The activation of Woollins' reagent. Isolation of pyridine stabilised PhPSe2
Laura Ascherl; Andreas Nordheider; Kasun S. Athukorala Arachchige; David B. Cordes; Konstantin Karaghiosoff; Michael Buhl; Alexandra M. Z. Slawin; J. Derek Woollins; Chem.Commun. 50 (2014) 6214–; doi:10.1039/C4CC01073F

data_7113937
_publ_section_title
;
 The activation of Woollins' reagent. Isolation of pyridine stabilised
 PhPSe2
;
_journal_name_full               Chem.Commun.
_journal_page_first              6214
_journal_paper_doi               10.1039/C4CC01073F
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C11 H10 N P Se2, C5 H5 N'
_chemical_formula_sum            'C16 H15 N2 P Se2'
_chemical_formula_weight         424.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-13
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   13.948(3)
_cell_length_b                   10.4836(18)
_cell_length_c                   11.642(2)
_cell_measurement_reflns_used    7626
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      3.00
_cell_volume                     1702.4(6)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 rc13'
_computing_data_collection
'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 rc13'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 7.353
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10588
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.329
_diffrn_reflns_theta_min         2.995
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.433
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             832.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.780
_refine_ls_abs_structure_details
'Parsons and Flack (2004), Acta Cryst. A60, s61'
_refine_ls_abs_structure_Flack   0.135(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2544
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0199P)^2^+2.8988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0803
_reflns_number_gt                2276
_reflns_number_total             2544
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c4cc01073f2.cif
_cod_data_source_block           10
_cod_original_cell_volume        1702.3(5)
_cod_database_code               7113937