Structure of a 4:1:4 Supramolecular Assembly of Neutral TiiiiPO Cavitands and Tetrakis(N-methylpyridinium)porphyrin Iodide
Rita De Zorzi; Béatrice Dubessy; Jean-Christophe Mulatier; Silvano Geremia; Lucio Randaccio; Jean-Pierre Dutasta; Journal of Organic Chemistry 72 (2007) 4528–4531; doi:10.1021/jo070109q

data_4022906
_publ_contact_author             'Geremia, Silvano'
_publ_contact_author_email       geremia@units.it
_publ_section_title
;
 Structure of a 4:1:4 Supramolecular Assembly of Neutral TiiiiPO
 Cavitands and Tetrakis(N-methylpyridinium)porphyrin Iodide
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4528
_journal_page_last               4531
_journal_paper_doi               10.1021/jo070109q
_journal_volume                  72
_journal_year                    2007
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C400 H330 Cl60 I4 N8 O48 P16'
_chemical_formula_sum            'C266.67 H220 Cl40 I2.67 N5.33 O32 P10.67'
_chemical_formula_weight         6097.89
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-02-17T15:35:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   28.2853(12)
_cell_length_b                   32.5755(8)
_cell_length_c                   51.646(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.9
_cell_volume                     47587(3)
_computing_cell_refinement       Mosflm
_computing_data_reduction        Mosflm
_computing_molecular_graphics    O
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device       'MAR CCD'
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       rotating
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.9
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.077
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24074
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.292
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             18568
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.705
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_coef       0.00291(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.446
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4577
_refine_ls_number_reflns         24074
_refine_ls_number_restraints     6442
_refine_ls_restrained_S_all      1.307
_refine_ls_R_factor_all          0.1574
_refine_ls_R_factor_gt           0.1302
_refine_ls_shift/su_max          1.421
_refine_ls_shift/su_mean         0.037
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3195
_refine_ls_wR_factor_ref         0.3519
_reflns_number_gt                16316
_reflns_number_total             24074
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo070109qrom20070125_035352.cif
_cod_data_source_block           finale
_cod_database_code               4022906