Complexation-Distribution Separated Solvent Extraction Process Designed for Rapid and Efficient Recovery of Inert Platinum Group Metals.
Zheng, Zhiwei; Arai, Tsuyoshi; Takao, Koichiro; ACS omega 6 (2021) 21809–21818; doi:10.1021/acsomega.1c03565

data_4519015
_publ_section_title
;
 Complexation-Distribution Separated Solvent Extraction Process Designed
 for Rapid and Efficient Recovery of Inert Platinum Group Metals.
;
_journal_issue                   33
_journal_name_full               'ACS omega'
_journal_page_first              21809
_journal_page_last               21818
_journal_paper_doi               10.1021/acsomega.1c03565
_journal_volume                  6
_journal_year                    2021
_chemical_formula_moiety         'C18 H16 N4 O8 Ru, O'
_chemical_formula_sum            'C20 H16 N2 O9 Ru'
_chemical_formula_weight         529.42
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-21 deposited with the CCDC.	2021-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.707(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9414(4)
_cell_length_b                   15.0754(3)
_cell_length_c                   12.8497(5)
_cell_measurement_reflns_used    5727
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.2740
_cell_measurement_theta_min      2.3140
_cell_volume                     2066.44(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     10.00 110.00   0.50   95.00    --   20.00  54.00-150.00  200
  2  \w     52.00 100.00   0.50   95.00    --   20.00  54.00 150.00   96
  3  \w    -38.00 -13.00   0.50   95.00    --   20.00  54.00   0.00   50
  4  \w    -74.00 -29.00   0.50   95.00    --   20.00  54.00 -90.00   90
  5  \w      6.00  62.00   0.50   95.00    --   20.00  54.00 -90.00  112
  6  \w    -61.00 -29.00   0.50   95.00    --   20.00  54.00-150.00   64
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.942
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11272
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.852
_diffrn_reflns_theta_min         2.230
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.905
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.60a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.121
_refine_diff_density_max         1.015
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.0026(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         5672
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0719P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1148
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4152
_reflns_number_total             5672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c03565_si_002.cif
_cod_data_source_block           200803_weber_ru-tbpda_a_
_cod_original_cell_volume        2066.44(14)
_cod_database_code               4519015
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C14(H14), C16(H16), C5(H5), C15(H15)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              5946
_shelx_hkl_checksum              86686
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;