Insertion of germanium atoms in high-nuclearity rhodium carbonyl compounds: synthesis, characterization and preliminary biological activity of the heterometallic [Rh13Ge(CO)25]3-, [Rh14Ge2(CO)30]2- and [Rh12Ge(CO)27]4- cluster anions.
Boccalini, Alberto; Dyson, Paul; Femoni, Cristina; Iapalucci, Maria Carmela; Ruggieri, Silvia; Zacchini, Stefano; Dalton Transactions  (2018) –; doi:10.1039/C8DT02466A

data_7047228
_publ_section_title
;
 Insertion of germanium atoms in high-nuclearity rhodium carbonyl
 compounds: synthesis, characterization and preliminary biological
 activity of the heterometallic [Rh13Ge(CO)25]3-, [Rh14Ge2(CO)30]2- and
 [Rh12Ge(CO)27]4- cluster anions.
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT02466A
_journal_year                    2018
_chemical_formula_sum            'C63 H86 Ge N6 O27 Rh12'
_chemical_formula_weight         2666.88
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-06-13 deposited with the CCDC.
2018-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                119.285(3)
_cell_angle_beta                 98.012(4)
_cell_angle_gamma                95.078(4)
_cell_formula_units_Z            4
_cell_length_a                   13.279(3)
_cell_length_b                   26.614(5)
_cell_length_c                   27.049(5)
_cell_measurement_reflns_used    9377
_cell_measurement_temperature    77(2)
_cell_measurement_theta_max      33.500
_cell_measurement_theta_min      2.326
_cell_volume                     8119(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'CMOS AREA DETECTOR'
_diffrn_measurement_method       'OMEGA SCANS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            76284
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.521
_exptl_absorpt_coefficient_mu    2.810
_exptl_absorpt_correction_type   'EMPIRICAL SADABS'
_exptl_crystal_colour            BLACK
_exptl_crystal_density_diffrn    2.182
_exptl_crystal_description       PRISMATIC
_exptl_crystal_F_000             5176
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.690
_exptl_transmission_factor_min   0.570
_refine_diff_density_max         2.892
_refine_diff_density_min         -2.092
_refine_diff_density_rms         0.295
_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     2029
_refine_ls_number_reflns         27668
_refine_ls_number_restraints     658
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+646.3442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2044
_refine_ls_wR_factor_ref         0.2114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26055
_reflns_number_total             27668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02466a2.cif
_cod_data_source_block           P-1
_cod_database_code               7047228
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.603
_shelx_estimated_absorpt_t_max   0.729
_shelx_res_checksum              51206