Thiodiphenol-Based n-Dialkylamino Extractants for Selective Platinum Group Metal Separation from Automotive Catalysts
Yamada, Manabu; Rajiv Gandhi, Muniyappan; Kaneta, Yu; Kimura, Nozomi; Katagiri, Hiroshi; Industrial & Engineering Chemistry Research  (2018) –; doi:10.1021/acs.iecr.7b05009

data_1548808
_publ_section_title
;
 Thiodiphenol-Based n-Dialkylamino Extractants for Selective Platinum
 Group Metal Separation from Automotive Catalysts
;
_journal_name_full
'Industrial &amp; Engineering Chemistry Research'
_journal_paper_doi               10.1021/acs.iecr.7b05009
_journal_year                    2018
_chemical_formula_moiety         'C34 H56 N2 O2 S'
_chemical_formula_sum            'C34 H56 N2 O2 S'
_chemical_formula_weight         556.86
_chemical_name_systematic
'2,2'-bis[diethylaminomethyl] -6,6'-thiobis[4-t-butylphenol]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.514(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9714(3)
_cell_length_b                   18.4729(4)
_cell_length_c                   11.1685(2)
_cell_measurement_reflns_used    24415
_cell_measurement_temperature    93
_cell_measurement_theta_max      30.5470
_cell_measurement_theta_min      1.7640
_cell_volume                     3291.96(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ORTEO-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'Yadokari-XG (Wakira, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            45098
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.132
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         7560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0511P)^2^+1.9019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6581
_reflns_number_total             7560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ie7b05009_si_002.cif
_cod_data_source_block           170808_Yamada_1
_cod_database_code               1548808
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.950
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              72097
_shelx_hkl_checksum              45072