#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/79/2227906.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_2227906
loop_
_publ_author_name
'Bian, Lin'
'Li, Lianzhi'
'Zhang, Qingfu'
'Wang, Daqi'
_publ_section_title
;
 Oxido{N-[(2-oxido-1-naphthyl-κO)methylidene]asparaginato-κ²O¹,N²}(1,10-phenanthroline-κ²N,N')vanadium(IV)
 N,N-dimethylformamide monosolvate
;
_journal_coeditor_code           PV2309
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1051
_journal_paper_doi               10.1107/S1600536810030126
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[V (C15 H12 N2 O4) O (C12 H8 N2)], C3 H7 N O'
_chemical_formula_moiety         'C27 H20 N4 O5 V, C3 H7 N O'
_chemical_formula_sum            'C30 H27 N5 O6 V'
_chemical_formula_weight         604.51
_chemical_name_systematic
;
Oxido{N-[(2-oxido-1-naphthyl-κO)methylidene]asparaginato-
κ²O¹,N²}(1,10-phenanthroline-
κ²N,N')vanadium(IV) N,N-dimethylformamide
monosolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.396(2)
_cell_angle_beta                 104.196(2)
_cell_angle_gamma                91.0100(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3570(10)
_cell_length_b                   11.1021(12)
_cell_length_c                   12.9119(14)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.694
_cell_measurement_theta_min      2.238
_cell_volume                     1407.5(3)
_computing_cell_refinement       'SAINT (Bruker, 1996)'
_computing_data_collection       'SMART (Bruker, 1996)'
_computing_data_reduction        'SAINT (Bruker, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0826
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7387
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_T_max  0.9054
_exptl_absorpt_correction_T_min  0.8677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             626
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.404
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         4892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0745
_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)+(0.130P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.2162
_reflns_number_gt                3123
_reflns_number_total             4892
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pv2309.cif
_cod_data_source_block           I
_cod_database_code               2227906
_cod_database_fobs_code          2227906
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V V1 0.21794(8) 0.72939(7) 0.12980(6) 0.0417(3) Uani d . 1 . .
N N1 -0.0395(4) 0.8528(4) 0.4060(3) 0.0547(11) Uani d . 1 . .
H H1A -0.0235 0.8842 0.4747 0.066 Uiso calc R 1 . .
H H1B -0.0620 0.7755 0.3824 0.066 Uiso calc R 1 . .
N N2 0.1611(3) 0.9001(3) 0.1906(3) 0.0381(8) Uani d . 1 . .
N N3 0.2777(3) 0.5734(3) 0.0261(3) 0.0402(9) Uani d . 1 . .
N N4 0.2988(4) 0.8051(3) -0.0030(3) 0.0435(9) Uani d . 1 . .
N N5 0.0667(5) 0.5958(5) 0.6803(4) 0.0717(13) Uani d . 1 . .
O O1 0.0481(3) 0.7362(3) 0.0169(3) 0.0495(8) Uani d . 1 . .
O O2 -0.1224(3) 0.8505(3) -0.0363(3) 0.0579(9) Uani d . 1 . .
O O3 0.0023(4) 1.0347(3) 0.3643(3) 0.0595(10) Uani d . 1 . .
O O4 0.4011(3) 0.7907(3) 0.2145(2) 0.0446(8) Uani d . 1 . .
O O5 0.1758(3) 0.6444(3) 0.2031(3) 0.0547(9) Uani d . 1 . .
O O6 0.1289(5) 0.4015(4) 0.6468(5) 0.1162(19) Uani d . 1 . .
C C1 -0.0249(5) 0.8286(4) 0.0315(4) 0.0453(11) Uani d . 1 . .
C C2 0.0166(4) 0.9110(4) 0.1475(3) 0.0392(10) Uani d . 1 . .
H H2 -0.0025 0.9968 0.1456 0.047 Uiso calc R 1 . .
C C3 -0.0627(5) 0.8583(4) 0.2161(4) 0.0459(11) Uani d . 1 . .
H H3A -0.1572 0.8630 0.1844 0.055 Uiso calc R 1 . .
H H3B -0.0462 0.7720 0.2120 0.055 Uiso calc R 1 . .
C C4 -0.0294(4) 0.9237(4) 0.3364(4) 0.0438(11) Uani d . 1 . .
C C5 0.2340(4) 0.9935(4) 0.2540(4) 0.0384(10) Uani d . 1 . .
