Synchrotron study of a fully protonated tetraphenyl porphyrin
Larsen, Frank B.; Hansen, Flemming G.; McKenzie, Christine J.; Acta Crystallographica Section E 60 (2004) o497–o499; doi:10.1107/S1600536804004489

data_2203524
_publ_section_title
;
 Synchrotron study of a fully protonated tetraphenyl porphyrin
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o497
_journal_page_last               o499
_journal_paper_doi               10.1107/S1600536804004489
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C44 H32 N4 2+ , 2Cl - , 2C2 H3 N , H2 O'
_chemical_formula_moiety         'C44 H32 N4 2+ , 2Cl - , 2C2 H3 N , H2 O'
_chemical_formula_sum            'C48 H40 Cl2 N6 O'
_chemical_formula_weight         787.76
_chemical_name_systematic
;
5,10,15,20-Tetraphenylporphyrindiium dichloride diacetonitrile monohydrate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL97 plus manual editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.975(4)
_cell_length_b                   25.920(5)
_cell_length_c                   8.228(2)
_cell_measurement_reflns_used    5893
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      58.62
_cell_measurement_theta_min      5.15
_cell_volume                     4046.8(15)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT '
_computing_molecular_graphics    'XP (Siemens, 1996)'
_computing_publication_material  'SHELXL97 '
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'thin slice \w'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS, Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6900
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13131
_diffrn_reflns_theta_full        29.40
_diffrn_reflns_theta_max         29.40
_diffrn_reflns_theta_min         2.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.396
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5658
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0488P)^2^+2.6837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1252
_reflns_number_gt                4241
_reflns_number_total             5658
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ww6167.cif
_cod_data_source_block           I
_cod_database_code               2203524
_cod_database_fobs_code          2203524