Pyridylporphyrin Metallacycles with a Slipped Cofacial Geometry: Spectroscopic, X-ray, and Photophysical Characterization
Elisabetta Iengo; Ennio Zangrando; Marco Bellini; Enzo Alessio; Anna Prodi; Claudio Chiorboli; Franco Scandola; Inorganic Chemistry 44 (2005) 9752–9762; doi:10.1021/ic051210l

data_4310235
_publ_contact_author_address
;
Dipartimento di Scienze Chimiche
Universit\`a di Trieste
Trieste 34127
Italy
;
_publ_contact_author_email       zangrando@univ.trieste.it
_publ_contact_author_name        'Prof Ennio Zangrando'
_publ_section_title
;
Pyridylporphyrin Metallacycles with a Slipped Cofacial Geometry:
Spectroscopic, X-ray, and Photophysical Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9752
_journal_page_last               9762
_journal_paper_doi               10.1021/ic051210l
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C92 H64 Cl4 N12 O6 Ru2 Zn2, 8(C H Cl3)'
_chemical_formula_sum            'C100 H72 Cl28 N12 O6 Ru2 Zn2'
_chemical_formula_weight         2863.18
_chemical_name_systematic
;
 bis[trans,cis,cis-dichloro-dicarbonyl-
 bis(ethanol-zinc(II)-5,10-bis(4'pyridyl)-15,20-diphenyl-porphyrinato)-
 -ruthenium(II)] octachloroform solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 90.95(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.239(4)
_cell_length_b                   14.018(4)
_cell_length_c                   37.997(7)
_cell_measurement_temperature    160(2)
_cell_volume                     5986(3)
_computing_cell_refinement       'Denzo (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius, Supergui'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep3/windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.64.05 (Farrugia, 1999)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELX97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 14
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  kappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            37767
_diffrn_reflns_theta_full        60.12
_diffrn_reflns_theta_max         60.12
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    8.662
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2856
_refine_diff_density_max         1.075
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.00020(7)
_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   1.056
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         8554
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0761
_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^)+(0.1620P)^2^+15.3605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2269
_refine_ls_wR_factor_ref         0.2529
_reflns_number_gt                6445
_reflns_number_total             8554
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051210lsi20050721_042745_1.cif
_cod_data_source_block           1a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4310235