Reactivity and Spectroscopy of the {Ru(DMAP)5} Fragment: An {Ru(NH3)5} Analogue
Melina B. Rossi; Oscar E. Piro; Eduardo E. Castellano; Pablo Alborés; Luis M. Baraldo; Inorganic Chemistry 47 (2008) 2416–2427; doi:10.1021/ic7016352

data_4304164
_publ_contact_author
;
       Luis M. Baraldo
       Departamento de Qu\'imica Inorg\'anica, Anal\'itica y Qu\'imica F\'isica
       INQUIMAE, Facultad de Ciencias Exactas y Naturales
       Universidad de Buenos Aires
       Pabell\'on 2, Ciudad Universitaria
       C1428EHA Buenos Aires 
       Argentina
;
_publ_contact_author_email       baraldo@qi.fcen.uba.ar
_publ_contact_author_fax         '54 11 4576 3341'
_publ_contact_author_phone       '54 11 4576 3380'
_publ_section_title
;
Reactivity and Spectroscopy of the {Ru(DMAP)5} Fragment: An {Ru(NH3)5}
Analogue
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2416
_journal_page_last               2427
_journal_paper_doi               10.1021/ic7016352
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C54 H96 Cl2 N12 O6 Ru'
_chemical_formula_weight         1181.40
_chemical_name_systematic
; 
 Hexakis(4-dimethylaminopyridine)ruthenium(II) chloride ethanol solvate 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   16.373(1)
_cell_length_b                   16.373(1)
_cell_length_c                   20.311(1)
_cell_measurement_reflns_used    10694
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      3.04
_cell_volume                     4715.4(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD with \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10694
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements Sortav (Blessing 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1890
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+10.1456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0780
_reflns_number_gt                1952
_reflns_number_total             2056
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic7016352-file001.cif
_cod_data_source_block           s97
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4304164