#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:59:13 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229743 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/56/7045682.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_7045682
loop_
_publ_author_name
'Konarev, Dmitri V.'
'Kuzmin, Alexey V.'
'Nakano, Yoshiaki'
'Khasanov, Salavat S.'
'Otsuka, Akihiro'
'Yamochi, Hideki'
'Kitagawa, Hiroshi'
'Lyubovskaya, Rimma N.'
_publ_section_title
;
 Synthesis and properties of N-methylimidazole solvates of vanadium(ii),
 chromium(ii) and iron(ii) phthalocyanines. Strong NIR absorption in
 VII(MeIm)₂(Pc²⁻).
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4661
_journal_page_last               4671
_journal_paper_doi               10.1039/c8dt00459e
_journal_volume                  47
_journal_year                    2018
_chemical_compound_source        no
_chemical_formula_moiety         '2(C20 H14 N6 V0.5), C4 H6 N2'
_chemical_formula_sum            'C44 H34 N14 V'
_chemical_formula_weight         809.79
_chemical_melting_point          ?
_chemical_name_common            no
_chemical_name_systematic
'N-methylimidazole complex of vanadium(II) phthalocyanine, N-methylimidazole solvate'
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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
_audit_creation_date             2017-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2018-02-19 deposited with the CCDC.
2018-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.715(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1243(6)
_cell_length_b                   11.2003(2)
_cell_length_c                   18.9602(5)
_cell_measurement_reflns_used    12840
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.1450
_cell_measurement_theta_min      2.1380
_cell_volume                     3823.17(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00  22.00   1.00   64.00    --  -12.05 -99.00 120.00   47
  2  ω    -87.00 -57.00   1.00   64.00    --  -12.05 -37.00 120.00   30
  3  ω    -24.00   9.00   1.00   64.00    --  -12.05 -37.00 120.00   33
  4  ω    -13.00  29.00   1.00   64.00    --  -12.05 -99.00 -90.00   42
  5  ω    -16.00  10.00   1.00   64.00    --  -12.05  37.00   0.00   26
  6  ω     13.00  56.00   1.00   64.00    --  -12.05  37.00   0.00   43
  7  ω    -38.00  33.00   1.00   64.00    --  -12.05  57.00  90.00   71
  8  ω    -30.00  62.00   1.00   64.00    --  -12.05  57.00 -90.00   92
  9  ω    -92.00 -60.00   1.00   64.00    --  -12.05-178.00 -90.00   32
 10  ω    -63.00 -37.00   1.00   64.00    --  -12.05 -19.00-120.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0315996000
_diffrn_orient_matrix_UB_12      -0.0153983000
_diffrn_orient_matrix_UB_13      -0.0096332000
_diffrn_orient_matrix_UB_21      0.0184523000
_diffrn_orient_matrix_UB_22      -0.0197035000
_diffrn_orient_matrix_UB_23      0.0372317000
_diffrn_orient_matrix_UB_31      -0.0145984000
_diffrn_orient_matrix_UB_32      -0.0581901000
_diffrn_orient_matrix_UB_33      -0.0100429000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45443
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.545
_diffrn_reflns_theta_min         2.141
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       block
_exptl_crystal_F_000             1676
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: o-dichlorobenzene/n-hexane/N-methylimidzole'
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         9733
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0395P)²+2.7602P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6895
_reflns_number_total             9733
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt00459e2.cif
_cod_data_source_block           VMeIm2PcMeIm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7045682--7045685.cif.
;
_cod_database_code               7045682
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C44 H34 N14 V '
_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.