H H5 0.1917 1.0660 0.2675 0.046 Uiso calc R 1 . .
C C6 0.3739(4) 0.9979(4) 0.3061(3) 0.0393(10) Uani d . 1 . .
C C7 0.4499(4) 0.8934(4) 0.2841(3) 0.0390(10) Uani d . 1 . .
C C8 0.5882(5) 0.9024(4) 0.3411(4) 0.0466(11) Uani d . 1 . .
H H8 0.6386 0.8353 0.3277 0.056 Uiso calc R 1 . .
C C9 0.6482(5) 1.0049(5) 0.4137(4) 0.0494(12) Uani d . 1 . .
H H9 0.7383 1.0060 0.4487 0.059 Uiso calc R 1 . .
C C10 0.5767(5) 1.1125(4) 0.4385(4) 0.0447(11) Uani d . 1 . .
C C11 0.4386(5) 1.1087(4) 0.3848(4) 0.0431(11) Uani d . 1 . .
C C12 0.3706(5) 1.2158(4) 0.4134(4) 0.0549(13) Uani d . 1 . .
H H12 0.2802 1.2173 0.3804 0.066 Uiso calc R 1 . .
C C13 0.4364(6) 1.3169(5) 0.4890(4) 0.0613(14) Uani d . 1 . .
H H13 0.3892 1.3854 0.5061 0.074 Uiso calc R 1 . .
C C14 0.5722(6) 1.3197(5) 0.5408(4) 0.0623(14) Uani d . 1 . .
H H14 0.6152 1.3894 0.5910 0.075 Uiso calc R 1 . .
C C15 0.6402(5) 1.2186(5) 0.5165(4) 0.0546(13) Uani d . 1 . .
H H15 0.7301 1.2190 0.5517 0.065 Uiso calc R 1 . .
C C16 0.2636(5) 0.4573(4) 0.0400(4) 0.0464(11) Uani d . 1 . .
H H16 0.2234 0.4435 0.0940 0.056 Uiso calc R 1 . .
C C17 0.3071(5) 0.3567(4) -0.0233(4) 0.0538(13) Uani d . 1 . .
H H17 0.2967 0.2778 -0.0109 0.065 Uiso calc R 1 . .
C C18 0.3653(5) 0.3757(5) -0.1039(4) 0.0540(13) Uani d . 1 . .
H H18 0.3962 0.3096 -0.1453 0.065 Uiso calc R 1 . .
C C19 0.3785(4) 0.4939(4) -0.1242(4) 0.0472(12) Uani d . 1 . .
C C20 0.3325(4) 0.5912(4) -0.0556(4) 0.0416(11) Uani d . 1 . .
C C21 0.3453(4) 0.7150(4) -0.0716(4) 0.0424(11) Uani d . 1 . .
C C22 0.4021(5) 0.7404(5) -0.1544(4) 0.0532(12) Uani d . 1 . .
C C23 0.4084(5) 0.8629(5) -0.1670(4) 0.0618(14) Uani d . 1 . .
H H23 0.4442 0.8831 -0.2212 0.074 Uiso calc R 1 . .
C C24 0.3612(5) 0.9528(5) -0.0986(4) 0.0632(14) Uani d . 1 . .
H H24 0.3659 1.0345 -0.1055 0.076 Uiso calc R 1 . .
C C25 0.3058(5) 0.9198(4) -0.0182(4) 0.0516(12) Uani d . 1 . .
H H25 0.2725 0.9811 0.0264 0.062 Uiso calc R 1 . .
C C26 0.4361(5) 0.5229(5) -0.2071(4) 0.0609(14) Uani d . 1 . .
H H26 0.4671 0.4599 -0.2518 0.073 Uiso calc R 1 . .
C C27 0.4466(5) 0.6385(6) -0.2220(4) 0.0629(15) Uani d . 1 . .
H H27 0.4836 0.6534 -0.2775 0.076 Uiso calc R 1 . .
