Chiral Dodecanuclear Palladium(II) Thio Cluster: Synthesis, Structure, and Formation Mechanism Explored by ESI-MS and DFT Calculations.
Lin, Zheng-Guo; Fan, Lin-Yuan; Kondinski, Aleksandar; Vankova, Nina; Heine, Thomas; Chen, Bao-Kuan; Haider, Ali; Wang, Bo; Kortz, Ulrich; Hu, Chang-Wen; Inorganic chemistry 55 (2016) 7811–7813; doi:10.1021/acs.inorgchem.6b01005

data_4348134
_publ_section_title
;
 Chiral Dodecanuclear Palladium(II) Thio Cluster: Synthesis, Structure,
 and Formation Mechanism Explored by ESI-MS and DFT Calculations.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7811
_journal_page_last               7813
_journal_paper_doi               10.1021/acs.inorgchem.6b01005
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_sum            'C72 H239 La N24 O97 Pd12 S24'
_chemical_formula_weight         5179.01
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                89.5650(10)
_cell_angle_beta                 74.3200(10)
_cell_angle_gamma                83.0720(10)
_cell_formula_units_Z            1
_cell_length_a                   13.2873(7)
_cell_length_b                   15.6841(8)
_cell_length_c                   23.4478(13)
_cell_measurement_reflns_used    8076
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.52
_cell_volume                     4668.7(4)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX 2 DUO'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23220
_diffrn_reflns_point_group_measured_fraction_full 0.569
_diffrn_reflns_point_group_measured_fraction_max 0.583
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_min         0.902
_exptl_absorpt_coefficient_mu    1.715
_exptl_absorpt_correction_T_max  0.710
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_description       plate
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.356
_refine_diff_density_min         -3.538
_refine_diff_density_rms         0.448
_refine_ls_abs_structure_details
;
 Flack x determined using 2540 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     931
_refine_ls_number_reflns         19201
_refine_ls_number_restraints     2567
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0835
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2100P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2474
_refine_ls_wR_factor_ref         0.2671
_reflns_Friedel_coverage         0.193
_reflns_Friedel_fraction_full    0.184
_reflns_Friedel_fraction_max     0.189
_reflns_number_gt                16572
_reflns_number_total             19201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01005_si_001.cif
_cod_data_source_block           11_sq_d
_cod_database_code               4348134
_shelx_estimated_absorpt_t_min   0.593
_shelx_estimated_absorpt_t_max   0.725
_shelxl_version_number           2014/6
_shelx_res_checksum              81194
_shelx_hkl_checksum              44559