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C604) = Uanis(C504)
Uanis(N602) = Uanis(N502)
Uanis(C601) = Uanis(C501)
Uanis(C603) = Uanis(C503)
Uanis(C602) = Uanis(C502)
Uanis(N601) = Uanis(N501)
3. Same fragment restrains
{N501, N502, C501, C502, C503, C504} sigma for 1-2: 0.001, 1-3: 0.001
as
{N601, N602, C601, C602, C603, C604}
4. Others
 Sof(N601)=Sof(N602)=Sof(C601)=Sof(H601)=Sof(C602)=Sof(H602)=Sof(C603)=
 Sof(H603)=Sof(C604)=Sof(H60A)=Sof(H60B)=Sof(H60C)=1-FVAR(1)
 Sof(N501)=Sof(N502)=Sof(C501)=Sof(H501)=Sof(C502)=Sof(H502)=Sof(C503)=
 Sof(H503)=Sof(C504)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C209(H209), C210(H210), C211(H211), C212(H212), C213(H213), C214(H214),
 C215(H215), C216(H216), C401(H401), C402(H402), C403(H403), C109(H109),
 C110(H110), C111(H111), C112(H112), C113(H113), C114(H114), C115(H115),
 C116(H116), C301(H301), C302(H302), C303(H303), C501(H501), C502(H502),
 C503(H503), C601(H601), C602(H602), C603(H603)
5.b Idealised Me refined as rotating group:
 C404(H40A,H40B,H40C), C304(H30A,H30B,H30C), C504(H50A,H50B,H50C), C604(H60A,
 H60B,H60C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.100
_oxdiff_exptl_absorpt_empirical_full_min 0.885
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
V0AA V 0.500000 0.000000 0.500000 0.01643(10) Uani 1 2 d S T P . .
N201 N 0.50849(8) 0.01817(13) 0.39816(8) 0.0180(3) Uani 1 1 d . . . . .
N202 N 0.41802(8) 0.11984(13) 0.47283(8) 0.0184(3) Uani 1 1 d . . . . .
N203 N 0.41150(8) 0.16618(13) 0.34465(8) 0.0198(3) Uani 1 1 d . . . . .
N204 N 0.39506(8) 0.13000(13) 0.59172(8) 0.0193(3) Uani 1 1 d . . . . .
N401 N 0.42511(9) -0.14661(14) 0.45736(9) 0.0219(3) Uani 1 1 d . . . . .
N402 N 0.34512(9) -0.26894(14) 0.37880(9) 0.0273(4) Uani 1 1 d . . . . .
C201 C 0.54125(10) -0.01587(15) 0.29318(10) 0.0189(4) Uani 1 1 d . . . . .
C202 C 0.48614(10) 0.07408(15) 0.27487(10) 0.0187(4) Uani 1 1 d . . . . .
C203 C 0.46528(10) 0.09208(16) 0.34148(10) 0.0187(4) Uani 1 1 d . . . . .
C204 C 0.39077(10) 0.17929(15) 0.40507(10) 0.0189(4) Uani 1 1 d . . . . .
C205 C 0.33410(10) 0.26407(16) 0.40894(10) 0.0201(4) Uani 1 1 d . . . . .
C206 C 0.32942(10) 0.25389(16) 0.48143(10) 0.0205(4) Uani 1 1 d . . . . .
C207 C 0.38303(10) 0.16242(15) 0.52065(10) 0.0185(4) Uani 1 1 d . . . . .
C208 C 0.44479(10) 0.04835(16) 0.62874(10) 0.0183(4) Uani 1 1 d . . . . .
C209 C 0.57037(11) -0.05794(17) 0.23955(10) 0.0230(4) Uani 1 1 d . . . . .
H209 H 0.605830 -0.118306 0.251048 0.028 Uiso 1 1 calc R . . . .
C210 C 0.54501(12) -0.00734(18) 0.16868(11) 0.0281(4) Uani 1 1 d . . . . .
H210 H 0.563282 -0.034932 0.132009 0.034 Uiso 1 1 calc R . . . .
C211 C 0.49211(12) 0.08500(18) 0.15135(11) 0.0286(4) Uani 1 1 d . . . . .
H211 H 0.477181 0.119148 0.103868 0.034 Uiso 1 1 calc R . . . .
C212 C 0.46174(11) 0.12618(16) 0.20380(10) 0.0234(4) Uani 1 1 d . . . . .
H212 H 0.426278 0.186549 0.191967 0.028 Uiso 1 1 calc R . . . .
C213 C 0.28858(10) 0.34240(17) 0.35649(11) 0.0229(4) Uani 1 1 d . . . . .
H213 H 0.291230 0.348318 0.308528 0.028 Uiso 1 1 calc R . . . .
C214 C 0.23896(11) 0.41161(17) 0.37816(11) 0.0262(4) Uani 1 1 d . . . . .
H214 H 0.208339 0.465380 0.344245 0.031 Uiso 1 1 calc R . . . .