C C28 0.0719(10) 0.4856(9) 0.7005(9) 0.078(3) Uani d P 0.732(13) A 1
H H28 0.0342 0.4672 0.7543 0.094 Uiso calc PR 0.732(13) A 1
C C29 0.1211(12) 0.6333(11) 0.5983(8) 0.102(4) Uani d P 0.732(13) A 1
H H29A 0.1869 0.5782 0.5812 0.153 Uiso calc PR 0.732(13) A 1
H H29B 0.1620 0.7155 0.6253 0.153 Uiso calc PR 0.732(13) A 1
H H29C 0.0508 0.6313 0.5336 0.153 Uiso calc PR 0.732(13) A 1
C C30 0.0016(13) 0.6932(11) 0.7444(10) 0.116(5) Uani d P 0.732(13) A 1
H H30A -0.0315 0.6592 0.7965 0.174 Uiso calc PR 0.732(13) A 1
H H30B -0.0711 0.7220 0.6956 0.174 Uiso calc PR 0.732(13) A 1
H H30C 0.0659 0.7608 0.7822 0.174 Uiso calc PR 0.732(13) A 1
C C28' 0.140(3) 0.508(2) 0.619(2) 0.085(9) Uani d P 0.268(13) A 2
H H28' 0.1863 0.5244 0.5694 0.102 Uiso calc PR 0.268(13) A 2
C C29' -0.006(3) 0.544(3) 0.737(3) 0.103(11) Uani d P 0.268(13) A 2
H H29D -0.0919 0.5131 0.6904 0.155 Uiso calc PR 0.268(13) A 2
H H29E -0.0175 0.6058 0.7977 0.155 Uiso calc PR 0.268(13) A 2
H H29F 0.0401 0.4783 0.7646 0.155 Uiso calc PR 0.268(13) A 2
C C30' 0.058(3) 0.710(3) 0.657(3) 0.107(11) Uani d P 0.268(13) A 2
H H30D 0.0192 0.7028 0.5802 0.161 Uiso calc PR 0.268(13) A 2
H H30E 0.1457 0.7508 0.6764 0.161 Uiso calc PR 0.268(13) A 2
H H30F 0.0031 0.7568 0.6977 0.161 Uiso calc PR 0.268(13) A 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'
O O 0.0106 0.0060 '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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O5 V1 O4 . . 101.87(16) ?
O5 V1 O1 . . 103.57(16) ?
O4 V1 O1 . . 153.16(14) ?
O5 V1 N2 . . 103.66(15) ?
O4 V1 N2 . . 86.43(13) ?
O1 V1 N2 . . 79.44(13) ?
O5 V1 N3 . . 91.99(15) ?
O4 V1 N3 . . 95.45(12) ?
O1 V1 N3 . . 92.06(13) ?
N2 V1 N3 . . 163.53(14) ?
O5 V1 N4 . . 164.43(15) ?
O4 V1 N4 . . 79.26(13) ?
O1 V1 N4 . . 78.54(13) ?
N2 V1 N4 . . 91.91(13) ?
N3 V1 N4 . . 72.46(13) ?
C4 N1 H1A . . 120.0 ?
C4 N1 H1B . . 120.0 ?
H1A N1 H1B . . 120.0 ?
C5 N2 C2 . . 119.5(4) ?
C5 N2 V1 . . 128.8(3) ?
C2 N2 V1 . . 111.7(2) ?
C16 N3 C20 . . 117.8(4) ?
C16 N3 V1 . . 122.2(3) ?
C20 N3 V1 . . 120.0(3) ?
C25 N4 C21 . . 117.7(4) ?
C25 N4 V1 . . 129.1(3) ?
C21 N4 V1 . . 113.2(3) ?
C28 N5 C30' . . 178.4(15) ?
C28 N5 C29' . . 52.5(14) ?
C30' N5 C29' . . 127(2) ?
C28 N5 C29 . . 123.9(9) ?
C30' N5 C29 . . 56.0(15) ?
C29' N5 C29 . . 166.6(15) ?
C28 N5 C28' . . 63.0(11) ?
C30' N5 C28' . . 117.0(19) ?
C29' N5 C28' . . 114.5(18) ?
C29 N5 C28' . . 61.0(11) ?
C28 N5 C30 . . 120.2(9) ?
C30' N5 C30 . . 59.9(16) ?
C29' N5 C30 . . 69.4(15) ?
C29 N5 C30 . . 115.9(9) ?
C28' N5 C30 . . 175.2(12) ?
C1 O1 V1 . . 119.2(3) ?
C7 O4 V1 . . 132.7(3) ?
C28 O6 C28' . . 68.3(13) ?
O2 C1 O1 . . 125.4(4) ?
O2 C1 C2 . . 120.4(4) ?
O1 C1 C2 . . 114.2(4) ?
N2 C2 C3 . . 110.1(4) ?
N2 C2 C1 . . 107.0(3) ?
