Hydrogen-bonded assemblies of 20-(4-pyridyl)porphyrin-5^4^,10^4^,15^4^-tribenzoic acid with dimethyl sulfoxide and 4-acetylpyridine in their dimethyl sulfoxide and tetrahydrofuran solvates
Sankar Muniappan; Sophia Lipstman; Israel Goldberg; Acta Crystallographica Section C 63 (2007) o395–o399; doi:10.1107/S0108270107024936

data_2016058
_publ_section_title
;
 Hydrogen-bonded assemblies of
 20-(4-pyridyl)porphyrin-5^4^,10^4^,15^4^-tribenzoic acid with dimethyl
 sulfoxide and 4-acetylpyridine in their dimethyl sulfoxide and
 tetrahydrofuran solvates
;
_journal_coeditor_code           LN3055
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o395
_journal_page_last               o399
_journal_paper_doi               10.1107/S0108270107024936
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C46 H29 N5 O6, 2.5C2 H6 S O'
_chemical_formula_moiety         'C46 H29 N5 O6, 2.5(C2 H6 S O)'
_chemical_formula_sum            'C51 H44 N5 O8.5 S2.5'
_chemical_formula_weight         943.06
_chemical_name_systematic
;
20-(4-pyridyl)porphyrin-5^4^,10^4^,15^4^-tribenzoic acid--dimethyl sulfoxide
(2/5)
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.521(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.5978(3)
_cell_length_b                   29.2458(15)
_cell_length_c                   28.6630(13)
_cell_measurement_reflns_used    5425
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.41
_cell_volume                     5530.5(5)
_computing_cell_refinement       'Denzo (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius, 1999)'
_computing_data_reduction        Denzo
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '0.3 deg. \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_sigmaI/netI    0.1338
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            18496
_diffrn_reflns_theta_full        27.85
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         2.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.312
_refine_ls_abs_structure_details 'Flack (1983), 5242 Friedel pairs'
_refine_ls_abs_structure_Flack   0.42(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         11808
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1522
_refine_ls_R_factor_gt           0.0852
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1905
_refine_ls_wR_factor_ref         0.2114
_reflns_number_gt                6211
_reflns_number_total             11808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ln3055.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2016058
_cod_database_fobs_code          2016058