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_4063677
_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            'C98 H112 Cl2 N2 O11 P4 Pd2'
_chemical_formula_weight         1901.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.1430(10)
_cell_angle_beta                 77.1560(10)
_cell_angle_gamma                76.2070(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0434(2)
_cell_length_b                   15.7309(2)
_cell_length_c                   23.69520(10)
_cell_measurement_temperature    293(2)
_cell_volume                     4602.46(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Smarta 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  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            54640
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         0.88
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_T_max  0.9333
_exptl_absorpt_correction_T_min  0.8023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         22500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+2.6510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                16277
_reflns_number_total             22500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100833w_si_001.cif
_cod_data_source_block           11a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        4602.46(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063677