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_4069630
_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         'C29 H30 N P2 Pd, C18 H12 O6 P, C2 H3 N'
_chemical_formula_sum            'C49 H45 N2 O6 P3 Pd'
_chemical_formula_weight         957.18
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 95.200(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0359(11)
_cell_length_b                   17.318(2)
_cell_length_c                   13.0347(16)
_cell_measurement_reflns_used    9813
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.9
_cell_measurement_theta_min      1.6
_cell_volume                     2256.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19836
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         9813
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+0.0849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0621
_reflns_number_gt                9433
_reflns_number_total             9813
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9003187_si_001.cif
_cod_data_source_block           dg092_0m
_cod_original_cell_volume        2256.2(5)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4069630