0.6675(2) 0.0431(17) Uani 1 1 d . . .
H11 H 0.0236 1.3341 0.6757 0.052 Uiso 1 1 calc R . .
C12 C 0.1008(3) 1.2666(7) 0.6724(2) 0.0388(16) Uani 1 1 d . . .
H12 H 0.1209 1.3527 0.6839 0.047 Uiso 1 1 calc R . .
C13 C 0.1285(2) 1.1543(7) 0.6606(2) 0.0328(15) Uani 1 1 d . . .
H13 H 0.1679 1.1630 0.6646 0.039 Uiso 1 1 calc R . .
C14 C 0.0990(2) 1.0247(6) 0.6424(2) 0.0258(14) Uani 1 1 d . . .
C15 C 0.2159(2) 0.8258(8) 0.7250(2) 0.0446(19) Uani 1 1 d . . .
H15A H 0.1740 0.8106 0.7132 0.067 Uiso 1 1 calc R . .
H15B H 0.2298 0.8878 0.7585 0.067 Uiso 1 1 calc R . .
H15C H 0.2362 0.7359 0.7349 0.067 Uiso 1 1 calc R . .
C16 C 0.2278(2) 0.8922(7) 0.6761(2) 0.0308(15) Uani 1 1 d . . .
C17 C 0.2854(2) 0.9217(7) 0.6851(2) 0.0310(15) Uani 1 1 d . . .
H17 H 0.3141 0.8804 0.7181 0.037 Uiso 1 1 calc R . .
C18 C 0.3061(2) 1.0042(6) 0.6517(2) 0.0284(15) Uani 1 1 d . . .
C19 C 0.3704(2) 1.0399(8) 0.6765(2) 0.0427(18) Uani 1 1 d . . .
H19A H 0.3797 1.0984 0.6492 0.064 Uiso 1 1 calc R . .
H19B H 0.3933 0.9536 0.6837 0.064 Uiso 1 1 calc R . .
H19C H 0.3799 1.0909 0.7127 0.064 Uiso 1 1 calc R . .
C20 C 0.20259(19) 1.1512(6) 0.4266(2) 0.0222(13) Uani 1 1 d . . .
C21 C 0.2084(2) 1.2948(7) 0.4185(2) 0.0259(14) Uani 1 1 d . . .
C22 C 0.2373(2) 1.3472(7) 0.3837(2) 0.0360(16) Uani 1 1 d . . .
H22 H 0.2539 1.2837 0.3652 0.043 Uiso 1 1 calc R . .
C23 C 0.2414(3) 1.4876(8) 0.3764(3) 0.0414(17) Uani 1 1 d . . .
H23 H 0.2601 1.5205 0.3523 0.050 Uiso 1 1 calc R . .
C24 C 0.2186(3) 1.5836(8) 0.4040(3) 0.0517(19) Uani 1 1 d . . .
H24 H 0.2227 1.6812 0.3994 0.062 Uiso 1 1 calc R . .
C25 C 0.1906(3) 1.5370(7) 0.4373(3) 0.0423(17) Uani 1 1 d . . .
H25 H 0.1751 1.6032 0.4557 0.051 Uiso 1 1 calc R . .
C26 C 0.1838(2) 1.3940(7) 0.4454(2) 0.0278(14) Uani 1 1 d . . .
C27 C 0.1524(2) 1.3424(7) 0.4770(2) 0.0291(14) Uani 1 1 d . . .
H27 H 0.1361 1.4075 0.4950 0.035 Uiso 1 1 calc R . .
C28 C 0.1441(2) 1.2023(7) 0.4830(2) 0.0248(14) Uani 1 1 d . . .
C29 C 0.1109(2) 1.1486(7) 0.5144(2) 0.0316(15) Uani 1 1 d . . .
H29 H 0.1036 1.2060 0.5417 0.038 Uiso 1 1 calc R . .
C30 C 0.0890(2) 1.0100(7) 0.5045(2) 0.0326(16) Uani 1 1 d . . .
H30 H 0.0558 0.9843 0.5122 0.039 Uiso 1 1 calc R . .
