Radical anion and dianion salts of titanyl macrocycles with acceptor substituents or an extended π-system.
Faraonov, Maxim A.; Konarev, Dmitri V.; Fatalov, Alexey M.; Khasanov, Salavat S.; Troyanov, Sergey I.; Lyubovskaya, Rimma N.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3547–3555; doi:10.1039/c6dt04896j

data_7042098
_publ_section_title
;
 Radical anion and dianion salts of titanyl macrocycles with acceptor
 substituents or an extended \p-system.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3547
_journal_page_last               3555
_journal_paper_doi               10.1039/c6dt04896j
_journal_volume                  46
_journal_year                    2017
_chemical_compound_source        no
_chemical_formula_moiety
'(C64 H24 N16 Ti O), 2(C36 H30 N P2), 0.8(C7 H5 N) 1.3(C6 H4 Cl2)'
_chemical_formula_sum            'C149.4 H93.2 Cl2.6 N18.8 O P4 Ti'
_chemical_formula_weight         2431.57
_chemical_melting_point          ?
_chemical_name_common            no
_chemical_name_systematic
'di(bis(triphenylphosphoranylidene)ammonium) titanyl tetra(acenapheno)pyrazinoporphyrazene , dichlorobenzene, benzonitrile 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
_audit_creation_date             2016-05-10
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-02-12 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.073(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.695(2)
_cell_length_b                   25.1999(8)
_cell_length_c                   27.4198(11)
_cell_measurement_reflns_used    12202
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.1380
_cell_measurement_theta_min      1.7720
_cell_volume                     24883.3(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    WinGX
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0901
_diffrn_reflns_av_unetI/netI     0.0947
_diffrn_reflns_Laue_measured_fraction_full 0.928
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            68100
_diffrn_reflns_point_group_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.707
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83031
_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    1.298
_exptl_crystal_description       prism
_exptl_crystal_F_000             10043
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: o-dichlorobenzene'
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1529
_refine_ls_number_reflns         20895
_refine_ls_number_restraints     797
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1984
_refine_ls_R_factor_gt           0.1158
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1298P)^2^+186.4310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2766
_refine_ls_wR_factor_ref         0.3277
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11354
_reflns_number_total             20895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04896j2.cif
_cod_data_source_block           2PPNTiOAcenaphPrzPz
_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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7042097--7042099.cif.
;
_cod_original_cell_volume        24883.5(19)
_cod_original_formula_sum        'C149.40 H93.20 Cl2.60 N18.80 O P4 Ti'
_cod_database_code               7042098
_shelx_estimated_absorpt_t_min   0.921
_shelx_estimated_absorpt_t_max   0.965
_shelxl_version_number           2013-4
_shelx_res_checksum              66305