Solid state structures and properties of free-base 5, 10, 15-triphenylcorrole (TPCor) anions obtained by deprotonation and reduction. Effective magnetic coupling of spins in (Cp*2Cr+)(H+){H2TPCor(.2-)}.C6H4Cl2
Konarev, Dmitri V.; Karimov, Dmitry R.; Khasanov, Salavat S.; Shestakov, Alexander F.; Otsuka, Akihiro; Yamochi, Hideki; Kitagawa, Hiroshi; Lyubovskaya, Rimma N.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02901B

data_7044274
_publ_section_title
;
 Solid state structures and properties of free-base 5, 10,
 15-triphenylcorrole (TPCor) anions obtained by deprotonation and
 reduction. Effective magnetic coupling of spins in
 (Cp*2Cr+)(H+){H2TPCor(.2-)}.C6H4Cl2
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02901B
_journal_year                    2017
_chemical_compound_source        no
_chemical_formula_moiety         'C37 H25 N4, C20 H30 Cr, C6 H4 Cl2'
_chemical_formula_sum            'C63 H59 Cl2 Cr N4'
_chemical_formula_weight         995.04
_chemical_melting_point          ?
_chemical_name_common            no
_chemical_name_systematic
'complex of decamethylchromocene with triphenylcorrole, o-dichlorobenzene solvate'
_chemical_properties_physical    ', Air-sensitive,Moisture-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
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Fri Jul 22 11:23:38 2016'
;
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-05-24 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.065(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.245(3)
_cell_length_b                   10.6383(6)
_cell_length_c                   36.765(3)
_cell_measurement_reflns_used    3768
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      21.7080
_cell_measurement_theta_min      2.6890
_cell_volume                     10264.9(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    WinGX
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.953
_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  0.1124
_diffrn_reflns_av_unetI/netI     0.1327
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            44240
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.906
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       ruler
_exptl_crystal_F_000             4184
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: o-dichlorobenzene/hexane'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         9723
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1572
_refine_ls_R_factor_gt           0.0787
_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^)+(0.0920P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1593
_refine_ls_wR_factor_ref         0.1959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5747
_reflns_number_total             9723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02901b2.cif
_cod_data_source_block           H2CorroleDMCp2Cr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'notmeasured' 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_original_cell_volume        10265.0(15)
_cod_database_code               7044274
_shelx_estimated_absorpt_t_min   0.946
_shelx_estimated_absorpt_t_max   0.993
_shelxl_version_number           2013-4
_shelx_res_checksum              66930