C31 C 0.1167(2) 0.9136(7) 0.4834(2) 0.0295(15) Uani 1 1 d . . .
H31 H 0.1040 0.8191 0.4785 0.035 Uiso 1 1 calc R . .
C32 C 0.1647(2) 0.9548(7) 0.4689(2) 0.0274(15) Uani 1 1 d . . .
H32 H 0.1916 0.8873 0.4662 0.033 Uiso 1 1 calc R . .
C33 C 0.1715(2) 1.1014(6) 0.4584(2) 0.0247(14) Uani 1 1 d . . .
C34 C 0.3817(2) 0.2148(6) 0.8796(2) 0.0221(13) Uani 1 1 d . . .
C35 C 0.4101(2) 0.3436(7) 0.8983(2) 0.0262(14) Uani 1 1 d . . .
C36 C 0.3823(2) 0.4606(7) 0.9106(2) 0.0333(15) Uani 1 1 d . . .
H36 H 0.3435 0.4523 0.9087 0.040 Uiso 1 1 calc R . .
C37 C 0.4107(3) 0.5855(7) 0.9254(2) 0.0361(16) Uani 1 1 d . . .
H37 H 0.3907 0.6640 0.9321 0.043 Uiso 1 1 calc R . .
C38 C 0.4689(3) 0.6008(8) 0.9309(2) 0.0427(18) Uani 1 1 d . . .
H38 H 0.4881 0.6883 0.9417 0.051 Uiso 1 1 calc R . .
C39 C 0.4975(3) 0.4895(8) 0.9206(2) 0.0407(17) Uani 1 1 d . . .
H39 H 0.5369 0.5000 0.9248 0.049 Uiso 1 1 calc R . .
C40 C 0.4697(2) 0.3569(7) 0.9035(2) 0.0287(15) Uani 1 1 d . . .
C41 C 0.4975(2) 0.2436(7) 0.8907(2) 0.0353(16) Uani 1 1 d . . .
H41 H 0.5370 0.2527 0.8949 0.042 Uiso 1 1 calc R . .
C42 C 0.4687(2) 0.1164(7) 0.8718(2) 0.0281(15) Uani 1 1 d . . .
C43 C 0.4973(3) 0.0019(8) 0.8582(2) 0.0398(17) Uani 1 1 d . . .
H43 H 0.5368 0.0104 0.8626 0.048 Uiso 1 1 calc R . .
C44 C 0.4684(3) -0.1200(8) 0.8390(3) 0.0471(19) Uani 1 1 d . . .
H44 H 0.4880 -0.1959 0.8299 0.056 Uiso 1 1 calc R . .
C45 C 0.4103(3) -0.1353(7) 0.8324(2) 0.0376(16) Uani 1 1 d . . .
H45 H 0.3907 -0.2213 0.8189 0.045 Uiso 1 1 calc R . .
C46 C 0.3817(2) -0.0275(7) 0.8452(2) 0.0308(15) Uani 1 1 d . . .
H46 H 0.3423 -0.0397 0.8408 0.037 Uiso 1 1 calc R . .
C47 C 0.4094(2) 0.1029(6) 0.8651(2) 0.0249(14) Uani 1 1 d . . .
C48 C 0.2924(2) 0.3014(7) 0.7806(2) 0.0417(18) Uani 1 1 d . . .
H48A H 0.3345 0.3145 0.7928 0.063 Uiso 1 1 calc R . .
H48B H 0.2730 0.3925 0.7716 0.063 Uiso 1 1 calc R . .
H48C H 0.2782 0.2419 0.7463 0.063 Uiso 1 1 calc R . .
C49 C 0.2795(2) 0.2327(6) 0.8282(2) 0.0252(13) Uani 1 1 d . . .
C50 C 0.2211(2) 0.2058(6) 0.8178(2) 0.0281(15) Uani 1 1 d . . .
H50 H 0.1934 0.2489 0.7846 0.034 Uiso 1 1 calc R . .
C51 C 0.1985(2) 0.1243(6) 0.8498(2) 0.0247(14) Uani 1 1 d . . .
