Synthesis and structure of tetranuclear orthometallated Pd(ii) complexes derived from bis-iminophosphoranes
Bielsa, Raquel; Navarro, Rafael; Soler, Tatiana; Urriolabeitia, Esteban P.; Dalton Transactions  (2008) 1787–1794; doi:10.1039/b718108f

data_7003659
_publ_section_title
;
 Synthesis and structure of tetranuclear orthometallated Pd(ii)
 complexes derived from bis-iminophosphoranes
;
_journal_issue                   13
_journal_name_full               'Dalton Transactions'
_journal_page_first              1787
_journal_page_last               1794
_journal_paper_doi               10.1039/b718108f
_journal_year                    2008
_chemical_formula_moiety         'C54 H46 N2 O6 P2 Pd2, 4(C H Cl3)'
_chemical_formula_sum            'C58 H50 Cl12 N2 O6 P2 Pd2'
_chemical_formula_weight         1571.14
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.1952(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.64371(14)
_cell_length_b                   29.8167(3)
_cell_length_c                   13.64503(9)
_cell_measurement_reflns_used    36628
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      32.66
_cell_measurement_theta_min      3.78
_cell_volume                     6364.60(10)
_computing_cell_refinement
;
CrysAlis RED (Oxford, 2005)
;
_computing_data_collection
;
CrysAlis CCD (Oxford, 2005)
;
_computing_data_reduction
;
CrysAlis RED (Oxford, 2005)
;
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'SIR92 (Altomare, Cascarano, Giacovazzo & Guagliardi, 1993)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            88744
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.63
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 120
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.169
_exptl_absorpt_correction_T_max  0.9468
_exptl_absorpt_correction_T_min  0.7934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker/Siemens SADABS V2.03'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.109
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         11159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+32.9488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1432
_reflns_number_gt                9970
_reflns_number_total             11159
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b718108f.txt
_cod_data_source_block           sq2c
_cod_original_sg_symbol_H-M      'P 2(1)/n'
_cod_database_code               7003659