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_7044275
_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, C18 H36 N2 O6 Na, 0.5(C6 H4 Cl2)'
_chemical_formula_sum            'C58 H63 Cl N6 Na O6'
_chemical_formula_weight         998.58
_chemical_melting_point          ?
_chemical_name_common            no
_chemical_name_systematic
'salt of deprotonated triphenylcorrole with cryptand sodium cations, o-dichlobenzene solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-01-12
_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                 96.142(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0302(2)
_cell_length_b                   18.0323(3)
_cell_length_c                   21.3928(4)
_cell_measurement_reflns_used    23554
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      27.5350
_cell_measurement_theta_min      2.4480
_cell_volume                     4997.69(15)
_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      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0227
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            55350
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.926
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       block
_exptl_crystal_F_000             2116
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: o-dichlobenzene/hexane'
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.280
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         11012
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0652P)^2^+3.4754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9172
_reflns_number_total             11012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02901b2.cif
_cod_data_source_block           H2CorCryptNa
_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_original_formula_sum        'C58 H63 Cl1 N6 Na1 O6'
_cod_database_code               7044275
_shelx_estimated_absorpt_t_min   0.947
_shelx_estimated_absorpt_t_max   0.961
_shelxl_version_number           2013-4
_shelx_res_checksum              77801