Interwoven hydrogen-bonded network assembly and supramolecular isomerism of <i>meso</i>-5,10,15,20-tetrakis(4-carboxyphenyl)porphyrin as its dimethylformamide solvate
Sophia Lipstman; Sankar Muniappan; Israel Goldberg; Acta Crystallographica Section C 63 (2007) o371–o373; doi:10.1107/S0108270107020975

data_2016036
_publ_section_title
;
 Interwoven hydrogen-bonded network assembly and supramolecular
 isomerism of <i>meso</i>-5,10,15,20-tetrakis(4-carboxyphenyl)porphyrin
 as its dimethylformamide solvate
;
_journal_coeditor_code           GD3109
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o371
_journal_page_last               o373
_journal_paper_doi               10.1107/S0108270107020975
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C48 H30 N4 O8'
_chemical_formula_moiety         'C48 H30 N4 O8'
_chemical_formula_sum            'C48 H30 N4 O8'
_chemical_formula_weight         790.76
_chemical_name_common
;
porphyrin-5^4^,10^4^,15^4^,20^4^-tetrabenzoic acid
;
_chemical_name_systematic
;
meso-5,10,15,20-tetrakis(4-carboxyphenyl)porphyrin
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.0164(3)
_cell_length_b                   8.5897(11)
_cell_length_c                   15.1952(6)
_cell_measurement_reflns_used    2650
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.41
_cell_volume                     4048.3(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>,  1994)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '1 \% \w'
_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  0.0720
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15184
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0482P)^2^+8.4601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1383
_reflns_number_gt                1653
_reflns_number_total             2033
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd3109.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               2016036
_cod_database_fobs_code          2016036