C3 C2 C1 . . 106.6(3) ?
N2 C2 H2 . . 111.0 ?
C3 C2 H2 . . 111.0 ?
C1 C2 H2 . . 111.0 ?
C4 C3 C2 . . 114.5(4) ?
C4 C3 H3A . . 108.6 ?
C2 C3 H3A . . 108.6 ?
C4 C3 H3B . . 108.6 ?
C2 C3 H3B . . 108.6 ?
H3A C3 H3B . . 107.6 ?
O3 C4 N1 . . 123.5(4) ?
O3 C4 C3 . . 121.1(4) ?
N1 C4 C3 . . 115.4(4) ?
N2 C5 C6 . . 126.9(4) ?
N2 C5 H5 . . 116.6 ?
C6 C5 H5 . . 116.6 ?
C7 C6 C5 . . 120.7(4) ?
C7 C6 C11 . . 119.7(4) ?
C5 C6 C11 . . 119.6(4) ?
O4 C7 C8 . . 118.0(4) ?
O4 C7 C6 . . 124.1(4) ?
C8 C7 C6 . . 117.9(4) ?
C9 C8 C7 . . 122.5(4) ?
C9 C8 H8 . . 118.8 ?
C7 C8 H8 . . 118.8 ?
C8 C9 C10 . . 121.9(5) ?
C8 C9 H9 . . 119.1 ?
C10 C9 H9 . . 119.1 ?
C15 C10 C11 . . 120.5(4) ?
C15 C10 C9 . . 121.3(5) ?
C11 C10 C9 . . 118.2(4) ?
C10 C11 C12 . . 116.6(4) ?
C10 C11 C6 . . 119.8(4) ?
C12 C11 C6 . . 123.6(4) ?
C13 C12 C11 . . 121.0(5) ?
C13 C12 H12 . . 119.5 ?
C11 C12 H12 . . 119.5 ?
C12 C13 C14 . . 121.9(5) ?
C12 C13 H13 . . 119.1 ?
C14 C13 H13 . . 119.1 ?
C15 C14 C13 . . 118.8(5) ?
C15 C14 H14 . . 120.6 ?
C13 C14 H14 . . 120.6 ?
C14 C15 C10 . . 121.3(5) ?
C14 C15 H15 . . 119.4 ?
C10 C15 H15 . . 119.4 ?
N3 C16 C17 . . 122.6(4) ?
N3 C16 H16 . . 118.7 ?
C17 C16 H16 . . 118.7 ?
C18 C17 C16 . . 119.3(5) ?
C18 C17 H17 . . 120.4 ?
C16 C17 H17 . . 120.4 ?
C17 C18 C19 . . 120.5(4) ?
C17 C18 H18 . . 119.8 ?
C19 C18 H18 . . 119.8 ?
C18 C19 C20 . . 116.8(4) ?
C18 C19 C26 . . 124.7(4) ?
C20 C19 C26 . . 118.6(5) ?
N3 C20 C19 . . 123.1(4) ?
N3 C20 C21 . . 117.7(4) ?
C19 C20 C21 . . 119.2(4) ?
N4 C21 C22 . . 122.7(4) ?
N4 C21 C20 . . 116.5(4) ?
C22 C21 C20 . . 120.8(4) ?
C23 C22 C21 . . 117.7(5) ?
C23 C22 C27 . . 124.4(5) ?
C21 C22 C27 . . 117.9(5) ?
C24 C23 C22 . . 119.6(5) ?
C24 C23 H23 . . 120.2 ?
C22 C23 H23 . . 120.2 ?
C23 C24 C25 . . 119.2(5) ?
C23 C24 H24 . . 120.4 ?
C25 C24 H24 . . 120.4 ?
N4 C25 C24 . . 123.1(5) ?
N4 C25 H25 . . 118.4 ?
C24 C25 H25 . . 118.4 ?
C27 C26 C19 . . 121.8(5) ?
C27 C26 H26 . . 119.1 ?
C19 C26 H26 . . 119.1 ?
C26 C27 C22 . . 121.7(5) ?
C26 C27 H27 . . 119.1 ?
C22 C27 H27 . . 119.1 ?
O6 C28 N5 . . 120.8(9) ?
O6 C28 H28 . . 119.6 ?
N5 C28 H28 . . 119.6 ?
N5 C29 H29A . . 109.5 ?
N5 C29 H29B . . 109.5 ?