C52 C 0.1340(2) 0.0974(7) 0.8246(2) 0.0368(17) Uani 1 1 d . . .
H52A H 0.1234 0.0384 0.8509 0.055 Uiso 1 1 calc R . .
H52B H 0.1235 0.0498 0.7876 0.055 Uiso 1 1 calc R . .
H52C H 0.1131 0.1865 0.8190 0.055 Uiso 1 1 calc R . .
C53 C 0.2956(2) -0.0277(6) 1.0740(2) 0.0206(13) Uani 1 1 d . . .
C54 C 0.2890(2) -0.1729(6) 1.0818(2) 0.0236(14) Uani 1 1 d . . .
C55 C 0.2595(2) -0.2242(7) 1.1160(2) 0.0296(15) Uani 1 1 d . . .
H55 H 0.2426 -0.1597 1.1338 0.036 Uiso 1 1 calc R . .
C56 C 0.2549(2) -0.3632(7) 1.1238(3) 0.0389(16) Uani 1 1 d . . .
H56 H 0.2352 -0.3951 1.1472 0.047 Uiso 1 1 calc R . .
C57 C 0.2794(3) -0.4612(7) 1.0973(3) 0.0437(18) Uani 1 1 d . . .
H57 H 0.2754 -0.5585 1.1023 0.052 Uiso 1 1 calc R . .
C58 C 0.3082(2) -0.4167(7) 1.0649(3) 0.0362(16) Uani 1 1 d . . .
H58 H 0.3244 -0.4837 1.0473 0.043 Uiso 1 1 calc R . .
C59 C 0.3151(2) -0.2720(6) 1.0563(2) 0.0258(14) Uani 1 1 d . . .
C60 C 0.3481(2) -0.2210(6) 1.0264(2) 0.0237(13) Uani 1 1 d . . .
H60 H 0.3652 -0.2866 1.0093 0.028 Uiso 1 1 calc R . .
C61 C 0.35709(19) -0.0814(6) 1.0205(2) 0.0202(13) Uani 1 1 d . . .
C62 C 0.3929(2) -0.0301(6) 0.9914(2) 0.0268(14) Uani 1 1 d . . .
H62 H 0.4026 -0.0889 0.9660 0.032 Uiso 1 1 calc R . .
C63 C 0.4135(2) 0.1097(6) 1.0013(2) 0.0264(15) Uani 1 1 d . . .
H63 H 0.4470 0.1360 0.9944 0.032 Uiso 1 1 calc R . .
C64 C 0.3848(2) 0.2066(7) 1.0208(2) 0.0271(14) Uani 1 1 d . . .
H64 H 0.3977 0.3010 1.0261 0.032 Uiso 1 1 calc R . .
C65 C 0.3353(2) 0.1660(6) 1.0331(2) 0.0225(13) Uani 1 1 d . . .
H65 H 0.3076 0.2333 1.0340 0.027 Uiso 1 1 calc R . .
C66 C 0.3287(2) 0.0209(6) 1.0441(2) 0.0222(14) Uani 1 1 d . . .
C67 C 0.4005(5) 0.5519(14) 0.7461(5) 0.139(4) Uiso 1 1 d . . .
H67A H 0.3581 0.5433 0.7323 0.208 Uiso 1 1 calc R . .
H67B H 0.4106 0.6259 0.7247 0.208 Uiso 1 1 calc R . .
H67C H 0.4161 0.5754 0.7871 0.208 Uiso 1 1 calc R . .
C68 C 0.4245(5) 0.4235(14) 0.7379(5) 0.132(4) Uiso 1 1 d . . .
H68A H 0.4078 0.3982 0.6967 0.158 Uiso 1 1 calc R . .
H68B H 0.4144 0.3487 0.7596 0.158 Uiso 1 1 calc R . .
C69 C 0.4919(4) 0.4344(12) 0.7585(4) 0.108(3) Uiso 1 1 d . . .
H69A H 0.5023 0.5111 0.7379 0.129 Uiso 1 1 calc R . .
H69B H 0.5091 0.4551 0.8001 0.129 Uiso 1 1 calc R . .
