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_4306854
_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            'C36 H42 Co10 N5 O22 Rh'
_chemical_formula_weight         1588.96
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2005-07-20T17:47:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 102.22(2)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   17.223(4)
_cell_length_b                   14.600(2)
_cell_length_c                   22.326(6)
_cell_measurement_temperature    293(2)
_cell_volume                     5487(2)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.048418
_diffrn_orient_matrix_UB_12      -0.000268
_diffrn_orient_matrix_UB_13      -0.033799
_diffrn_orient_matrix_UB_21      -0.004547
_diffrn_orient_matrix_UB_22      -0.067771
_diffrn_orient_matrix_UB_23      0.004351
_diffrn_orient_matrix_UB_31      -0.03402
_diffrn_orient_matrix_UB_32      0.009337
_diffrn_orient_matrix_UB_33      0.030581
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.1136
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9644
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        14
_diffrn_standards_interval_time  240
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.306
_exptl_absorpt_correction_T_max  0.9998
_exptl_absorpt_correction_T_min  0.7031
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   1
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_size_rad          0.1
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.96
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         9644
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1799
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+8.8117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.163
_reflns_number_gt                4271
_reflns_number_total             9644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0608288si20060515_060827_3.cif
_cod_data_source_block           mart29
_cod_database_code               4306854