Pyridylporphyrins peripherally coordinated to ruthenium-nitrosyls, including the water-soluble Na4[Zn·4′TPyP{RuCl4(NO)}4]: synthesis and structural characterization
Gianferrara, Teresa; Serli, Barbara; Zangrando, Ennio; Iengo, Elisabetta; Alessio, Enzo; New Journal of Chemistry 29 (2005) 895–; doi:10.1039/b418855a

data_7050080
_publ_section_title
;
 Pyridylporphyrins peripherally coordinated to ruthenium-nitrosyls,
 including the water-soluble Na4[Zn&#x00B7;4&#x2032;TPyP{RuCl4(NO)}4]:
 synthesis and structural characterization
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              895
_journal_paper_doi               10.1039/b418855a
_journal_volume                  29
_journal_year                    2005
_chemical_formula_moiety
'C40 H26 Cl16 N12 O4 Ru4, 4(C16 H36 N1) 2(C1 H3 N1 O2) 0.5(C4 H10 O1)'
_chemical_formula_sum            'C108 H181 Cl16 N18 O8.5 Ru4'
_chemical_formula_weight         2839.19
_chemical_name_systematic
;
(5,10,15,20-(4'pyridyl)-porphyrin)-tetra-(tetrachloro-nitrosyl-ruthenate(III))
tetra(tetrabutylamonium) bis(nitromethane) diethylether solvate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 103.49(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   38.252(6)
_cell_length_b                   8.936(3)
_cell_length_c                   40.475(6)
_cell_measurement_temperature    100(2)
_cell_volume                     13453(6)
_computing_cell_refinement       'Mosflm (Acta Cryst. D50, 760, 1994)'
_computing_data_reduction        'Scala (Acta Cryst. D50, 760, 1994)'
_computing_molecular_graphics    'Ortep3/windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.64.04 (Farrugia, 1999)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELX97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device_type  'CCD MarResearch'
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         'Elettra Synchrotron, Trieste (Italy)'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.0000
_diffrn_reflns_av_R_equivalents  0.0840
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            32476
_diffrn_reflns_theta_full        30.78
_diffrn_reflns_theta_max         30.78
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    2.203
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5884
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         11985
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0646P)^2^+82.8504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1541
_reflns_number_gt                11713
_reflns_number_total             11985
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b418855a.txt
_cod_data_source_block           5
_cod_original_cell_volume        13453(5)
_cod_original_sg_symbol_H-M      'C c'
_cod_original_formula_sum        'C108 H181 Cl16 N18 O8.50 Ru4'
_cod_database_code               7050080