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_7113939
_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         'C36 H40 N4 P2 Se6'
_chemical_formula_sum            'C36 H40 N4 P2 Se6'
_chemical_formula_weight         1064.45
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 99.693(11)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.406(5)
_cell_length_b                   15.548(7)
_cell_length_c                   26.232(10)
_cell_measurement_reflns_used    6287
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.38
_cell_volume                     4184(3)
_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    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0469
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13217
_diffrn_reflns_theta_full        25.29
_diffrn_reflns_theta_max         25.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.355
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2072.00
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.540
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3777
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0377P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0979
_reflns_number_gt                2814
_reflns_number_total             3777
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c4cc01073f2.cif
_cod_data_source_block           LADW20
_cod_database_code               7113939