C215 C 0.23415(11) 0.40193(17) 0.45033(11) 0.0265(4) Uani 1 1 d . . . . .
H215 H 0.200247 0.449058 0.463181 0.032 Uiso 1 1 calc R . . . .
C216 C 0.27914(11) 0.32320(17) 0.50273(11) 0.0243(4) Uani 1 1 d . . . . .
H216 H 0.275910 0.316812 0.550442 0.029 Uiso 1 1 calc R . . . .
C401 C 0.38216(11) -0.16503(17) 0.38680(11) 0.0260(4) Uani 1 1 d . . . . .
H401 H 0.378204 -0.112407 0.347699 0.031 Uiso 1 1 calc R . . . .
C402 C 0.41520(12) -0.24606(19) 0.49567(12) 0.0318(5) Uani 1 1 d . . . . .
H402 H 0.438795 -0.259457 0.546614 0.038 Uiso 1 1 calc R . . . .
C403 C 0.36611(13) -0.32141(19) 0.44832(12) 0.0350(5) Uani 1 1 d . . . . .
H403 H 0.349802 -0.394297 0.460449 0.042 Uiso 1 1 calc R . . . .
C404 C 0.29420(13) -0.3172(2) 0.30851(12) 0.0377(5) Uani 1 1 d . . . . .
H40A H 0.287941 -0.260100 0.269077 0.056 Uiso 1 1 calc GR . . . .
H40B H 0.246959 -0.333265 0.313903 0.056 Uiso 1 1 calc GR . . . .
H40C H 0.314301 -0.389821 0.296427 0.056 Uiso 1 1 calc GR . . . .
V1AA V 1.000000 0.500000 0.500000 0.01680(10) Uani 1 2 d S T P . .
N101 N 0.89703(8) 0.43579(13) 0.45285(8) 0.0191(3) Uani 1 1 d . . . . .
N102 N 0.96692(8) 0.65760(13) 0.45051(8) 0.0191(3) Uani 1 1 d . . . . .
N103 N 0.83511(9) 0.61453(14) 0.38801(8) 0.0220(3) Uani 1 1 d . . . . .
N104 N 1.08386(9) 0.76692(13) 0.49761(8) 0.0215(3) Uani 1 1 d . . . . .
N301 N 1.03139(9) 0.43984(14) 0.40768(8) 0.0218(3) Uani 1 1 d . . . . .
N302 N 1.05937(10) 0.32347(16) 0.32714(9) 0.0300(4) Uani 1 1 d . . . . .
C101 C 0.79500(11) 0.31096(17) 0.42004(10) 0.0228(4) Uani 1 1 d . . . . .
C102 C 0.77145(10) 0.42282(17) 0.38703(10) 0.0233(4) Uani 1 1 d . . . . .
C103 C 0.83667(10) 0.50019(16) 0.40833(10) 0.0199(4) Uani 1 1 d . . . . .
C104 C 0.89464(10) 0.68608(16) 0.40801(10) 0.0206(4) Uani 1 1 d . . . . .
C105 C 0.89224(11) 0.81222(17) 0.38804(10) 0.0233(4) Uani 1 1 d . . . . .
C106 C 0.96524(11) 0.85644(16) 0.41824(10) 0.0229(4) Uani 1 1 d . . . . .
C107 C 1.01117(11) 0.75749(16) 0.45858(10) 0.0204(4) Uani 1 1 d . . . . .
C108 C 1.12553(10) 0.67877(16) 0.53786(10) 0.0208(4) Uani 1 1 d . . . . .
C109 C 0.74499(11) 0.21650(18) 0.40937(12) 0.0285(4) Uani 1 1 d . . . . .
H109 H 0.760377 0.142006 0.430601 0.034 Uiso 1 1 calc R . . . .
C110 C 0.67142(12) 0.2373(2) 0.36599(13) 0.0350(5) Uani 1 1 d . . . . .
H110 H 0.637118 0.175598 0.358254 0.042 Uiso 1 1 calc R . . . .
C111 C 0.64772(12) 0.3489(2) 0.33368(13) 0.0345(5) Uani 1 1 d . . . . .
H111 H 0.597975 0.360279 0.305378 0.041 Uiso 1 1 calc R . . . .
C112 C 0.69743(11) 0.44280(19) 0.34328(12) 0.0285(4) Uani 1 1 d . . . . .
