Metallacycles of Porphyrins as Building Blocks in the Construction of Higher Order Assemblies through Axial Coordination of Bridging Ligands: Solution- and Solid-State Characterization of Molecular Sandwiches and Molecular Wires
Elisabetta Iengo; Ennio Zangrando; Romina Minatel; Enzo Alessio; Journal of the American Chemical Society 124 (2002) 1003–1013; doi:10.1021/ja016162s

data_4114609
_publ_section_title
;
 Metallacycles of Porphyrins as Building Blocks in the Construction of
 Higher Order Assemblies through Axial Coordination of Bridging Ligands:
 Solution- and Solid-State Characterization of Molecular Sandwiches and
 Molecular Wires
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1003
_journal_page_last               1013
_journal_paper_doi               10.1021/ja016162s
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety
'(C130 H78 Cl4 N18 O4 Ru2 Zn2) 3(C6 H14) 1.5(CH2 Cl2)'
_chemical_formula_sum            'C149.5 H125 Cl7 N18 O4 Ru2 Zn2'
_chemical_formula_weight         2815.00
_chemical_name_systematic
;
 bis([trans,cis,cis-RuCl2(CO)2(Zn.4'-cis-DpyP)]2) (mu-4'-trans-DpyP)2 solvated
       cis-DpyP =(5,10-bis(4'pyridyl)-15-20-diphenylporphyrin)
       trans-DpyP =(5,15-bis(4'pyridyl)-10-20-diphenylporphyrin)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.06(2)
_cell_angle_beta                 84.87(2)
_cell_angle_gamma                89.00(2)
_cell_formula_units_Z            2
_cell_length_a                   11.923(4)
_cell_length_b                   21.890(4)
_cell_length_c                   27.183(6)
_cell_measurement_temperature    100(2)
_cell_volume                     6599(3)
_computing_cell_refinement       'MOSFLM (Leslie, 1992)'
_computing_data_reduction        'MOSFLM (Leslie, 1992)'
_computing_molecular_graphics    'Ortep3/Windows (Farrugia,1997)'
_computing_publication_material  'WinGX 1.63 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  mar2000
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         'Elettra Synchrotron, Trieste (Italy)'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.000
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1112
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6465
_diffrn_reflns_theta_full        23.58
_diffrn_reflns_theta_max         23.58
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    1.896
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_F_000             2893
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0020(3)
_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   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         6465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1395
_refine_ls_R_factor_gt           0.0972
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2555
_refine_ls_wR_factor_ref         0.2912
_reflns_number_gt                3859
_reflns_number_total             6465
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja016162s_s3_2.cif
_cod_data_source_block           9
_cod_original_formula_sum        'C149.50 H125 Cl7 N18 O4 Ru2 Zn2'
_cod_database_code               4114609