Size and Charge Effect of Guest Cations in Formation of Polyoxopalladates: A Theoretical and Experimental Study
Lang, Zhongling; Yang, Peng; Lin, Zhengguo; Yan, Li-Kai; Li, Ming-Xing; Carbó, Jorge J.; Kortz, Ulrich; Poblet, Josep M.; Chem. Sci.  (2017) –; doi:10.1039/C7SC03441E

data_1547345
_publ_section_title
;
 Size and Charge Effect of Guest Cations in Formation of
 Polyoxopalladates: A Theoretical and Experimental Study
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC03441E
_journal_year                    2017
_chemical_formula_sum            'C42 H122 As6 La Na3 O73 Pd12'
_chemical_formula_weight         3729.59
_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-2014/6
_audit_update_record
;
2017-06-10 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                103.266(3)
_cell_angle_beta                 92.094(3)
_cell_angle_gamma                97.633(4)
_cell_formula_units_Z            1
_cell_length_a                   13.0985(9)
_cell_length_b                   16.2291(12)
_cell_length_c                   22.9839(14)
_cell_measurement_reflns_used    9467
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.83
_cell_volume                     4701.9(6)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD x8'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            160109
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.333
_diffrn_reflns_theta_min         1.303
_exptl_absorpt_coefficient_mu    2.453
_exptl_absorpt_correction_T_max  0.692
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             1798
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_refine_diff_density_max         5.252
_refine_diff_density_min         -4.815
_refine_diff_density_rms         0.695
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         23219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0845
_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^)+(0.1200P)^2^+195.7335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2376
_refine_ls_wR_factor_ref         0.2626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18151
_reflns_number_total             23219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03441e2.cif
_cod_data_source_block           try
_cod_database_code               1547345
_shelx_estimated_absorpt_t_min   0.640
_shelx_estimated_absorpt_t_max   0.710
_shelxl_version_number           2014/6
_shelx_res_checksum              97572