C70 C 0.5151(5) 0.2985(14) 0.7468(5) 0.137(4) Uiso 1 1 d . . .
H70A H 0.5009 0.2844 0.7047 0.165 Uiso 1 1 calc R . .
H70B H 0.4995 0.2214 0.7630 0.165 Uiso 1 1 calc R . .
C71 C 0.5817(4) 0.2902(11) 0.7720(4) 0.094(3) Uiso 1 1 d . . .
H71A H 0.5966 0.2845 0.8144 0.113 Uiso 1 1 calc R . .
H71B H 0.5949 0.2063 0.7574 0.113 Uiso 1 1 calc R . .
C72 C 0.6023(5) 0.4128(14) 0.7548(5) 0.142(5) Uiso 1 1 d . . .
H72A H 0.6449 0.4120 0.7705 0.213 Uiso 1 1 calc R . .
H72B H 0.5886 0.4949 0.7693 0.213 Uiso 1 1 calc R . .
H72C H 0.5875 0.4166 0.7128 0.213 Uiso 1 1 calc R . .
N1 N 0.18293(17) 0.9261(5) 0.62755(17) 0.0270(12) Uani 1 1 d . . .
N2 N 0.27174(17) 1.0544(5) 0.60047(17) 0.0238(11) Uani 1 1 d . . .
N3 N 0.32334(16) 0.1958(5) 0.87694(16) 0.0212(11) Uani 1 1 d . . .
N4 N 0.23161(16) 0.0688(5) 0.90048(17) 0.0223(11) Uani 1 1 d . . .
V1 V 0.18589(4) 1.02001(11) 0.55674(4) 0.0247(3) Uani 1 1 d . . .
V2 V 0.31752(3) 0.09935(10) 0.94597(4) 0.0217(3) 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'
Cl Cl 0.1484 0.1585 '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
C2 C1 C14 121.3(5) . . ?
C2 C1 N1 120.6(5) . . ?
C14 C1 N1 117.9(5) . . ?
C1 C2 C3 122.8(5) . . ?
C1 C2 C7 119.1(5) . . ?
C3 C2 C7 118.1(5) . . ?
C4 C3 C2 120.9(6) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 121.5(7) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C6 C5 C4 119.2(6) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C7 121.9(6) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 H6 119.0 . . ?
C8 C7 C6 122.4(5) . . ?
C8 C7 C2 119.2(6) . . ?
C6 C7 C2 118.3(6) . . ?
C7 C8 C9 122.2(5) . . ?
C7 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C8 C9 C14 118.9(6) . . ?
C8 C9 C10 122.7(6) . . ?
C14 C9 C10 118.4(6) . . ?
C11 C10 C9 122.1(6) . . ?
C11 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C10 C11 C12 119.9(6) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 120.6(6) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 120.8(5) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C1 C14 C9 119.3(6) . . ?
C1 C14 C13 122.5(5) . . ?
C9 C14 C13 118.2(6) . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C16 C17 122.9(5) . . ?
N1 C16 C15 119.4(5) . . ?
C17 C16 C15 117.6(5) . . ?
C18 C17 C16 127.9(5) . . ?
C18 C17 H17 116.0 . . ?
C16 C17 H17 116.0 . . ?
N2 C18 C17 122.9(5) . . ?
N2 C18 C19 120.0(5) . . ?
C17 C18 C19 117.1(5) . . ?
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 . . ?
C33 C20 C21 121.9(5) . . ?
C33 C20 N2 119.9(5) . 2_556 ?
C21 C20 N2 118.2(5) . 2_556 ?
C20 C21 C22 122.6(6) . . ?
C20 C21 C26 119.5(5) . . ?
C22 C21 C26 117.9(6) . . ?
C23 C22 C21 120.7(6) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C22 C23 C24 121.0(6) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C25 C24 C23 119.7(7) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C26 121.9(7) . . ?
C24 C25 H25 119.0 . . ?
C26 C25 H25 119.0 . . ?
C27 C26 C25 123.3(6) . . ?
C27 C26 C21 117.9(6) . . ?
