Redox active Ni-Pd carbonyl alloy nanoclusters: syntheses, molecular structures and electrochemistry of [Ni<sub>22-x</sub>Pd<sub>20+x</sub>(CO)<sub>48</sub>]<sup>6-</sup> (x = 0.62), [Ni<sub>29-x</sub>Pd<sub>6+x</sub>(CO)<sub>42</sub>]<sup>6-</sup> (x = 0.09) and [Ni<sub>29+x</sub>Pd<sub>6-x</sub>(CO)<sub>42</sub>]<sup>6-</sup> (x = 0.27).
Berti, Beatrice; Cesari, Cristiana; Femoni, Cristina; Funaioli, Tiziana; Iapalucci, Maria Carmela; Zacchini, Stefano; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5513–5522; doi:10.1039/d0dt00337a

data_7703930
_publ_section_title
;
 Redox active Ni-Pd carbonyl alloy nanoclusters: syntheses, molecular
 structures and electrochemistry of
 [Ni<sub>22-x</sub>Pd<sub>20+x</sub>(CO)<sub>48</sub>]<sup>6-</sup> (x =
 0.62), [Ni<sub>29-x</sub>Pd<sub>6+x</sub>(CO)<sub>42</sub>]<sup>6-</sup>
 (x = 0.09) and
 [Ni<sub>29+x</sub>Pd<sub>6-x</sub>(CO)<sub>42</sub>]<sup>6-</sup> (x =
 0.27).
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5513
_journal_page_last               5522
_journal_paper_doi               10.1039/d0dt00337a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C95 H129 N9 Ni28.91 O42 Pd6.09'
_chemical_formula_weight         4414.11
_space_group_crystal_system      trigonal
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-01-28 deposited with the CCDC.	2020-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   18.0295(15)
_cell_length_b                   18.0295(15)
_cell_length_c                   23.386(2)
_cell_measurement_reflns_used    9501
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.2145
_cell_measurement_theta_min      2.259
_cell_volume                     6583.5(10)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'SCHAKAL99 (Keller, 1999)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'PHOTON2 area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            103805
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.045
_diffrn_reflns_theta_max         25.045
_diffrn_reflns_theta_min         2.176
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.903
_exptl_absorpt_correction_T_max  0.2612
_exptl_absorpt_correction_T_min  0.1241
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1680 (selected reflections only, before parameter refinement)
 R(int) = 0.0808 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.227
_exptl_crystal_description       prism
_exptl_crystal_F_000             4375
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.660
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3889
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.1011
_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^)+(0.0516P)^2^+219.6175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2246
_refine_ls_wR_factor_ref         0.2390
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3153
_reflns_number_total             3889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00337a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7703928--7703930.cif.'
_cod_original_cell_volume        6583.6(12)
_cod_database_code               7703930
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.412
_shelx_estimated_absorpt_t_max   0.547
_shelx_res_checksum              50735
_shelx_fab_checksum              44947