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_7042099
_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         'C48 H24 N8 O Ti, C36 H30 N P2, 2(C6 H4 Cl2)'
_chemical_formula_sum            'C96 H62 Cl4 N9 O P2 Ti'
_chemical_formula_weight         1609.18
_chemical_melting_point          ?
_chemical_name_common            no
_chemical_name_systematic
'bis(triphenylphosphoranylidene ammonium titanyl naphthalocyanine radical anion o-dichlorobenzene solvate'
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-11-22 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.402(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1213(3)
_cell_length_b                   18.0169(3)
_cell_length_c                   29.1976(6)
_cell_measurement_reflns_used    51455
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.4290
_cell_measurement_theta_min      1.8090
_cell_volume                     7869.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    WinGx
_computing_publication_material  WinGx
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            100772
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         29.374
_diffrn_reflns_theta_min         1.811
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 - Bruker AXS area detector scaling 
and absorption correction 
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       prism
_exptl_crystal_F_000             3316
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: o-dichlorobenzene'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1035
_refine_ls_number_reflns         20327
_refine_ls_number_restraints     1238
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0818
_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^)+(0.0627P)^2^+13.5578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.1824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15449
_reflns_number_total             20327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04896j2.cif
_cod_data_source_block           PPNTiONaphthalocyanine
_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_database_code               7042099
_shelx_estimated_absorpt_t_min   0.875
_shelx_estimated_absorpt_t_max   0.935
_shelxl_version_number           2013-4
_shelx_res_checksum              30107