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_7121302
_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_moiety
'C164 H144 Cl2 N4 O14 P8 Pd4, 2(F6 P), 4(C3 H6), 4(O), 2(H2 O) '
_chemical_formula_sum            'C176 H172 Cl2 F12 N4 O20 P10 Pd4'
_chemical_formula_weight         3697.37
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-26 deposited with the CCDC.
2018-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                82.897(2)
_cell_angle_beta                 71.882(2)
_cell_angle_gamma                75.240(2)
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_cell_length_b                   16.5332(6)
_cell_length_c                   17.1548(5)
_cell_measurement_reflns_used    1981
_cell_measurement_temperature    97(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.56
_cell_volume                     4295.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      97(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            140354
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.275
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.9010
_exptl_absorpt_correction_T_min  0.8216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.250
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_exptl_crystal_size_min          0.160
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_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1046
_refine_ls_number_reflns         15101
_refine_ls_number_restraints     774
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+7.1466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13014
_reflns_number_total             15101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01046c2.cif
_cod_data_source_block           shelxcl_x
_cod_depositor_comments
'Adding full bibliography for 7121301--7121303.cif.'
_cod_database_code               7121302
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.908
_shelx_res_checksum              58875
_platon_squeeze_void_probe_radius 1.20