Dimetalated Crown Ether Schiff Base Palladacycles. Influence of the Carbon Chain Length on the Coordination Mode of Bidentate Phosphines. Crystal and Molecular Structure of the Novel Complex [Pd2{1,4-[C(H)═N{9,10-(C8H16O5)C6H3}]2C6H2-C2,C5}(Cl)2{μ-Ph2P(CH2)5PPh2}2]
Fernández, Alberto; López-Torres, Margarita; Castro-Juiz, Samuel; Merino, Manuel; Vázquez-García, Digna; Vila, José M.; Fernández, Jesús J.; Organometallics 30 (2011) 386–; doi:10.1021/om100833w

data_4063678
_publ_section_title
;
 Dimetalated Crown Ether Schiff Base Palladacycles. Influence of the
 Carbon Chain Length on the Coordination Mode of Bidentate Phosphines.
 Crystal and Molecular Structure of the Novel Complex
 [Pd2{1,4-[C(H)&#x2550;N{9,10-(C8H16O5)C6H3}]2C6H2-C2,C5}(Cl)2{\m-Ph2P(CH2)5PPh2}2]
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              386
_journal_paper_doi               10.1021/om100833w
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C106.5 H110.5 Cl9.5 N2 O10 P6 Pd2'
_chemical_formula_weight         2313.86
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.1080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.0430(2)
_cell_length_b                   16.6127(3)
_cell_length_c                   22.0454(2)
_cell_measurement_temperature    293(2)
_cell_volume                     5852.15(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart 1k'
_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  0.0733
_diffrn_reflns_av_sigmaI/netI    0.0914
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30971
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2374
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.581
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         10285
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.0658
_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^)+(0.1026P)^2^+6.5965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1764
_refine_ls_wR_factor_ref         0.2107
_reflns_number_gt                6240
_reflns_number_total             10285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100833w_si_001.cif
_cod_data_source_block           13a
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C106.50 H110.50 Cl9.50 N2 O10 P6 Pd2'
_cod_database_code               4063678