Crystal structures of bis[2-(diphenylphosphinothioyl)phenyl] ether and bis{2-[diphenyl(selanylidene)phosphanyl]phenyl} ether
Janzen, Daron E.; Kooyman, Arianna M.; Lange, Kayla A.; Acta Crystallographica Section E 70 (2014) 536–540; doi:10.1107/S1600536814023988

data_2240224
_publ_section_title
;
 Crystal structures of bis[2-(diphenylphosphinothioyl)phenyl] ether and
 bis{2-[diphenyl(selanylidene)phosphanyl]phenyl} ether
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              536
_journal_page_last               540
_journal_paper_doi               10.1107/S1600536814023988
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C36 H28 O P2 S2'
_chemical_formula_moiety         'C36 H28 O P2 S2'
_chemical_formula_sum            'C36 H28 O P2 S2'
_chemical_formula_weight         602.64
_chemical_name_common
;
Bis[2-(diphenylphosphinothioyl)phenyl] ether
;
_chemical_name_systematic
;
{2-[2-(Diphenylphosphinothioyl)phenoxy]phenyl}diphenylphosphanethione
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.1161(9)
_cell_length_b                   18.0874(12)
_cell_length_c                   23.1986(16)
_cell_measurement_reflns_used    42656
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.52
_cell_measurement_theta_min      3.00
_cell_volume                     5923.1(7)
_computing_cell_refinement
;
<i>CrystalClear-SM Expert</i> (Rigaku Americas and Rigaku, 2011)
;
_computing_data_collection
;
<i>CrystalClear-SM Expert</i> (Rigaku Americas and Rigaku, 2011)
;
_computing_data_reduction
;
<i>CrystalClear-SM Expert</i> (Rigaku Americas and Rigaku, 2011)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2010)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR2004 (Burla <i>et al</i>., 2005)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 6.849
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            54343
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.098
_exptl_absorpt_coefficient_mu    0.317
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>REQAB</i>; Rigaku, 1998)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.333
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+4.2594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                4671
_reflns_number_total             6050
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su5010sup1.cif
_cod_data_source_block           1
_cod_database_code               2240224
_cod_database_fobs_code          2240224
_shelx_hkl_checksum              52721
_shelx_res_checksum              57819
_shelxl_version_number           2.013