Meso-Substituent Effects on Redox Properties of the 5,10-Porphodimethene-Type P,S,N2-Hybrid Calixphyrins and Their Metal Complexes
Matano, Yoshihiro; Fujita, Masato; Miyajima, Tooru; Imahori, Hiroshi; Organometallics 28 (2009) 6213–; doi:10.1021/om900745t

data_4070348
_publ_section_title
;
 Meso-Substituent Effects on Redox Properties of the
 5,10-Porphodimethene-Type P,S,N2-Hybrid Calixphyrins and Their Metal
 Complexes
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6213
_journal_paper_doi               10.1021/om900745t
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C48 H43 Cl N2 O3 P Rh S, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C48.5 H44 Cl2 N2 O3 P Rh S'
_chemical_formula_weight         939.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 100.612(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.168(5)
_cell_length_b                   14.487(4)
_cell_length_c                   18.921(6)
_cell_measurement_reflns_used    10331
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     4356(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        'CrystalStructure 3.8.2'
_computing_publication_material  'CrystalStructure 3.8.2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_detector_area_resol_mean 29.26
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_sigmaI/netI    0.0901
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33314
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  0.9747
_exptl_absorpt_correction_T_min  0.8303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         9943
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.1001
_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^)+(0.0200P)^2^+16.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                8062
_reflns_number_total             9943
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900745t_si_002.cif
_cod_data_source_block           shelxl
_cod_original_formula_sum        'C48.50 H44 Cl2 N2 O3 P Rh S'
_cod_database_code               4070348