C25 C26 C21 118.7(6) . . ?
C28 C27 C26 123.2(6) . . ?
C28 C27 H27 118.4 . . ?
C26 C27 H27 118.4 . . ?
C27 C28 C29 123.4(6) . . ?
C27 C28 C33 119.1(5) . . ?
C29 C28 C33 117.4(6) . . ?
C27 C28 V1 137.3(4) . . ?
C29 C28 V1 60.0(3) . . ?
C33 C28 V1 73.8(3) . . ?
C30 C29 C28 119.8(5) . . ?
C30 C29 V1 75.8(3) . . ?
C28 C29 V1 84.5(3) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
V1 C29 H29 110.0 . . ?
C31 C30 C29 118.6(5) . . ?
C31 C30 V1 70.9(3) . . ?
C29 C30 V1 66.8(3) . . ?
C31 C30 H30 120.7 . . ?
C29 C30 H30 120.7 . . ?
V1 C30 H30 135.0 . . ?
C30 C31 C32 120.4(6) . . ?
C30 C31 V1 73.5(3) . . ?
C32 C31 V1 68.4(3) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
V1 C31 H31 130.9 . . ?
C31 C32 C33 118.7(5) . . ?
C31 C32 V1 73.6(3) . . ?
C33 C32 V1 84.8(3) . . ?
C31 C32 H32 120.6 . . ?
C33 C32 H32 120.6 . . ?
V1 C32 H32 111.5 . . ?
C20 C33 C32 124.4(5) . . ?
C20 C33 C28 118.3(5) . . ?
C32 C33 C28 117.3(5) . . ?
C20 C33 V1 141.2(3) . . ?
C32 C33 V1 59.8(3) . . ?
C28 C33 V1 72.1(3) . . ?
C47 C34 C35 121.5(5) . . ?
C47 C34 N3 118.9(5) . . ?
C35 C34 N3 119.6(5) . . ?
C34 C35 C36 122.7(5) . . ?
C34 C35 C40 118.3(5) . . ?
C36 C35 C40 119.0(6) . . ?
C37 C36 C35 120.4(6) . . ?
C37 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C36 C37 C38 121.5(6) . . ?
C36 C37 H37 119.2 . . ?
C38 C37 H37 119.2 . . ?
C39 C38 C37 119.6(6) . . ?
C39 C38 H38 120.2 . . ?
C37 C38 H38 120.2 . . ?
C38 C39 C40 121.6(6) . . ?
C38 C39 H39 119.2 . . ?
C40 C39 H39 119.2 . . ?
C41 C40 C39 122.3(5) . . ?
C41 C40 C35 119.8(5) . . ?
C39 C40 C35 117.9(6) . . ?
C40 C41 C42 121.4(5) . . ?
C40 C41 H41 119.3 . . ?
C42 C41 H41 119.3 . . ?
C41 C42 C43 121.0(5) . . ?
C41 C42 C47 119.4(5) . . ?
C43 C42 C47 119.6(6) . . ?
C44 C43 C42 120.3(6) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C45 120.9(6) . . ?
C43 C44 H44 119.5 . . ?
C45 C44 H44 119.5 . . ?
C46 C45 C44 120.2(6) . . ?
C46 C45 H45 119.9 . . ?
C44 C45 H45 119.9 . . ?
C45 C46 C47 121.4(6) . . ?
C45 C46 H46 119.3 . . ?
C47 C46 H46 119.3 . . ?
C34 C47 C46 122.9(5) . . ?
C34 C47 C42 119.5(5) . . ?
C46 C47 C42 117.6(5) . . ?
C49 C48 H48A 109.5 . . ?
C49 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C49 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N3 C49 C50 123.0(5) . . ?
N3 C49 C48 119.8(4) . . ?
C50 C49 C48 117.1(4) . . ?
C51 C50 C49 128.2(5) . . ?
C51 C50 H50 115.9 . . ?
C49 C50 H50 115.9 . . ?
N4 C51 C50 122.8(4) . . ?
N4 C51 C52 120.1(5) . . ?