H112 H 0.681914 0.516752 0.321247 0.034 Uiso 1 1 calc R . . . .
C113 C 0.83347(12) 0.88716(18) 0.34905(11) 0.0293(5) Uani 1 1 d . . . . .
H113 H 0.785041 0.858640 0.329898 0.035 Uiso 1 1 calc R . . . .
C114 C 0.84993(13) 1.00575(18) 0.33992(11) 0.0333(5) Uani 1 1 d . . . . .
H114 H 0.811779 1.057430 0.314238 0.040 Uiso 1 1 calc R . . . .
C115 C 0.92283(13) 1.04910(18) 0.36860(11) 0.0328(5) Uani 1 1 d . . . . .
H115 H 0.932172 1.128589 0.360720 0.039 Uiso 1 1 calc R . . . .
C116 C 0.98128(13) 0.97609(17) 0.40844(11) 0.0283(4) Uani 1 1 d . . . . .
H116 H 1.029484 1.005471 0.427989 0.034 Uiso 1 1 calc R . . . .
C301 C 1.04502(11) 0.32882(18) 0.39166(11) 0.0259(4) Uani 1 1 d . . . . .
H301 H 1.044679 0.262952 0.421407 0.031 Uiso 1 1 calc R . . . .
C302 C 1.03893(12) 0.50884(19) 0.35023(11) 0.0309(5) Uani 1 1 d . . . . .
H302 H 1.033595 0.591360 0.346425 0.037 Uiso 1 1 calc R . . . .
C303 C 1.05538(12) 0.4371(2) 0.30022(12) 0.0350(5) Uani 1 1 d . . . . .
H303 H 1.062535 0.460909 0.256155 0.042 Uiso 1 1 calc R . . . .
C304 C 1.07741(16) 0.2161(2) 0.29273(15) 0.0501(7) Uani 1 1 d . . . . .
H30A H 1.129201 0.216840 0.298290 0.075 Uiso 1 1 calc GR . . . .
H30B H 1.048188 0.214430 0.240443 0.075 Uiso 1 1 calc GR . . . .
H30C H 1.066687 0.146557 0.316883 0.075 Uiso 1 1 calc GR . . . .
N501 N 0.1224(13) 0.7775(13) 0.2979(9) 0.0429(8) Uani 0.158(14) 1 d D . . A 1
N502 N 0.1800(12) 0.9398(13) 0.3574(6) 0.0393(7) Uani 0.158(14) 1 d D . . A 1
C501 C 0.1405(12) 0.8414(15) 0.3602(7) 0.0442(9) Uani 0.158(14) 1 d D . . A 1
H501 H 0.127376 0.820521 0.401572 0.053 Uiso 0.158(14) 1 calc R . . A 1
C502 C 0.1473(12) 0.8451(15) 0.2506(7) 0.0350(8) Uani 0.158(14) 1 d D . . A 1
H502 H 0.140476 0.825745 0.201041 0.042 Uiso 0.158(14) 1 calc R . . A 1
C503 C 0.1833(15) 0.9444(17) 0.2863(7) 0.0365(6) Uani 0.158(14) 1 d D . . A 1
H503 H 0.205671 1.003201 0.266583 0.044 Uiso 0.158(14) 1 calc R . . A 1
C504 C 0.2091(15) 1.0290(16) 0.4172(8) 0.0521(13) Uani 0.158(14) 1 d D . . A 1
H50A H 0.178601 1.030232 0.448405 0.078 Uiso 0.158(14) 1 calc GR . . A 1
H50B H 0.208539 1.106422 0.395326 0.078 Uiso 0.158(14) 1 calc GR . . A 1
H50C H 0.259099 1.008532 0.446993 0.078 Uiso 0.158(14) 1 calc GR . . A 1
N601 N 0.1088(3) 0.7795(3) 0.2850(2) 0.0429(8) Uani 0.842(14) 1 d D . . A 2
N602 N 0.1850(2) 0.9184(4) 0.35344(16) 0.0393(7) Uani 0.842(14) 1 d D . . A 2
C601 C 0.1444(3) 0.8201(4) 0.3533(2) 0.0442(9) Uani 0.842(14) 1 d D . . A 2
H601 H 0.141707 0.784531 0.396649 0.053 Uiso 0.842(14) 1 calc R . . A 2
C602 C 0.1294(3) 0.8564(3) 0.2390(2) 0.0350(8) Uani 0.842(14) 1 d D . . A 2
