Crystalline salts of metal phthalocyanine radical anions [M{Pc(•3-)}](•-) (M = Cu(II), Pb(II), V(IV)O, Sn(IV)Cl2) with cryptand(Na+) cations: structure, optical and magnetic properties
Konarev, Dmitri V.; Faraonov, Maxim A.; Kuz`min, Alexey V.; Khasanov, Salavat S.; Nakano, Yoshiaki; Norko, Semen I.; Otsuka, Akihiro; Yamochi, Hideki; Saito, Gunzi; Lyubovskaya, Rimma N.; Batov, Mikhail S.; New J. Chem. 41 (2017) 6866–6874; doi:10.1039/C7NJ00530J

data_7056292
_publ_section_title
;
 Crystalline salts of metal phthalocyanine radical anions
 [M{Pc(&#x2022;3-)}](&#x2022;-) (M = Cu(II), Pb(II), V(IV)O, Sn(IV)Cl2)
 with cryptand(Na+) cations: structure, optical and magnetic properties
;
_journal_issue                   14
_journal_name_full               'New J. Chem.'
_journal_page_first              6866
_journal_page_last               6874
_journal_paper_doi               10.1039/C7NJ00530J
_journal_volume                  41
_journal_year                    2017
_chemical_compound_source        no
_chemical_formula_moiety         'C32 H16 Cu N8, C18 H36 N2 Na O6, C6 H4 Cl2'
_chemical_formula_sum            'C56 H56 Cl2 Cu N10 Na O6'
_chemical_formula_weight         1122.53
_chemical_melting_point          ?
_chemical_name_common            no
_chemical_name_systematic
'copper phthalocyanine salt with cryptand[2,2,2] sodium cations, dichlorobenzene solvate'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2013
_audit_update_record
;
2017-01-21 deposited with the CCDC.
2017-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                81.244(5)
_cell_angle_beta                 72.634(5)
_cell_angle_gamma                64.528(7)
_cell_formula_units_Z            2
_cell_length_a                   12.5241(8)
_cell_length_b                   12.6333(10)
_cell_length_c                   19.1273(10)
_cell_measurement_reflns_used    4342
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.7380
_cell_measurement_theta_min      1.8630
_cell_volume                     2606.6(3)
_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    WinGx
_computing_publication_material  WinGx
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.1040
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21481
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.089
_diffrn_reflns_theta_min         1.866
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.908
_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            black
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: o-dichlorobenzene'
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         11830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0260P)^2^+0.2590P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7575
_reflns_number_total             11830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00530j2.cif
_cod_data_source_block           CuPccrypt222Na
_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 
;
_cod_database_code               7056292
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.986
_oxdiff_exptl_absorpt_empirical_full_min 0.971
_oxdiff_exptl_absorpt_empirical_full_max 1.129
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2013-2
_shelx_res_checksum              38133