Tetra-2,3-pyrazinoporphyrazines with Externally Appended Pyridine Rings. 3. A New Highly Electron-Deficient Octacationic Macrocycle: Tetrakis-2,3-[5,6-di{2-(N-methyl)pyridiniumyl}pyrazino]porphyrazine, [(2-Mepy)8TPyzPzH2]8+
Costanza Bergami; Maria Pia Donzello; Claudio Ercolani; Fabrizio Monicelli; Karl M. Kadish; Corrado Rizzoli; Inorganic Chemistry 44 (2005) 9852–9861; doi:10.1021/ic051084l

data_4310221
_publ_contact_author
;
     Prof. Corrado Rizzoli
     Universit\'a di Parma
     Dipartimento di Chimica Generale ed Inorganica
     Chimica Analitica, Chimica Fisica
     Viale delle Scienze 17/A
     I-43100 Parma
     Italy
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_publ_contact_author_email       corrado.rizzoli@at@unipr.it
_publ_contact_author_fax         '[++39]521 905 556'
_publ_contact_author_phone       '[++39]521 905 449'
_publ_section_title
;
Tetra-2,3-pyrazinoporphyrazines with Externally Appended Pyridine Rings. 3.
A New Highly Electron-Deficient Octacationic Macrocycle:
Tetrakis-2,3-[5,6-di{2-(N-methyl)pyridiniumyl}pyrazino]porphyrazine,
[(2-Mepy)8TPyzPzH2]8+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9852
_journal_page_last               9861
_journal_paper_doi               10.1021/ic051084l
_journal_volume                  44
_journal_year                    2005
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C17 H11 N6, C7 H7 O3 S'
_chemical_formula_sum            'C24 H18 N6 O3 S'
_chemical_formula_weight         470.5
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             02/02/2005
_audit_creation_method           'ModiCIF v1.12'
_cell_angle_alpha                90.00(0)
_cell_angle_beta                 90.00(0)
_cell_angle_gamma                90.00(0)
_cell_formula_units_Z            4.00
_cell_length_a                   14.178(3)
_cell_length_b                   14.442(4)
_cell_length_c                   11.400(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      41.1
_cell_measurement_theta_min      17.4
_cell_volume                     2334.2(9)
_computing_cell_refinement       'Belletti et al., 1993'
_computing_data_collection       'Belletti, Cantoni & Pasquinelli,1993'
_computing_data_reduction        'DIFAU (Belletti et al.)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1998)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       omega/2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         fine-focussealedtube
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4824
_diffrn_reflns_theta_full        70.04
_diffrn_reflns_theta_max         70.04
_diffrn_reflns_theta_min         4.37
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.556
_exptl_absorpt_correction_T_max  0.616
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             976.0
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.125
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 'Flack (1983), 1928 Friedel pairs'
_refine_ls_abs_structure_Flack   0.10(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.062
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.205
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0821P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1334
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                3978
_reflns_number_total             4428
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic051084lsi20050628_101525_1.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2334.3(9)
_cod_database_code               4310221