Construction of a Planar Tetrapalladium Cluster by the Reaction of Palladium(0) Bis(isocyanide) with Cyclic Tetrasilane
Sunada, Y.; Taniyama, N.; Shimamoto, K.; Kyushin, S.; Nagashima, H.; Inorganics 5 (2017) 84–; doi:10.3390/inorganics5040084

data_1556554
_publ_section_title
;
 Construction of a Planar Tetrapalladium Cluster by the Reaction of
 Palladium(0) Bis(isocyanide) with Cyclic Tetrasilane
;
_journal_name_full               Inorganics
_journal_page_first              84
_journal_paper_doi               10.3390/inorganics5040084
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety         'C38 H78 N4 Pd4 Si3'
_chemical_formula_sum            'C38 H78 N4 Pd4 Si3'
_chemical_formula_weight         1100.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.1391(12)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.8179(6)
_cell_length_b                   22.0783(12)
_cell_length_c                   22.8654(12)
_cell_measurement_reflns_used    20078
_cell_measurement_temperature    193
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.25
_cell_volume                     5457.4(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.2.5'
_computing_publication_material  'CrystalStructure 4.2.5 (Rigaku, 2017)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      193
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            77678
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         3.144
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.389
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2240.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.30
_refine_diff_density_min         -0.81
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     470
_refine_ls_number_reflns         12489
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0898P)^2^+12.9959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1518
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11907
_reflns_number_total             12489
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            Inorganics-2017-5-84.cif
_cod_data_source_block           Pd4Si3(CNtBu)4
_cod_database_code               1556554
_shelxl_version_number           2014-1
_shelx_res_checksum              17393
_shelx_hkl_checksum              8119