N5 C29 H29C . . 109.5 ?
N5 C30 H30A . . 109.5 ?
N5 C30 H30B . . 109.5 ?
N5 C30 H30C . . 109.5 ?
O6 C28' N5 . . 107.7(19) ?
O6 C28' H28' . . 126.1 ?
N5 C28' H28' . . 126.1 ?
N5 C29' H29D . . 109.5 ?
N5 C29' H29E . . 109.5 ?
H29D C29' H29E . . 109.5 ?
N5 C29' H29F . . 109.5 ?
H29D C29' H29F . . 109.5 ?
H29E C29' H29F . . 109.5 ?
N5 C30' H30D . . 109.5 ?
N5 C30' H30E . . 109.5 ?
H30D C30' H30E . . 109.5 ?
N5 C30' H30F . . 109.5 ?
H30D C30' H30F . . 109.5 ?
H30E C30' H30F . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 O5 . 1.587(3) ?
V1 O4 . 1.975(3) ?
V1 O1 . 2.004(3) ?
V1 N2 . 2.057(3) ?
V1 N3 . 2.168(3) ?
V1 N4 . 2.366(4) ?
N1 C4 . 1.326(6) ?
N1 H1A . 0.8600 ?
N1 H1B . 0.8600 ?
N2 C5 . 1.284(5) ?
N2 C2 . 1.480(5) ?
N3 C16 . 1.346(5) ?
N3 C20 . 1.359(5) ?
N4 C25 . 1.329(6) ?
N4 C21 . 1.376(6) ?
N5 C28 . 1.299(10) ?
N5 C30' . 1.36(3) ?
N5 C29' . 1.36(3) ?
N5 C29 . 1.439(11) ?
N5 C28' . 1.48(3) ?
N5 C30 . 1.503(11) ?
O1 C1 . 1.297(5) ?
O2 C1 . 1.226(6) ?
O3 C4 . 1.228(5) ?
O4 C7 . 1.310(5) ?
O6 C28 . 1.290(12) ?
O6 C28' . 1.31(3) ?
C1 C2 . 1.547(6) ?
C2 C3 . 1.531(6) ?
C2 H2 . 0.9800 ?
C3 C4 . 1.530(6) ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C5 C6 . 1.436(6) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.435(6) ?
C6 C11 . 1.462(6) ?
C7 C8 . 1.432(6) ?
C8 C9 . 1.352(6) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.440(7) ?
C9 H9 . 0.9300 ?
C10 C15 . 1.419(6) ?
C10 C11 . 1.424(6) ?
C11 C12 . 1.424(7) ?
C12 C13 . 1.375(7) ?
C12 H12 . 0.9300 ?
C13 C14 . 1.398(7) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.361(7) ?
C14 H14 . 0.9300 ?
C15 H15 . 0.9300 ?
C16 C17 . 1.399(6) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.370(7) ?
C17 H17 . 0.9300 ?
C18 C19 . 1.398(7) ?
C18 H18 . 0.9300 ?
C19 C20 . 1.423(6) ?
C19 C26 . 1.432(7) ?
C20 C21 . 1.438(6) ?
C21 C22 . 1.410(6) ?
C22 C23 . 1.403(7) ?
C22 C27 . 1.443(7) ?
C23 C24 . 1.377(7) ?
C23 H23 . 0.9300 ?
C24 C25 . 1.406(7) ?
C24 H24 . 0.9300 ?
C25 H25 . 0.9300 ?
C26 C27 . 1.342(8) ?
C26 H26 . 0.9300 ?
C27 H27 . 0.9300 ?
C28 H28 . 0.9300 ?
C29 H29A . 0.9600 ?
C29 H29B . 0.9600 ?
C29 H29C . 0.9600 ?
C30 H30A . 0.9600 ?
C30 H30B . 0.9600 ?
C30 H30C . 0.9600 ?
C28' H28' . 0.9300 ?
C29' H29D . 0.9600 ?
C29' H29E . 0.9600 ?
C29' H29F . 0.9600 ?
C30' H30D . 0.9600 ?
C30' H30E . 0.9600 ?
C30' H30F . 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1A O3 2_576 0.86 2.05 2.909(5) 175 y
N1 H1B O6 2_566 0.86 2.00 2.852(6) 169 y
C16 H16 O5 . 0.93 2.52 2.975(5) 111 ?
C29 H29A O6 . 0.96 2.41 2.764(11) 102 ?
