Synthesis of a homoleptic tris(silylene)-palladium(0) complex and a silylyne-bridged tetranuclear palladium cluster
Sekiguchi, Jueri; Kazama, Yugo; Ishii, Akihiko; Nakata, Norio; Chemical Communications  (2023) –; doi:10.1039/D3CC02543H

data_7131894
_publ_section_title
;
 Synthesis of a homoleptic tris(silylene)-palladium(0) complex and a
 silylyne-bridged tetranuclear palladium cluster
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC02543H
_journal_year                    2023
_chemical_formula_moiety         'C60 H84 Cl3 N6 P3 Pd Si3'
_chemical_formula_sum            'C60 H84 Cl3 N6 P3 Pd Si3'
_chemical_formula_weight         1279.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2023-05-01 deposited with the CCDC.	2023-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                108.610(3)
_cell_angle_beta                 104.396(3)
_cell_angle_gamma                100.007(3)
_cell_formula_units_Z            2
_cell_length_a                   15.160(3)
_cell_length_b                   15.382(3)
_cell_length_c                   15.980(3)
_cell_measurement_reflns_used    2200
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.20
_cell_measurement_theta_min      2.20
_cell_volume                     3288.1(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1778
_diffrn_reflns_av_unetI/netI     0.2205
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16599
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.422
_diffrn_reflns_theta_min         1.443
_diffrn_source                   'Bruker TXS fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.9775
_exptl_absorpt_correction_T_min  0.9397
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.804
_refine_diff_density_min         -1.375
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         11884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0709
_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^)+(0.0065P)^2^+0.0001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1495
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6523
_reflns_number_total             11884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02543h2.cif
_cod_data_source_block           534
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        3288.2(11)
_cod_database_code               7131894
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.940
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              33382
_shelx_hkl_checksum              382