(<i>R</i>~P~,<i>R</i>~P~)-Bis[(3-menthyloxy)(phenyl)phosphinoyl] disulfide
Xu, Zhong-Yuan; Zhao, Chang-Qiu; Acta Crystallographica Section E 67 (2011) o2802–; doi:10.1107/S1600536811038165

data_2232111
_publ_section_title
;
 (<i>R</i>~P~,<i>R</i>~P~)-Bis[(3-menthyloxy)(phenyl)phosphinoyl]
 disulfide
;
_journal_coeditor_code           XU5323
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2802
_journal_paper_doi               10.1107/S1600536811038165
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C32 H48 O4 P2 S2'
_chemical_formula_moiety         'C32 H48 O4 P2 S2'
_chemical_formula_sum            'C32 H48 O4 P2 S2'
_chemical_formula_weight         622.76
_chemical_name_common
;
(<i>R</i>~p~,<i>R</i>~p~)-Bis[(3-menthyloxy)(phenyl)phosphinoyl] disulfide
;
_chemical_name_systematic
;
(<i>R</i>~P~,<i>R</i>~P~)-Bis[(2-isopropyl-5-
methylcyclohexyloxy)(phenyl)phosphinoyl] disulfide
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9910(9)
_cell_length_b                   18.9100(17)
_cell_length_c                   8.9747(7)
_cell_measurement_reflns_used    1878
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.07
_cell_measurement_theta_min      3.13
_cell_volume                     1695.6(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0583
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7818
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.9559
_exptl_absorpt_correction_T_min  0.8947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.159
_refine_ls_abs_structure_details 'Flack (1983), 1736 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0799
_reflns_number_gt                2141
_reflns_number_total             2989
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            xu5323.cif
_cod_data_source_block           I
_cod_database_code               2232111
_cod_database_fobs_code          2232111