Synthesis and properties of N-methylimidazole solvates of vanadium(ii), chromium(ii) and iron(ii) phthalocyanines. Strong NIR absorption in V<sup>II</sup>(MeIm)<sub>2</sub>(Pc<sup>2-</sup>).
Konarev, Dmitri V.; Kuzmin, Alexey V.; Nakano, Yoshiaki; Khasanov, Salavat S.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Lyubovskaya, Rimma N.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 4661–4671; doi:10.1039/c8dt00459e

data_7045682
_publ_section_title
;
 Synthesis and properties of N-methylimidazole solvates of vanadium(ii),
 chromium(ii) and iron(ii) phthalocyanines. Strong NIR absorption in
 V<sup>II</sup>(MeIm)<sub>2</sub>(Pc<sup>2-</sup>).
;
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -25.00  22.00   1.00   64.00    --  -12.05 -99.00 120.00   47
  2  \w    -87.00 -57.00   1.00   64.00    --  -12.05 -37.00 120.00   30
  3  \w    -24.00   9.00   1.00   64.00    --  -12.05 -37.00 120.00   33
  4  \w    -13.00  29.00   1.00   64.00    --  -12.05 -99.00 -90.00   42
  5  \w    -16.00  10.00   1.00   64.00    --  -12.05  37.00   0.00   26
  6  \w     13.00  56.00   1.00   64.00    --  -12.05  37.00   0.00   43
  7  \w    -38.00  33.00   1.00   64.00    --  -12.05  57.00  90.00   71
  8  \w    -30.00  62.00   1.00   64.00    --  -12.05  57.00 -90.00   92
  9  \w    -92.00 -60.00   1.00   64.00    --  -12.05-178.00 -90.00   32
 10  \w    -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       '\w 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/[\s^2^(Fo^2^)+(0.0395P)^2^+2.7602P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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 '
_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