Complex salts of Pd(ii) and Pt(ii) with Co(ii) and Ni(ii) aqua-cations as single-source precursors for bimetallic nanoalloys and mixed oxides
Zadesenets, Andrey V.; Filatov, Evgeniy Yu.; Plyusnin, Pavel E.; Asanova, Tatyana I.; Korolkov, Ilya V.; Baidina, Iraida A.; Shlyakhova, Elena V.; Asanov, Igor P.; Korenev, Sergey V.; New Journal of Chemistry 42 (2018) 8843–; doi:10.1039/C8NJ00956B

data_7057342
_publ_section_title
;
 Complex salts of Pd(ii) and Pt(ii) with Co(ii) and Ni(ii) aqua-cations as
 single-source precursors for bimetallic nanoalloys and mixed oxides
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8843
_journal_paper_doi               10.1039/C8NJ00956B
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'Co H16 N4 O16 Pd'
_chemical_formula_weight         493.50
_chemical_name_common            'cobalt(II) nitropalladate octahydrate'
_chemical_name_systematic
'hexaaquacobalt(II) tetranitropalladate(II) dihydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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   difmap
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2017-12-10 deposited with the CCDC.
2018-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                110.055(2)
_cell_angle_beta                 105.100(3)
_cell_angle_gamma                96.203(3)
_cell_formula_units_Z            1
_cell_length_a                   6.0051(3)
_cell_length_b                   7.8865(4)
_cell_length_c                   8.6872(5)
_cell_measurement_reflns_used    5475
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.15
_cell_measurement_theta_min      2.63
_cell_volume                     364.18(3)
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8 Apex'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9020
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.170
_diffrn_reflns_theta_min         3.600
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.465
_exptl_absorpt_correction_T_max  0.7087
_exptl_absorpt_correction_T_min  0.6938
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            ruby
_exptl_crystal_density_diffrn    2.250
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             245
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_coef       0.023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         5211
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          1.431
_refine_ls_shift/su_mean         0.316
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0495
_reflns_Friedel_coverage         0.874
_reflns_Friedel_fraction_full    0.942
_reflns_Friedel_fraction_max     0.872
_reflns_number_gt                4800
_reflns_number_total             5211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj00956b2.cif
_cod_data_source_block           CoPd
_cod_depositor_comments
'Adding full bibliography for 7057339--7057343.cif.'
_cod_database_code               7057342
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.694
_shelx_estimated_absorpt_t_max   0.709
_shelx_res_checksum              87057