Hydrogen-bonded assemblies of 5,10,15,20-tetrakis(4-hydroxyphenyl)porphyrin with dimethylformamide, dimethylacetamide and water
Lipstman, Sophia; Goldberg, Israel; Acta Crystallographica Section C 65 (2009) o3–o7; doi:10.1107/S0108270108040018

data_2016923
_publ_section_title
;
 Hydrogen-bonded assemblies of
 5,10,15,20-tetrakis(4-hydroxyphenyl)porphyrin with dimethylformamide,
 dimethylacetamide and water
;
_journal_coeditor_code           GD3260
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o3
_journal_page_last               o7
_journal_paper_doi               10.1107/S0108270108040018
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C44 H30 N4 O4 , 4C3 H7 N O'
_chemical_formula_moiety         'C44 H30 N4 O4 , 4C3 H7 N O'
_chemical_formula_sum            'C56 H58 N8 O8'
_chemical_formula_weight         971.10
_chemical_name_systematic
;
5,10,15,20-tetrakis(4-hydroxyphenyl)porphyrin
<i>N</i>,<i>N</i>'-dimethylformamide tetrasolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                101.7445(12)
_cell_angle_beta                 92.4786(12)
_cell_angle_gamma                114.9158(8)
_cell_formula_units_Z            4
_cell_length_a                   13.6255(2)
_cell_length_b                   16.0184(3)
_cell_length_c                   26.2466(5)
_cell_measurement_reflns_used    14137
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.38
_cell_volume                     5032.65(16)
_computing_cell_refinement       '[Please provide details]'
_computing_data_collection       '[Please provide details]'
_computing_data_reduction        '[Please provide details]'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  '[Please provide details]'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_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       '0.7 deg. \f and \w scan'
_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  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0904
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            50610
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.38
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.386
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1370
_refine_ls_number_reflns         23877
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0777P)^2^+0.4228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1691
_reflns_number_gt                13053
_reflns_number_total             23879
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd3260.cif
_cod_data_source_block           I
_cod_original_cell_volume        5032.65(15)
_cod_database_code               2016923
_cod_database_fobs_code          2016923