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_7045684
_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         'C40 H28 Cr N12, 2(C6 H4 Cl2)'
_chemical_formula_sum            'C52 H36 Cl4 Cr N12'
_chemical_formula_weight         1022.73
_chemical_melting_point          ?
_chemical_name_common            no
_chemical_name_systematic
'N-methylimidazole complex of vanadium(II) phthalocyanine o-dichlorobenzene solvate'
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-25
_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                 108.240(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.7918(9)
_cell_length_b                   10.5704(3)
_cell_length_c                   18.1334(7)
_cell_measurement_reflns_used    5351
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0040
_cell_measurement_theta_min      2.0990
_cell_volume                     4513.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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 10.4566
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.841
_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    -33.00  32.00   1.00   60.00    --   11.81  19.00 150.00   65
  2  \w    -26.00  93.00   1.00   60.00    --   11.81  19.00  30.00  119
  3  \w    -92.00 -67.00   1.00   60.00    --  -12.05-178.00  30.00   25
;
_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      -0.0286494000
_diffrn_orient_matrix_UB_12      0.0205827000
_diffrn_orient_matrix_UB_13      -0.0137338000
_diffrn_orient_matrix_UB_21      -0.0070202000
_diffrn_orient_matrix_UB_22      -0.0424527000
_diffrn_orient_matrix_UB_23      0.0258804000
_diffrn_orient_matrix_UB_31      0.0061113000
_diffrn_orient_matrix_UB_32      0.0477065000
_diffrn_orient_matrix_UB_33      0.0289576000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12816
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.493
_diffrn_reflns_theta_min         1.730
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    1.505
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             2096
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: o-dichlorobenzene/n-hexane/N-methylimidazole'
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5301
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+6.3915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4185
_reflns_number_total             5301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00459e2.cif
_cod_data_source_block           CrMeIm2PcC6H4Cl2
_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               7045684
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C26Cl2Cr0.5N6
_reflns_odcompleteness_completeness 99.92
_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(C1T) = Uanis(C1S)
Uanis(C6T) = Uanis(C6S)
Uanis(C5T) = Uanis(C5S)
Uanis(C4T) = Uanis(C4S)
Uanis(C3T) = Uanis(C3S)
Uanis(C2T) = Uanis(C2S)
Uanis(Cl1T) = Uanis(Cl1S)
Uanis(Cl2T) = Uanis(Cl2S)
3. Same fragment restrains
{Cl1S, Cl2S, C1S, C2S, C3S, C4S, C5S, C6S} sigma for 1-2: 0.001, 1-3: 0.001
as
{Cl1T, Cl2T, C1T, C2T, C3T, C4T, C5T, C6T}
4. Others
 Sof(Cl1T)=Sof(Cl2T)=Sof(C1T)=Sof(C2T)=Sof(C3T)=Sof(H3T)=Sof(C4T)=Sof(H4T)=
 Sof(C5T)=Sof(H5T)=Sof(C6T)=Sof(H6T)=1-FVAR(1)
 Sof(Cl1S)=Sof(Cl2S)=Sof(C1S)=Sof(C2S)=Sof(C3S)=Sof(H3S)=Sof(C4S)=Sof(H4S)=
 Sof(C5S)=Sof(H5S)=Sof(C6S)=Sof(H6S)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C109(H109), C110(H110), C111(H111), C112(H112), C113(H113), C114(H114),
 C115(H115), C116(H116), C201(H201), C202(H202), C203(H203), C3S(H3S), C4S(H4S),
  C5S(H5S), C6S(H6S), C3T(H3T), C4T(H4T), C5T(H5T), C6T(H6T)
5.b Idealised Me refined as rotating group:
 C204(H20A,H20B,H20C)
;
_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 1.053
_oxdiff_exptl_absorpt_empirical_full_min 0.961