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_4317404
_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)14(H2N(CH2)4)NH2)Rh5(CO)14]2- 2[P(C6H5)4]+'
_chemical_formula_sum            'C80 H52 N2 O28 P2 Rh10'
_chemical_formula_weight         2580.29
_chemical_name_systematic        ?
_space_group_IT_number           13
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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      2.2
_audit_creation_date             2001-07-16T08:49:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 110.230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.209(3)
_cell_length_b                   9.8300(10)
_cell_length_c                   23.683(3)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     5069.8(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      571(2)
_diffrn_detector                 CCD
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_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  0.0536
_diffrn_reflns_av_unetI/netI     0.058
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12830
_diffrn_reflns_theta_full        29.3
_diffrn_reflns_theta_max         29.3
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    1.691
_exptl_absorpt_correction_T_max  0.8491
_exptl_absorpt_correction_T_min  0.7285
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
          nn
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2740
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         12830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+5.1710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0944
_reflns_number_gt                8039
_reflns_number_total             12830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0107936_1.cif
_cod_data_source_block           compound_1
_cod_database_code               4317404