Synthesis and Structural Characterization of the {[Rh5(CO)14]-(H2N(CH2)4NH2)-[Rh5(CO)14])}2- and [Rh5(CO)13(H2N(CH2)2NH2)]- Anions (as [PPh4]+ Salts): An Unprecedented Example of Carbonyl Substitution by Alkylamines in a Homoleptic Metal Carbonyl Cluster Anion
Alessandro Fumagalli; Maria Carlotta Malatesta; Anna Tentori; Diego Monti; Piero Macchi; Angelo Sironi; Inorganic Chemistry 41 (2002) 76–85; doi:10.1021/ic0107936

data_4317405
_publ_section_title
;
 Synthesis and Structural Characterization of the
 {[Rh5(CO)14]-(H2N(CH2)4NH2)-[Rh5(CO)14])}2- and
 [Rh5(CO)13(H2N(CH2)2NH2)]- Anions (as [PPh4]+ Salts): An Unprecedented
 Example of Carbonyl Substitution by Alkylamines in a Homoleptic Metal
 Carbonyl Cluster Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              76
_journal_page_last               85
_journal_paper_doi               10.1021/ic0107936
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         '[Rh5(CO)13(H2N(CH2)2NH2)]- [P(C6H5)4]+ THF'
_chemical_formula_sum            'C43 H36 N2 O14 P Rh5'
_chemical_formula_weight         1350.26
_chemical_name_systematic        ?
_space_group_IT_number           2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2001-07-16T08:29:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                99.940(10)
_cell_angle_beta                 101.400(10)
_cell_angle_gamma                106.300(10)
_cell_formula_units_Z            2
_cell_length_a                   11.999(2)
_cell_length_b                   12.760(2)
_cell_length_c                   16.919(2)
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      25.
_cell_measurement_theta_min      3.
_cell_volume                     2364.5(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      233(2)
_diffrn_detector                 CCD
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device       Diffractometer
_diffrn_measurement_device_type  SMART-CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27376
_diffrn_reflns_theta_full        29.24
_diffrn_reflns_theta_max         29.24
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    1.808
_exptl_absorpt_correction_T_max  0.8399
_exptl_absorpt_correction_T_min  0.6607
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   dd
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.842
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         11515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.842
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.045
_reflns_number_gt                8299
_reflns_number_total             11515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0107936_2.cif
_cod_data_source_block           compound_2
_cod_database_code               4317405