C50 C51 C52 117.1(4) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C66 C53 C54 121.6(5) . . ?
C66 C53 N4 120.5(5) . 2_557 ?
C54 C53 N4 117.9(5) . 2_557 ?
C55 C54 C53 122.4(5) . . ?
C55 C54 C59 118.3(6) . . ?
C53 C54 C59 119.3(5) . . ?
C56 C55 C54 121.4(6) . . ?
C56 C55 H55 119.3 . . ?
C54 C55 H55 119.3 . . ?
C55 C56 C57 120.2(6) . . ?
C55 C56 H56 119.9 . . ?
C57 C56 H56 119.9 . . ?
C58 C57 C56 120.2(7) . . ?
C58 C57 H57 119.9 . . ?
C56 C57 H57 119.9 . . ?
C57 C58 C59 121.5(6) . . ?
C57 C58 H58 119.3 . . ?
C59 C58 H58 119.3 . . ?
C60 C59 C58 123.4(6) . . ?
C60 C59 C54 118.2(6) . . ?
C58 C59 C54 118.4(5) . . ?
C61 C60 C59 123.5(5) . . ?
C61 C60 H60 118.3 . . ?
C59 C60 H60 118.3 . . ?
C60 C61 C62 123.0(5) . . ?
C60 C61 C66 119.0(5) . . ?
C62 C61 C66 118.0(5) . . ?
C60 C61 V2 137.0(3) . . ?
C62 C61 V2 61.1(3) . . ?
C66 C61 V2 74.1(3) . . ?
C63 C62 C61 118.9(5) . . ?
C63 C62 V2 74.7(3) . . ?
C61 C62 V2 83.4(3) . . ?
C63 C62 H62 120.6 . . ?
C61 C62 H62 120.6 . . ?
V2 C62 H62 111.9 . . ?
C64 C63 C62 119.9(5) . . ?
C64 C63 V2 71.3(3) . . ?
C62 C63 V2 68.0(3) . . ?
C64 C63 H63 120.1 . . ?
C62 C63 H63 120.1 . . ?
V2 C63 H63 134.0 . . ?
C63 C64 C65 120.2(6) . . ?
C63 C64 V2 73.2(3) . . ?
C65 C64 V2 68.3(3) . . ?
C63 C64 H64 119.9 . . ?
C65 C64 H64 119.9 . . ?
V2 C64 H64 131.2 . . ?
C64 C65 C66 118.3(5) . . ?
C64 C65 V2 73.6(3) . . ?
C66 C65 V2 85.2(3) . . ?
C64 C65 H65 120.9 . . ?
C66 C65 H65 120.9 . . ?
V2 C65 H65 110.9 . . ?
C53 C66 C65 124.1(5) . . ?
C53 C66 C61 118.4(5) . . ?
C65 C66 C61 117.5(5) . . ?
C53 C66 V2 140.6(3) . . ?
C65 C66 V2 59.8(3) . . ?
C61 C66 V2 71.7(3) . . ?
C68 C67 H67A 109.5 . . ?
C68 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C68 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C67 C68 C69 110.8(11) . . ?
C67 C68 H68A 109.5 . . ?
C69 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
C69 C68 H68B 109.5 . . ?
H68A C68 H68B 108.1 . . ?
C70 C69 C68 108.9(10) . . ?
C70 C69 H69A 109.9 . . ?
C68 C69 H69A 109.9 . . ?
C70 C69 H69B 109.9 . . ?
C68 C69 H69B 109.9 . . ?
H69A C69 H69B 108.3 . . ?
C69 C70 C71 113.7(10) . . ?
C69 C70 H70A 108.8 . . ?
C71 C70 H70A 108.8 . . ?
C69 C70 H70B 108.8 . . ?
C71 C70 H70B 108.8 . . ?
H70A C70 H70B 107.7 . . ?
C72 C71 C70 106.9(9) . . ?
C72 C71 H71A 110.3 . . ?
C70 C71 H71A 110.3 . . ?
C72 C71 H71B 110.3 . . ?
C70 C71 H71B 110.3 . . ?
H71A C71 H71B 108.6 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C16 N1 C1 117.0(4) . . ?
