Unsolvated 5,10,15,20-tetra-4-pyridylporphyrin, its sesquihydrate and its 2-chlorophenol disolvate: conformational versatility of the ligand
Lipstman, Sophia; Goldberg, Israel; Acta Crystallographica Section C 65 (2009) o447–o452; doi:10.1107/S0108270109030753

data_2017296
_publ_section_title
;
 Unsolvated 5,10,15,20-tetra-4-pyridylporphyrin, its sesquihydrate and
 its 2-chlorophenol disolvate: conformational versatility of the ligand
;
_journal_coeditor_code           GD3300
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o447
_journal_page_last               o452
_journal_paper_doi               10.1107/S0108270109030753
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C40 H26 N8, 1.514H2 O'
_chemical_formula_moiety         'C40 H26 N8, 1.514(H2 O)'
_chemical_formula_sum            'C40 H29.028 N8 O1.514'
_chemical_formula_weight         645.96
_chemical_name_systematic
;
5,10,15,20-tetra-4-pyridylporphyrin 1.514-hydrate
;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2155(4)
_cell_length_b                   15.2155(4)
_cell_length_c                   13.5388(6)
_cell_measurement_reflns_used    4891
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      1.95
_cell_volume                     3134.39(18)
_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>,  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'
_diffrn_measurement_method       '1 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  0.0670
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16180
_diffrn_reflns_theta_full        27.85
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         2.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1348.9
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.129
_refine_diff_density_min         -0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         757
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0618P)^2^+0.3277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1151
_reflns_number_gt                757
_reflns_number_total             1042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            gd3300.cif
_cod_data_source_block           II
_cod_database_code               2017296
_cod_database_fobs_code          2017296