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_4069628
_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         'C18 H12 O6 P, C4 H13 S2'
_chemical_formula_sum            'C22 H25 O8 P S2'
_chemical_formula_weight         512.51
_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                 108.507(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.767(3)
_cell_length_b                   13.932(3)
_cell_length_c                   13.625(3)
_cell_measurement_reflns_used    5370
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.9
_cell_volume                     2298.1(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39445
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          1.1
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0354P)^2^+1.0160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                4293
_reflns_number_total             5373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9003187_si_001.cif
_cod_data_source_block           dg053_0m
_cod_original_cell_volume        2298.2(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4069628