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_2016925
_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 , 6C4 H9 N O , 2H2 O'
_chemical_formula_moiety         'C44 H30 N4 O4 , 6C4 H9 N O , 2H2 O'
_chemical_formula_sum            'C68 H88 N10 O12'
_chemical_formula_weight         1237.48
_chemical_name_systematic
;
5,10,15,20-tetrakis(4-hydroxyphenyl)porphyrin
<i>N</i>,<i>N</i>'-dimethylformamide hexasolvate dihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 102.2713(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.5243(8)
_cell_length_b                   6.5265(2)
_cell_length_c                   29.2172(9)
_cell_measurement_reflns_used    5086
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.48
_cell_measurement_theta_min      1.41
_cell_volume                     6619.2(3)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '1 deg. \f and \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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            16577
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.479
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         6116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0425P)^2^+19.1457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1542
_reflns_number_gt                4359
_reflns_number_total             6116
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd3260.cif
_cod_data_source_block           III
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2016925
_cod_database_fobs_code          2016925