The chelate-to-bridging shift of phosphane dipalladacycles: convenient synthesis of double A-frame tetranuclear complexes.
Frieiro-Gomis, Pablo; Lucio-Martínez, Fátima; Munín-Cruz, Paula; Ortigueira, Juan M.; Pereira, M. Teresa; Polo-Ces, Paula; Vázquez-García, Digna; Vila, José M; Chemical communications (Cambridge, England) 54 (2018) 2662–2665; doi:10.1039/c8cc01046c

data_7121301
_publ_section_title
;
 The chelate-to-bridging shift of phosphane dipalladacycles: convenient
 synthesis of double A-frame tetranuclear complexes.
;
_journal_issue                   21
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2662
_journal_page_last               2665
_journal_paper_doi               10.1039/c8cc01046c
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C173 H163 Cl8 F12 N4 O18 P10 Pd4 S2'
_chemical_formula_weight         3897.09
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-07-26 deposited with the CCDC.
2018-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.090(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.8431(11)
_cell_length_b                   26.413(2)
_cell_length_c                   22.3504(19)
_cell_measurement_reflns_used    1138
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.100
_cell_measurement_theta_min      4.711
_cell_volume                     8749.8(12)
_computing_cell_refinement       ' SAINT V7.68A (Bruker: Madison, 2009 )'
_computing_data_collection       'Apex2, Bruker Instrument Service v2010'
_computing_data_reduction        'SAINT and XPREP Version 2008/2 (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 apex'
_diffrn_measurement_method       'omega-phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2121
_diffrn_reflns_av_sigmaI/netI    0.1524
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            87544
_diffrn_reflns_theta_full        24.43
_diffrn_reflns_theta_max         24.43
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2008/1 (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3966
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.323
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1074
_refine_ls_number_reflns         14410
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1533
_refine_ls_R_factor_gt           0.0773
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1389P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1950
_refine_ls_wR_factor_ref         0.2570
_reflns_number_gt                7751
_reflns_number_total             14410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8cc01046c2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7121301--7121303.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7121301