C16 N1 V1 127.8(4) . . ?
C1 N1 V1 114.9(3) . . ?
C18 N2 C20 117.1(4) . 2_556 ?
C18 N2 V1 128.3(4) . . ?
C20 N2 V1 114.6(3) 2_556 . ?
C49 N3 C34 117.4(4) . . ?
C49 N3 V2 127.4(3) . . ?
C34 N3 V2 114.9(3) . . ?
C51 N4 C53 117.4(4) . 2_557 ?
C51 N4 V2 127.9(4) . . ?
C53 N4 V2 114.6(3) 2_557 . ?
N2 V1 N1 88.82(17) . . ?
N2 V1 C29 135.6(2) . . ?
N1 V1 C29 111.92(19) . . ?
N2 V1 C32 113.40(18) . . ?
N1 V1 C32 134.3(2) . . ?
C29 V1 C32 80.4(2) . . ?
N2 V1 C31 147.7(2) . . ?
N1 V1 C31 104.5(2) . . ?
C29 V1 C31 66.6(2) . . ?
C32 V1 C31 38.00(19) . . ?
N2 V1 C30 172.8(2) . . ?
N1 V1 C30 95.94(19) . . ?
C29 V1 C30 37.4(2) . . ?
C32 V1 C30 66.7(2) . . ?
C31 V1 C30 35.6(2) . . ?
N2 V1 C28 110.34(18) . . ?
N1 V1 C28 146.11(18) . . ?
C29 V1 C28 35.56(18) . . ?
C32 V1 C28 64.3(2) . . ?
C31 V1 C28 74.3(2) . . ?
C30 V1 C28 62.9(2) . . ?
N2 V1 C33 102.17(17) . . ?
N1 V1 C33 167.56(18) . . ?
C29 V1 C33 63.94(19) . . ?
C32 V1 C33 35.4(2) . . ?
C31 V1 C33 63.04(19) . . ?
C30 V1 C33 73.70(18) . . ?
C28 V1 C33 34.02(17) . . ?
N4 V2 N3 89.25(16) . . ?
N4 V2 C65 112.22(18) . . ?
N3 V2 C65 133.2(2) . . ?
N4 V2 C62 136.7(2) . . ?
N3 V2 C62 112.42(19) . . ?
C65 V2 C62 80.4(2) . . ?
N4 V2 C64 146.3(2) . . ?
N3 V2 C64 103.82(19) . . ?
C65 V2 C64 38.05(19) . . ?
C62 V2 C64 66.5(2) . . ?
N4 V2 C63 173.6(2) . . ?
N3 V2 C63 95.95(18) . . ?
C65 V2 C63 66.68(19) . . ?
C62 V2 C63 37.3(2) . . ?
C64 V2 C63 35.51(19) . . ?
N4 V2 C61 110.95(17) . . ?
N3 V2 C61 146.79(17) . . ?
C65 V2 C61 64.25(19) . . ?
C62 V2 C61 35.52(18) . . ?
C64 V2 C61 74.2(2) . . ?
C63 V2 C61 62.69(19) . . ?
N4 V2 C66 102.16(16) . . ?
N3 V2 C66 166.35(18) . . ?
C65 V2 C66 34.98(19) . . ?
C62 V2 C66 63.91(19) . . ?
C64 V2 C66 62.53(19) . . ?
C63 V2 C66 73.22(17) . . ?
C61 V2 C66 34.20(17) . . ?
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 1.390(8) . ?
C1 C14 1.414(8) . ?
C1 N1 1.443(6) . ?
C2 C3 1.420(8) . ?
C2 C7 1.433(7) . ?
C3 C4 1.346(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.421(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.340(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.426(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.390(8) . ?
C8 C9 1.394(8) . ?
C8 H8 0.9500 . ?
C9 C14 1.423(7) . ?
C9 C10 1.426(9) . ?
C10 C11 1.339(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.410(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.369(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.424(8) . ?
C13 H13 0.9500 . ?
C15 C16 1.514(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 N1 1.342(6) . ?