H602 H 0.113884 0.850272 0.187124 0.042 Uiso 0.842(14) 1 calc R . . A 2
C603 C 0.1755(3) 0.9428(4) 0.27989(19) 0.0365(6) Uani 0.842(14) 1 d D . . A 2
H603 H 0.196355 1.005489 0.261644 0.044 Uiso 0.842(14) 1 calc R . . A 2
C604 C 0.2299(3) 0.9867(6) 0.41954(18) 0.0521(13) Uani 0.842(14) 1 d D . . A 2
H60A H 0.200626 1.003904 0.450641 0.078 Uiso 0.842(14) 1 calc GR . . A 2
H60B H 0.245800 1.060160 0.403626 0.078 Uiso 0.842(14) 1 calc GR . . A 2
H60C H 0.272630 0.940662 0.447459 0.078 Uiso 0.842(14) 1 calc GR . . 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'
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 -3 -5 0.0850
0 0 -1 0.0541
-1 0 0 0.0764
-4 4 5 0.0765
0 0 1 0.0620
-5 -4 4 0.0852
1 5 -2 0.1085
4 5 -5 0.1023
1 -5 1 0.0996
-1 0 1 0.1005
5 0 -4 0.0846
5 0 2 0.0345
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
N201 V0AA N201 180.0 3_656 .
N201 V0AA N401 91.41(6) . 3_656
N201 V0AA N401 88.59(6) . .
N201 V0AA N401 88.59(6) 3_656 3_656
N201 V0AA N401 91.41(6) 3_656 .
N202 V0AA N201 89.71(6) . .
N202 V0AA N201 90.29(6) 3_656 .
N202 V0AA N201 90.29(6) . 3_656
N202 V0AA N201 89.71(6) 3_656 3_656
N202 V0AA N202 180.0 3_656 .
N202 V0AA N401 87.08(6) . 3_656
N202 V0AA N401 92.92(6) 3_656 3_656
N202 V0AA N401 92.92(6) . .
N202 V0AA N401 87.08(6) 3_656 .
N401 V0AA N401 180.0 3_656 .
C203 N201 V0AA 125.94(12) . .
C208 N201 V0AA 124.92(12) 3_656 .
C208 N201 C203 108.98(14) 3_656 .
C204 N202 V0AA 125.50(12) . .
C207 N202 V0AA 125.14(12) . .
C207 N202 C204 109.23(14) . .
C203 N203 C204 124.01(16) . .
C208 N204 C207 124.41(15) . .
C401 N401 V0AA 127.19(13) . .
C401 N401 C402 104.90(16) . .
C402 N401 V0AA 127.75(13) . .
C401 N402 C403 106.85(16) . .
C401 N402 C404 125.87(17) . .
C403 N402 C404 127.25(17) . .
C202 C201 C208 107.02(15) . 3_656
C209 C201 C202 120.62(17) . .
C209 C201 C208 132.35(17) . 3_656
C201 C202 C203 106.53(15) . .
C212 C202 C201 120.88(16) . .
C212 C202 C203 132.59(17) . .
N201 C203 C202 108.80(15) . .
N203 C203 N201 126.96(16) . .
N203 C203 C202 124.22(16) . .
N202 C204 C205 108.63(15) . .
N203 C204 N202 127.84(16) . .
N203 C204 C205 123.52(16) . .
C206 C205 C204 106.75(16) . .
C213 C205 C204 132.09(17) . .
C213 C205 C206 121.15(17) . .
C205 C206 C207 106.72(15) . .
C216 C206 C205 120.83(17) . .
C216 C206 C207 132.45(17) . .
N202 C207 C206 108.66(15) . .
N204 C207 N202 127.63(16) . .
N204 C207 C206 123.70(16) . .
N201 C208 C201 108.63(15) 3_656 3_656
N204 C208 N201 127.43(16) . 3_656
N204 C208 C201 123.94(16) . 3_656
C201 C209 H209 120.9 . .
C210 C209 C201 118.23(18) . .
C210 C209 H209 120.9 . .
C209 C210 H210 119.5 . .
