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_7047229
_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            'C46 H40 Ge2 N2 O30 Rh14'
_chemical_formula_weight         2686.72
_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                112.059(2)
_cell_angle_beta                 98.082(2)
_cell_angle_gamma                94.045(3)
_cell_formula_units_Z            1
_cell_length_a                   11.4246(4)
_cell_length_b                   11.5375(4)
_cell_length_c                   13.4617(5)
_cell_measurement_reflns_used    1639
_cell_measurement_temperature    77(2)
_cell_measurement_theta_max      24.00
_cell_measurement_theta_min      2.228
_cell_volume                     1613.40(10)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD AREA DETECTOR'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1320
_diffrn_reflns_av_unetI/netI     0.1224
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23355
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.660
_exptl_absorpt_coefficient_mu    4.474
_exptl_absorpt_correction_type   'EMPIRICAL SADABS'
_exptl_crystal_colour            BLACK
_exptl_crystal_density_diffrn    2.765
_exptl_crystal_description       PRISMATIC
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.130
_exptl_transmission_factor_max   0.60
_exptl_transmission_factor_min   0.40
_refine_diff_density_max         2.397
_refine_diff_density_min         -1.639
_refine_diff_density_rms         0.311
_refine_ls_extinction_coef       0.00067(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         5690
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3391
_reflns_number_total             5690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02466a2.cif
_cod_data_source_block           P-1_CCDC1
_cod_database_code               7047229
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.500
_shelx_estimated_absorpt_t_max   0.594
_shelx_res_checksum              18668