C29 H29C O6 2_566 0.96 2.56 3.511(12) 173 ?
C25 H25 O2 2_575 0.93 2.46 3.275(6) 147 ?
C17 H17 O2 2_565 0.93 2.54 3.288(6) 138 ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O5 V1 N2 C5 . . . . 102.7(4) ?
O4 V1 N2 C5 . . . . 1.4(4) ?
O1 V1 N2 C5 . . . . -155.7(4) ?
N3 V1 N2 C5 . . . . -95.8(6) ?
N4 V1 N2 C5 . . . . -77.7(4) ?
O5 V1 N2 C2 . . . . -80.4(3) ?
O4 V1 N2 C2 . . . . 178.3(3) ?
O1 V1 N2 C2 . . . . 21.2(3) ?
N3 V1 N2 C2 . . . . 81.1(5) ?
N4 V1 N2 C2 . . . . 99.2(3) ?
O5 V1 N3 C16 . . . . 2.5(4) ?
O4 V1 N3 C16 . . . . 104.7(3) ?
O1 V1 N3 C16 . . . . -101.1(4) ?
N2 V1 N3 C16 . . . . -159.5(4) ?
N4 V1 N3 C16 . . . . -178.4(4) ?
O5 V1 N3 C20 . . . . -176.8(3) ?
O4 V1 N3 C20 . . . . -74.7(3) ?
O1 V1 N3 C20 . . . . 79.5(3) ?
N2 V1 N3 C20 . . . . 21.2(7) ?
N4 V1 N3 C20 . . . . 2.2(3) ?
O5 V1 N4 C25 . . . . -178.2(6) ?
O4 V1 N4 C25 . . . . -82.5(4) ?
O1 V1 N4 C25 . . . . 82.3(4) ?
N2 V1 N4 C25 . . . . 3.5(4) ?
N3 V1 N4 C25 . . . . 178.2(4) ?
O5 V1 N4 C21 . . . . 1.1(8) ?
O4 V1 N4 C21 . . . . 96.8(3) ?
O1 V1 N4 C21 . . . . -98.4(3) ?
N2 V1 N4 C21 . . . . -177.2(3) ?
N3 V1 N4 C21 . . . . -2.5(3) ?
O5 V1 O1 C1 . . . . 96.2(3) ?
O4 V1 O1 C1 . . . . -64.9(4) ?
N2 V1 O1 C1 . . . . -5.5(3) ?
N3 V1 O1 C1 . . . . -171.3(3) ?
N4 V1 O1 C1 . . . . -99.6(3) ?
O5 V1 O4 C7 . . . . -97.9(4) ?
O1 V1 O4 C7 . . . . 63.3(5) ?
N2 V1 O4 C7 . . . . 5.3(4) ?
N3 V1 O4 C7 . . . . 168.9(4) ?
N4 V1 O4 C7 . . . . 98.0(4) ?
V1 O1 C1 O2 . . . . 171.5(4) ?
V1 O1 C1 C2 . . . . -11.2(5) ?
C5 N2 C2 C3 . . . . -98.3(4) ?
V1 N2 C2 C3 . . . . 84.5(3) ?
C5 N2 C2 C1 . . . . 146.2(4) ?
V1 N2 C2 C1 . . . . -31.0(4) ?
O2 C1 C2 N2 . . . . -155.0(4) ?
O1 C1 C2 N2 . . . . 27.5(5) ?
O2 C1 C2 C3 . . . . 87.2(5) ?
O1 C1 C2 C3 . . . . -90.3(4) ?
N2 C2 C3 C4 . . . . 61.0(5) ?
C1 C2 C3 C4 . . . . 176.7(4) ?
C2 C3 C4 O3 . . . . 33.3(6) ?
C2 C3 C4 N1 . . . . -147.8(4) ?
C2 N2 C5 C6 . . . . 177.5(4) ?
V1 N2 C5 C6 . . . . -5.9(6) ?
N2 C5 C6 C7 . . . . 4.5(6) ?
N2 C5 C6 C11 . . . . -173.8(4) ?
V1 O4 C7 C8 . . . . 172.9(3) ?
V1 O4 C7 C6 . . . . -7.7(6) ?
C5 C6 C7 O4 . . . . 2.3(6) ?
C11 C6 C7 O4 . . . . -179.4(4) ?
C5 C6 C7 C8 . . . . -178.3(4) ?
