py2P2S7: a bis(pyridine)adduct stabilized phosphorus sulfide
Rotter, Christiane; Evangelisti, Camilla; Schönberger, Stefanie; Klapötke, Thomas M.; Karaghiosoff, Konstantin; Chemical Communications 46 (2010) 5024–5025; doi:10.1039/c0cc00106f

data_7111653
_publ_section_title
;
 py2P2S7: a bis(pyridine)adduct stabilized phosphorus sulfide
;
_journal_issue                   27
_journal_name_full               'Chemical Communications'
_journal_page_first              5024
_journal_page_last               5025
_journal_paper_doi               10.1039/c0cc00106f
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C10 H10 N2 P2 S7'
_chemical_formula_sum            'C10 H10 N2 P2 S7'
_chemical_formula_weight         444.63
_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_date             01-09-2009
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.000(3)
_cell_length_b                   8.0185(16)
_cell_length_c                   17.332(4)
_cell_measurement_reflns_used    6173
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      3.134
_cell_volume                     1790.5(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       ' 95mm CCD camera on \k-goniostat'
_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  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11002
_diffrn_reflns_theta_full        25.29
_diffrn_reflns_theta_max         25.29
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0372P)^2^+1.1655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0980
_reflns_number_gt                2316
_reflns_number_total             3259
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            C0CC00106Fsup1.cif
_cod_data_source_block           v1
_cod_original_cell_volume        1790.5(6)
_cod_original_sg_symbol_Hall     ' -P 2ybc'
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        ' C10 H10 N2 P2 S7'
_cod_database_code               7111653