Synthesis and Structure of Multinuclear Pd(II) Complexes Bridged by Phosphide or Azide Ligands.
Takeuchi, Katsuhiko; Kim, Kun-Woo; Kim, Yong-Joo; Fukaya, Norihisa; Sato, Kazuhiko; Choi, Jun-Chul; ACS omega 5 (2020) 29706–29713; doi:10.1021/acsomega.0c03317

data_4518221
_publ_section_title
;
 Synthesis and Structure of Multinuclear Pd(II) Complexes Bridged by
 Phosphide or Azide Ligands.
;
_journal_issue                   46
_journal_name_full               'ACS omega'
_journal_page_first              29706
_journal_page_last               29713
_journal_paper_doi               10.1021/acsomega.0c03317
_journal_volume                  5
_journal_year                    2020
_chemical_formula_moiety         'C32 H44 N24 P4 Pd4, 2(C7 H8)'
_chemical_formula_sum            'C46 H60 N24 P4 Pd4'
_chemical_formula_weight         1498.66
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.5646(2)
_cell_length_b                   13.30840(10)
_cell_length_c                   38.4626(3)
_cell_measurement_reflns_used    173476
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      30.9920
_cell_measurement_theta_min      2.1020
_cell_volume                     12062.15(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'CCD plate'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            171548
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.728
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       Block
_exptl_crystal_F_000             5984
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.160
_refine_diff_density_max         2.216
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Flack x determined using 9983 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.176(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1490
_refine_ls_number_reflns         21194
_refine_ls_number_restraints     1987
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0464P)^2^+43.8388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                21028
_reflns_number_total             21194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c03317_si_007.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4518217--4518222.cif.'
_cod_database_code               4518221
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.675
_shelx_estimated_absorpt_t_max   0.815
_shelx_res_checksum              64796
_shelx_hkl_checksum              64591