C16 C17 1.393(7) . ?
C17 C18 1.388(8) . ?
C17 H17 0.9500 . ?
C18 N2 1.335(6) . ?
C18 C19 1.519(7) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C33 1.396(7) . ?
C20 C21 1.403(8) . ?
C20 N2 1.437(7) 2_556 ?
C21 C22 1.422(8) . ?
C21 C26 1.433(8) . ?
C22 C23 1.364(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.397(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.358(9) . ?
C24 H24 0.9500 . ?
C25 C26 1.403(8) . ?
C25 H25 0.9500 . ?
C26 C27 1.402(8) . ?
C27 C28 1.373(8) . ?
C27 H27 0.9500 . ?
C28 C29 1.442(7) . ?
C28 C33 1.451(7) . ?
C28 V1 2.468(5) . ?
C29 C30 1.419(8) . ?
C29 V1 2.147(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.375(8) . ?
C30 V1 2.264(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.432(7) . ?
C31 V1 2.230(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.448(8) . ?
C32 V1 2.162(5) . ?
C32 H32 0.9500 . ?
C33 V1 2.491(5) . ?
C34 C47 1.395(8) . ?
C34 C35 1.410(8) . ?
C34 N3 1.439(6) . ?
C35 C36 1.413(8) . ?
C35 C40 1.442(7) . ?
C36 C37 1.364(8) . ?
C36 H36 0.9500 . ?
C37 C38 1.410(8) . ?
C37 H37 0.9500 . ?
C38 C39 1.359(9) . ?
C38 H38 0.9500 . ?
C39 C40 1.429(8) . ?
C39 H39 0.9500 . ?
C40 C41 1.389(8) . ?
C41 C42 1.400(8) . ?
C41 H41 0.9500 . ?
C42 C43 1.418(8) . ?
C42 C47 1.425(7) . ?
C43 C44 1.357(9) . ?
C43 H43 0.9500 . ?
C44 C45 1.400(8) . ?
C44 H44 0.9500 . ?
C45 C46 1.360(8) . ?
C45 H45 0.9500 . ?
C46 C47 1.421(8) . ?
C46 H46 0.9500 . ?
C48 C49 1.508(7) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 N3 1.341(6) . ?
C49 C50 1.398(7) . ?
C50 C51 1.387(7) . ?
C50 H50 0.9500 . ?
C51 N4 1.336(6) . ?
C51 C52 1.505(6) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C66 1.395(7) . ?
C53 C54 1.421(8) . ?
C53 N4 1.435(7) 2_557 ?
C54 C55 1.417(7) . ?
C54 C59 1.432(7) . ?
C55 C56 1.356(8) . ?
C55 H55 0.9500 . ?
C56 C57 1.417(9) . ?
C56 H56 0.9500 . ?
C57 C58 1.348(8) . ?
C57 H57 0.9500 . ?
C58 C59 1.421(8) . ?
C58 H58 0.9500 . ?
C59 C60 1.399(7) . ?
C60 C61 1.371(8) . ?
C60 H60 0.9500 . ?
C61 C62 1.441(7) . ?
C61 C66 1.459(7) . ?
C61 V2 2.465(5) . ?
C62 C63 1.420(8) . ?
C62 V2 2.172(5) . ?
C62 H62 0.9500 . ?
C63 C64 1.370(8) . ?
C63 V2 2.259(5) . ?
C63 H63 0.9500 . ?
C64 C65 1.435(7) . ?
C64 V2 2.234(5) . ?
C64 H64 0.9500 . ?
C65 C66 1.436(8) . ?
C65 V2 2.164(5) . ?
C65 H65 0.9500 . ?
C66 V2 2.496(5) . ?
C67 C68 1.416(14) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 C69 1.556(13) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C69 C70 1.497(13) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C70 C71 1.534(12) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C71 C72 1.412(13) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
N1 V1 2.025(4) . ?
N2 C20 1.437(7) 2_556 ?
N2 V1 2.020(4) . ?
N3 V2 2.024(4) . ?
N4 C53 1.435(7) 2_557 ?
N4 V2 2.023(4) . ?
