HL2[P(1,2-O2C6H4)3] (L = DMSO or DMF): A Convenient Proton Source with a Weakly Basic Phosphorus(V) Anion
Siu, Paul W.; Gates, Derek P.; Organometallics 28 (2009) 4491–; doi:10.1021/om9003187

data_4069632
_publ_section_title
;
 HL2[P(1,2-O2C6H4)3] (L = DMSO or DMF): A Convenient Proton Source with a
 Weakly Basic Phosphorus(V) Anion
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4491
_journal_paper_doi               10.1021/om9003187
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C30 H30 N2 P2 Pd, 2(C18 H12 O6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C70 H60 N4 O12 P4 Pd'
_chemical_formula_weight         1379.50
_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                81.711(5)
_cell_angle_beta                 83.998(5)
_cell_angle_gamma                68.021(5)
_cell_formula_units_Z            2
_cell_length_a                   12.1730(14)
_cell_length_b                   15.6728(18)
_cell_length_c                   18.0478(18)
_cell_measurement_reflns_used    15158
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      1.41
_cell_volume                     3154.8(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            67930
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         15158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+1.3829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                10862
_reflns_number_total             15158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9003187_si_001.cif
_cod_data_source_block           dg084_0m
_cod_database_code               4069632