C11 C6 C7 C8 . . . . 0.0(6) ?
O4 C7 C8 C9 . . . . 179.3(4) ?
C6 C7 C8 C9 . . . . -0.1(6) ?
C7 C8 C9 C10 . . . . -0.1(7) ?
C8 C9 C10 C15 . . . . 178.7(4) ?
C8 C9 C10 C11 . . . . 0.6(7) ?
C15 C10 C11 C12 . . . . 0.4(6) ?
C9 C10 C11 C12 . . . . 178.5(4) ?
C15 C10 C11 C6 . . . . -178.9(4) ?
C9 C10 C11 C6 . . . . -0.7(6) ?
C7 C6 C11 C10 . . . . 0.4(6) ?
C5 C6 C11 C10 . . . . 178.7(4) ?
C7 C6 C11 C12 . . . . -178.7(4) ?
C5 C6 C11 C12 . . . . -0.5(6) ?
C10 C11 C12 C13 . . . . 0.1(7) ?
C6 C11 C12 C13 . . . . 179.3(4) ?
C11 C12 C13 C14 . . . . 0.1(8) ?
C12 C13 C14 C15 . . . . -0.8(8) ?
C13 C14 C15 C10 . . . . 1.3(7) ?
C11 C10 C15 C14 . . . . -1.1(7) ?
C9 C10 C15 C14 . . . . -179.2(5) ?
C20 N3 C16 C17 . . . . 2.2(7) ?
V1 N3 C16 C17 . . . . -177.2(3) ?
N3 C16 C17 C18 . . . . -0.7(7) ?
C16 C17 C18 C19 . . . . -1.4(7) ?
C17 C18 C19 C20 . . . . 1.7(7) ?
C17 C18 C19 C26 . . . . -179.2(4) ?
C16 N3 C20 C19 . . . . -1.8(6) ?
V1 N3 C20 C19 . . . . 177.6(3) ?
C16 N3 C20 C21 . . . . 178.9(4) ?
V1 N3 C20 C21 . . . . -1.7(5) ?
C18 C19 C20 N3 . . . . -0.1(7) ?
C26 C19 C20 N3 . . . . -179.3(4) ?
C18 C19 C20 C21 . . . . 179.1(4) ?
C26 C19 C20 C21 . . . . 0.0(7) ?
C25 N4 C21 C22 . . . . 1.6(6) ?
V1 N4 C21 C22 . . . . -177.8(3) ?
C25 N4 C21 C20 . . . . -178.0(4) ?
V1 N4 C21 C20 . . . . 2.6(5) ?
N3 C20 C21 N4 . . . . -0.8(6) ?
C19 C20 C21 N4 . . . . 179.9(4) ?
N3 C20 C21 C22 . . . . 179.6(4) ?
C19 C20 C21 C22 . . . . 0.3(7) ?
N4 C21 C22 C23 . . . . -1.1(7) ?
C20 C21 C22 C23 . . . . 178.5(4) ?
N4 C21 C22 C27 . . . . -179.6(4) ?
C20 C21 C22 C27 . . . . 0.0(7) ?
C21 C22 C23 C24 . . . . 0.7(8) ?
C27 C22 C23 C24 . . . . 179.1(5) ?
C22 C23 C24 C25 . . . . -0.9(8) ?
C21 N4 C25 C24 . . . . -1.7(7) ?
V1 N4 C25 C24 . . . . 177.6(4) ?
C23 C24 C25 N4 . . . . 1.4(8) ?
C18 C19 C26 C27 . . . . -179.6(5) ?
C20 C19 C26 C27 . . . . -0.5(7) ?
C19 C26 C27 C22 . . . . 0.9(8) ?
C23 C22 C27 C26 . . . . -178.9(5) ?
C21 C22 C27 C26 . . . . -0.6(8) ?
C28' O6 C28 N5 . . . . 3.5(14) ?
C29' N5 C28 O6 . . . . 165(2) ?
C29 N5 C28 O6 . . . . 0.5(13) ?
C28' N5 C28 O6 . . . . -3.2(13) ?
C30 N5 C28 O6 . . . . -179.2(8) ?
C28 O6 C28' N5 . . . . -2.8(11) ?
C28 N5 C28' O6 . . . . 2.9(11) ?
C30' N5 C28' O6 . . . . -175.3(18) ?
C29' N5 C28' O6 . . . . -8(2) ?
C29 N5 C28' O6 . . . . -174(2) ?
