Mixed Co-Rh Nitrido-Encapsulated Carbonyl Clusters. Synthesis, Solid-State Structure, and Electrochemical/EPR Characterization of the Anions [Co10Rh(N)2(CO)21]3-, [Co10Rh2(N)2(CO)24]2-, and [Co11Rh(N)2(CO)24]2-
Michela Costa; Roberto Della Pergola; Alessandro Fumagalli; Franco Laschi; Serena Losi; Piero Macchi; Angelo Sironi; Piero Zanello; Inorganic Chemistry 46 (2007) 552–560; doi:10.1021/ic0608288

data_4306852
_publ_section_title
;
Mixed Co-Rh Nitrido-Encapsulated Carbonyl Clusters. Synthesis,
Solid-State Structure, and Electrochemical/EPR Characterization of the
Anions [Co10Rh(N)2(CO)21]3-, [Co10Rh2(N)2(CO)24]2-, and [Co11Rh(N)2(CO)24]2-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              552
_journal_page_last               560
_journal_paper_doi               10.1021/ic0608288
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C38 H24 Co11 N4 O26 Rh'
_chemical_formula_weight         1703.75
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2005-07-20T17:38:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 109.740(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   23.608(5)
_cell_length_b                   11.054(5)
_cell_length_c                   22.550(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5539(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.92
_diffrn_measured_fraction_theta_max 0.92
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4486
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    3.573
_exptl_absorpt_correction_T_max  0.3746
_exptl_absorpt_correction_T_min  0.3643
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
        Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
        for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
        p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
        A31,146-148) is used with some modification.
;
_exptl_crystal_density_diffrn    2.043
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3320
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_crystal_size_rad          0.2
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4486
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.025
_refine_ls_shift/su_max          0.06
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+9.2287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                3800
_reflns_number_total             4486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0608288si20060515_060827_1.cif
_cod_data_source_block           mart28
_cod_database_code               4306852