C209 C210 C211 121.06(18) . .
C211 C210 H210 119.5 . .
C210 C211 H211 119.4 . .
C212 C211 C210 121.25(18) . .
C212 C211 H211 119.4 . .
C202 C212 H212 121.0 . .
C211 C212 C202 117.90(18) . .
C211 C212 H212 121.0 . .
C205 C213 H213 121.1 . .
C205 C213 C214 117.75(17) . .
C214 C213 H213 121.1 . .
C213 C214 H214 119.3 . .
C213 C214 C215 121.31(18) . .
C215 C214 H214 119.3 . .
C214 C215 H215 119.4 . .
C216 C215 C214 121.14(18) . .
C216 C215 H215 119.4 . .
C206 C216 H216 121.1 . .
C215 C216 C206 117.82(17) . .
C215 C216 H216 121.1 . .
N401 C401 N402 111.80(17) . .
N401 C401 H401 124.1 . .
N402 C401 H401 124.1 . .
N401 C402 H402 125.0 . .
C403 C402 N401 110.03(18) . .
C403 C402 H402 125.0 . .
N402 C403 H403 126.8 . .
C402 C403 N402 106.41(18) . .
C402 C403 H403 126.8 . .
N402 C404 H40A 109.5 . .
N402 C404 H40B 109.5 . .
N402 C404 H40C 109.5 . .
H40A C404 H40B 109.5 . .
H40A C404 H40C 109.5 . .
H40B C404 H40C 109.5 . .
N101 V1AA N101 180.00(8) 3_766 .
N101 V1AA N301 88.47(6) . 3_766
N101 V1AA N301 91.53(6) 3_766 3_766
N101 V1AA N301 91.53(6) . .
N101 V1AA N301 88.47(6) 3_766 .
N102 V1AA N101 89.99(6) . .
N102 V1AA N101 89.99(6) 3_766 3_766
N102 V1AA N101 90.01(6) . 3_766
N102 V1AA N101 90.01(6) 3_766 .
N102 V1AA N102 180.0 . 3_766
N102 V1AA N301 88.52(6) . 3_766
N102 V1AA N301 88.52(6) 3_766 .
N102 V1AA N301 91.48(6) 3_766 3_766
N102 V1AA N301 91.48(6) . .
N301 V1AA N301 180.0 . 3_766
C103 N101 V1AA 125.36(12) . .
C103 N101 C108 109.26(15) . 3_766
C108 N101 V1AA 125.33(12) 3_766 .
C104 N102 V1AA 124.98(12) . .
C107 N102 V1AA 125.37(12) . .
C107 N102 C104 109.44(15) . .
C103 N103 C104 123.96(16) . .
C108 N104 C107 124.42(16) . .
C301 N301 V1AA 127.80(13) . .
C301 N301 C302 105.24(16) . .
C302 N301 V1AA 126.92(13) . .
C301 N302 C303 107.25(17) . .
C301 N302 C304 126.46(19) . .
C303 N302 C304 126.29(19) . .
C102 C101 C108 106.91(16) . 3_766
C109 C101 C102 120.71(18) . .
C109 C101 C108 132.38(18) . 3_766
C101 C102 C103 106.89(16) . .
C112 C102 C101 121.06(18) . .
C112 C102 C103 132.05(19) . .
N101 C103 C102 108.61(16) . .
N103 C103 N101 127.60(17) . .
N103 C103 C102 123.78(17) . .
N102 C104 C105 108.20(16) . .
N103 C104 N102 127.95(16) . .
N103 C104 C105 123.84(17) . .
C106 C105 C104 107.16(16) . .
C113 C105 C104 131.90(19) . .
C113 C105 C106 120.92(18) . .
C105 C106 C107 106.54(16) . .
C116 C106 C105 120.92(18) . .
C116 C106 C107 132.51(19) . .
N102 C107 C106 108.63(16) . .
N104 C107 N102 127.45(16) . .
N104 C107 C106 123.91(17) . .
N101 C108 C101 108.33(16) 3_766 3_766
N104 C108 N101 127.37(17) . 3_766
N104 C108 C101 124.30(17) . 3_766
C101 C109 H109 121.1 . .
C110 C109 C101 117.82(19) . .
C110 C109 H109 121.1 . .
