O,O'-Diester Methylenediphosphonotetrathioate: Synthesis, Characterization, and Potential Applications
Aviran Amir; Alon H. Sayer; Rostislav Zagalsky; Linda J. W. Shimon; Bilha Fischer; Journal of Organic Chemistry 78 (2013) 270–277; doi:10.1021/jo301786m

data_4027838
_publ_section_title
;
 O,O'-Diester Methylenediphosphonotetrathioate: Synthesis,
 Characterization, and Potential Applications
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              270
_journal_page_last               277
_journal_paper_doi               10.1021/jo301786m
_journal_volume                  78
_journal_year                    2013
_chemical_formula_moiety         'C5 H10 P2 S6'
_chemical_formula_sum            'C5 H10 P2 S6'
_chemical_formula_weight         324.43
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 104.8996(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1901(2)
_cell_length_b                   13.8414(2)
_cell_length_c                   10.0300(2)
_cell_measurement_reflns_used    2670
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     1232.96(4)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Collect package (Bruker Nonius)'
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11012
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       needle
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+1.6038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                2496
_reflns_number_total             2810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo301786m_si_002.cif
_cod_data_source_block           aa68
_cod_database_code               4027838