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_4310222
_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
;
_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, I1'
_chemical_formula_sum            'C17 H11 I N6'
_chemical_formula_weight         426.22
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_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                 112.48(2)
_cell_angle_gamma                90.00(0)
_cell_formula_units_Z            4.00
_cell_length_a                   13.489(3)
_cell_length_b                   13.181(3)
_cell_length_c                   11.005(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      42.6
_cell_measurement_theta_min      18.2
_cell_volume                     1808.0(7)
_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 0.98
_diffrn_measured_fraction_theta_max 0.98
_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  0.0152
_diffrn_reflns_av_sigmaI/netI    0.0136
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3474
_diffrn_reflns_theta_full        69.94
_diffrn_reflns_theta_max         69.94
_diffrn_reflns_theta_min         4.88
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    13.9986
_exptl_absorpt_correction_T_max  0.210
_exptl_absorpt_correction_T_min  0.166
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.5658
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             832.0
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.143
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details 'Flack (1983), 1716 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.003(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         1728
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.269
_refine_ls_restrained_S_obs      1.042
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0558
_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^)+(0.1440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1829
_refine_ls_wR_factor_ref         0.1471
_reflns_number_gt                1677
_reflns_number_total             1756
_reflns_threshold_expression     I>\2s(I)
_cod_data_source_file            ic051084lsi20050628_101525_2.cif
_cod_data_source_block           Compound1
_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_formula_sum        'C17 H11 I1 N6'
_cod_database_code               4310222