C109 C110 H110 119.2 . .
C109 C110 C111 121.6(2) . .
C111 C110 H110 119.2 . .
C110 C111 H111 119.6 . .
C112 C111 C110 120.9(2) . .
C112 C111 H111 119.6 . .
C102 C112 H112 121.0 . .
C111 C112 C102 117.9(2) . .
C111 C112 H112 121.0 . .
C105 C113 H113 121.2 . .
C114 C113 C105 117.7(2) . .
C114 C113 H113 121.2 . .
C113 C114 H114 119.3 . .
C113 C114 C115 121.4(2) . .
C115 C114 H114 119.3 . .
C114 C115 H115 119.3 . .
C116 C115 C114 121.41(19) . .
C116 C115 H115 119.3 . .
C106 C116 H116 121.2 . .
C115 C116 C106 117.7(2) . .
C115 C116 H116 121.2 . .
N301 C301 N302 111.52(17) . .
N301 C301 H301 124.2 . .
N302 C301 H301 124.2 . .
N301 C302 H302 125.4 . .
C303 C302 N301 109.26(19) . .
C303 C302 H302 125.4 . .
N302 C303 H303 126.6 . .
C302 C303 N302 106.72(18) . .
C302 C303 H303 126.6 . .
N302 C304 H30A 109.5 . .
N302 C304 H30B 109.5 . .
N302 C304 H30C 109.5 . .
H30A C304 H30B 109.5 . .
H30A C304 H30C 109.5 . .
H30B C304 H30C 109.5 . .
C501 N501 C502 104.0(2) . .
C501 N502 C503 106.4(2) . .
C501 N502 C504 126.6(3) . .
C503 N502 C504 126.9(2) . .
N501 C501 N502 112.8(3) . .
N501 C501 H501 123.6 . .
N502 C501 H501 123.6 . .
N501 C502 H502 124.6 . .
C503 C502 N501 110.7(2) . .
C503 C502 H502 124.6 . .
N502 C503 H503 127.0 . .
C502 C503 N502 105.9(2) . .
C502 C503 H503 127.0 . .
N502 C504 H50A 109.5 . .
N502 C504 H50B 109.5 . .
N502 C504 H50C 109.5 . .
H50A C504 H50B 109.5 . .
H50A C504 H50C 109.5 . .
H50B C504 H50C 109.5 . .
C601 N601 C602 104.0(2) . .
C601 N602 C603 106.4(2) . .
C601 N602 C604 126.6(2) . .
C603 N602 C604 126.9(2) . .
N601 C601 N602 112.9(2) . .
N601 C601 H601 123.6 . .
N602 C601 H601 123.6 . .
N601 C602 H602 124.6 . .
C603 C602 N601 110.7(2) . .
C603 C602 H602 124.6 . .
N602 C603 H603 127.0 . .
C602 C603 N602 106.0(2) . .
C602 C603 H603 127.0 . .
N602 C604 H60A 109.5 . .
N602 C604 H60B 109.5 . .
N602 C604 H60C 109.5 . .
H60A C604 H60B 109.5 . .
H60A C604 H60C 109.5 . .
H60B C604 H60C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V0AA N201 2.0019(14) 3_656
V0AA N201 2.0019(14) .
V0AA N202 1.9950(15) 3_656
V0AA N202 1.9950(15) .
V0AA N401 2.1494(15) .
V0AA N401 2.1494(15) 3_656
N201 C203 1.387(2) .
N201 C208 1.386(2) 3_656
N202 C204 1.383(2) .
N202 C207 1.381(2) .
N203 C203 1.339(2) .
N203 C204 1.341(2) .
N204 C207 1.338(2) .
N204 C208 1.335(2) .
N401 C401 1.329(2) .
N401 C402 1.377(2) .
N402 C401 1.344(2) .
N402 C403 1.374(3) .
N402 C404 1.463(3) .
C201 C202 1.414(3) .
C201 C208 1.459(2) 3_656
C201 C209 1.396(2) .
C202 C203 1.461(2) .
C202 C212 1.396(3) .
C204 C205 1.461(2) .
C205 C206 1.412(2) .
C205 C213 1.390(3) .
C206 C207 1.463(3) .
C206 C216 1.397(3) .
C209 H209 0.9300 .
C209 C210 1.386(3) .
