Facile Formation of Stable Tris(imido)phosphate Trianions as Their Tri- and Hexanuclear Pd(II) Complexes in Protic Solvents
Arvind K. Gupta; S. Arun Dixith Reddy; Ramamoorthy Boomishankar; Inorganic Chemistry 52 (2013) 7608–7614; doi:10.1021/ic400686e

data_4335361
_publ_section_title
;
 Facile Formation of Stable Tris(imido)phosphate Trianions as Their Tri-
 and Hexanuclear Pd(II) Complexes in Protic Solvents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7608
_journal_page_last               7614
_journal_paper_doi               10.1021/ic400686e
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C31 H64 N6 O16 P2 Pd6'
_chemical_formula_weight         1477.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 90.015(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.8019(16)
_cell_length_b                   18.678(2)
_cell_length_c                   38.140(4)
_cell_measurement_reflns_used    5188
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.18
_cell_volume                     10544.6(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Smart Apex II'
_diffrn_measurement_method       'phi and omega 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  0.0792
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            44465
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         4.11
_exptl_absorpt_coefficient_mu    2.125
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_description       plate
_exptl_crystal_F_000             5808
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.073
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       0.000194(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         9288
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0251P)^2^+106.2838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                8126
_reflns_number_total             9288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400686e_7.cif
_cod_data_source_block           compound7
_cod_original_cell_volume        10545(2)
_cod_database_code               4335361