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_7131895
_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 Pd4 Si3, 2(C6 H6)'
_chemical_formula_sum            'C72 H96 Cl3 N6 P3 Pd4 Si3'
_chemical_formula_weight         1754.67
_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                80.8930(10)
_cell_angle_beta                 76.3520(10)
_cell_angle_gamma                76.1360(10)
_cell_formula_units_Z            2
_cell_length_a                   14.9430(12)
_cell_length_b                   15.0116(12)
_cell_length_c                   18.1731(14)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.45
_cell_measurement_theta_min      2.36
_cell_volume                     3823.6(5)
_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      120(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.980
_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  0.0716
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19376
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.464
_diffrn_reflns_theta_min         1.160
_diffrn_source                   'Bruker TXS fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.418
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         13903
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0695P)^2^+2.5060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12141
_reflns_number_total             13903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02543h2.cif
_cod_data_source_block           599
_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_database_code               7131895
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.806
_shelx_estimated_absorpt_t_max   0.852
_shelx_res_checksum              91349
_shelx_hkl_checksum              87879