C210 H210 0.9300 .
C210 C211 1.406(3) .
C211 H211 0.9300 .
C211 C212 1.389(3) .
C212 H212 0.9300 .
C213 H213 0.9300 .
C213 C214 1.390(3) .
C214 H214 0.9300 .
C214 C215 1.406(3) .
C215 H215 0.9300 .
C215 C216 1.389(3) .
C216 H216 0.9300 .
C401 H401 0.9300 .
C402 H402 0.9300 .
C402 C403 1.353(3) .
C403 H403 0.9300 .
C404 H40A 0.9600 .
C404 H40B 0.9600 .
C404 H40C 0.9600 .
V1AA N101 2.0016(15) .
V1AA N101 2.0016(15) 3_766
V1AA N102 1.9990(15) .
V1AA N102 1.9991(15) 3_766
V1AA N301 2.1418(15) 3_766
V1AA N301 2.1417(15) .
N101 C103 1.381(2) .
N101 C108 1.384(2) 3_766
N102 C104 1.382(2) .
N102 C107 1.380(2) .
N103 C103 1.335(2) .
N103 C104 1.338(2) .
N104 C107 1.341(2) .
N104 C108 1.335(2) .
N301 C301 1.326(2) .
N301 C302 1.382(2) .
N302 C301 1.342(2) .
N302 C303 1.364(3) .
N302 C304 1.464(3) .
C101 C102 1.405(3) .
C101 C108 1.463(3) 3_766
C101 C109 1.394(3) .
C102 C103 1.459(3) .
C102 C112 1.396(3) .
C104 C105 1.459(3) .
C105 C106 1.408(3) .
C105 C113 1.398(3) .
C106 C107 1.460(3) .
C106 C116 1.401(3) .
C109 H109 0.9300 .
C109 C110 1.389(3) .
C110 H110 0.9300 .
C110 C111 1.398(3) .
C111 H111 0.9300 .
C111 C112 1.388(3) .
C112 H112 0.9300 .
C113 H113 0.9300 .
C113 C114 1.389(3) .
C114 H114 0.9300 .
C114 C115 1.401(3) .
C115 H115 0.9300 .
C115 C116 1.385(3) .
C116 H116 0.9300 .
C301 H301 0.9300 .
C302 H302 0.9300 .
C302 C303 1.358(3) .
C303 H303 0.9300 .
C304 H30A 0.9600 .
C304 H30B 0.9600 .
C304 H30C 0.9600 .
N501 C501 1.324(4) .
N501 C502 1.374(3) .
N502 C501 1.347(3) .
N502 C503 1.372(3) .
N502 C504 1.473(4) .
C501 H501 0.9300 .
C502 H502 0.9300 .
C502 C503 1.361(3) .
C503 H503 0.9300 .
C504 H50A 0.9600 .
C504 H50B 0.9600 .
C504 H50C 0.9600 .
N601 C601 1.324(3) .
N601 C602 1.374(3) .
N602 C601 1.346(3) .
N602 C603 1.372(3) .
N602 C604 1.472(3) .
C601 H601 0.9300 .
C602 H602 0.9300 .
C602 C603 1.361(3) .
C603 H603 0.9300 .
C604 H60A 0.9600 .
C604 H60B 0.9600 .
C604 H60C 0.9600 .
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.9996 -3.0000 -5.0000 0.1891 -0.0717 0.1810
-0.0001 0.0000 -1.0000 0.0096 -0.0372 0.0100
-1.0000 0.0000 0.0000 -0.0316 -0.0185 0.0146
-3.9996 4.0000 5.0000 -0.2361 0.0335 -0.2246
0.0001 -0.0000 1.0000 -0.0096 0.0372 -0.0100
-4.9995 -4.0000 4.0000 -0.1349 0.1355 0.2656
0.9998 5.0000 -2.0000 -0.0261 -0.1545 -0.2855
3.9995 5.0000 -4.9999 0.0976 -0.2109 -0.2991
1.0001 -5.0000 1.0000 0.0990 0.1542 0.2663
-0.9999 0.0000 1.0000 -0.0412 0.0188 0.0046
4.9996 -0.0000 -4.0000 0.1965 -0.0567 -0.0328
5.0000 -0.0000 2.0000 0.1387 0.1667 -0.0931
