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_7703928
_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            'C156 H240 N6 Ni21.37 O52 Pd20.63'
_chemical_formula_weight         6481.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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                 119.3140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.6411(12)
_cell_length_b                   17.6379(6)
_cell_length_c                   33.0067(17)
_cell_measurement_reflns_used    9497
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.5345
_cell_measurement_theta_min      2.5415
_cell_volume                     19615.1(14)
_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 0.996
_diffrn_measured_fraction_theta_max 0.990
_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  0.0510
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            149731
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.692
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.902
_exptl_absorpt_correction_T_max  0.3380
_exptl_absorpt_correction_T_min  0.2308
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1514 (selected reflections only, before parameter refinement)
 R(int) = 0.0648 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.195
_exptl_crystal_description       prism
_exptl_crystal_F_000             12725
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_refine_diff_density_max         3.595
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1129
_refine_ls_number_reflns         21214
_refine_ls_number_restraints     445
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0246P)^2^+451.1749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17542
_reflns_number_total             21214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00337a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7703928--7703930.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7703928
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.495
_shelx_estimated_absorpt_t_max   0.611
_shelx_res_checksum              8567