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_7113938
_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_formula_moiety         'C32 H32 N4 P2 Se6'
_chemical_formula_sum            'C32 H32 N4 P2 Se6'
_chemical_formula_weight         1008.34
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                94.891(8)
_cell_angle_beta                 94.728(11)
_cell_angle_gamma                106.893(9)
_cell_formula_units_Z            2
_cell_length_a                   9.422(3)
_cell_length_b                   9.570(3)
_cell_length_c                   21.600(6)
_cell_measurement_reflns_used    5428
_cell_measurement_temperature    125
_cell_measurement_theta_max      25.41
_cell_measurement_theta_min      3.13
_cell_volume                     1845.0(10)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r5'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r5'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      125
_diffrn_detector_area_resol_mean 14.286
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13315
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.065
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             972.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.340
_refine_diff_density_min         -0.860
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6183
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0356P)^2^+7.4159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1118
_reflns_number_gt                4576
_reflns_number_total             6185
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c4cc01073f2.cif
_cod_data_source_block           LADW5-fs
_cod_original_cell_volume        1845.2(9)
_cod_database_code               7113938