Electrochemical removal of toxic metals from reaction media following catalysis.
Husbands, David R.; Booth, Elisha M.; Donaldson, Niall W. B.; Kapur, Nikil; Willans, Rebecca M.; Willans, Charlotte E.; Chemical communications (Cambridge, England) 60 (2024) 8876–8879; doi:10.1039/d4cc02000f

data_7133433
_publ_section_title
;
 Electrochemical removal of toxic metals from reaction media following
 catalysis.
;
_journal_issue                   67
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8876
_journal_page_last               8879
_journal_paper_doi               10.1039/d4cc02000f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C18 H19 N3 O4'
_chemical_formula_sum            'C18 H19 N3 O4'
_chemical_formula_weight         341.36
_chemical_name_systematic        DRH-04-35
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-26 deposited with the CCDC.	2024-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.665(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6692(4)
_cell_length_b                   12.8126(5)
_cell_length_c                   11.3946(5)
_cell_measurement_reflns_used    2076
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      76.2020
_cell_measurement_theta_min      3.8190
_cell_volume                     1688.42(12)
_computing_cell_refinement       'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.95a 64-bit (release 03-11-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -20.00  24.00   0.50    1.00    --  -48.64  54.00  12.00   88
  2  \w    -63.00 -24.00   0.50    1.00    --  -48.64  54.00  12.00   78
  3  \w   -120.00 -34.00   0.50    1.00    --  -48.64 -54.00-131.00  172
  4  \w     94.00 130.00   0.50    3.00    --  107.75  54.00  12.00   72
  5  \w    134.00 178.00   0.50    3.00    --  107.75  54.00  12.00   88
  6  \w     36.00 103.00   0.50    3.00    --  107.75 -54.00-131.00  134
  7  \w   -117.00 -78.00   0.50    1.00    --  -48.64-125.00-180.00   78
  8  \w   -101.00 -73.00   0.50    1.00    --  -48.64-125.00  30.00   56
  9  \w     36.00  92.00   0.50    1.00    --   48.64-125.00  90.00  112
 10  \w     53.00  78.00   0.50    1.00    --   48.64  54.00  12.00   50
 11  \w     -4.00  21.00   0.50    1.00    --   48.64 -54.00-131.00   50
 12  \w     37.00  84.00   0.50    3.00    --  107.75 -99.00-150.00   94
 13  \w     37.00 106.00   0.50    3.00    --  107.75 -99.00  60.00  138
 14  \w     41.00  74.00   0.50    3.00    --  107.75 -19.00 -90.00   66
 15  \w    107.00 169.00   0.50    3.00    --  107.75  19.00 150.00  124
 16  \w     94.00 119.00   0.50    3.00    --  107.75 -19.00 -90.00   50
 17  \w     62.00  88.00   0.50    3.00    --  107.75 -99.00 120.00   52
 18  \w     95.00 167.00   0.50    3.00    --  107.75  37.00 -90.00  144
 19  \w     72.00 102.00   0.50    3.00    --  107.75 -99.00 -90.00   60
 20  \w     49.00  83.00   0.50    3.00    --  107.75 -99.00-180.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1126684000
_diffrn_orient_matrix_UB_12      0.0395235000
_diffrn_orient_matrix_UB_13      0.0416616000
_diffrn_orient_matrix_UB_21      -0.0710092000
_diffrn_orient_matrix_UB_22      -0.0672357000
_diffrn_orient_matrix_UB_23      -0.0951716000
_diffrn_orient_matrix_UB_31      0.0039674000
_diffrn_orient_matrix_UB_32      -0.0915074000
_diffrn_orient_matrix_UB_33      0.0883641000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9320
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.822
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.94a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       plate
_exptl_crystal_F_000             720
_exptl_crystal_recrystallization_method 'Solvent Methanol'
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.258
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0574P)^2^+0.5502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2646
_reflns_number_total             3013
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02000f2.cif
_cod_data_source_block           cew24001
_cod_depositor_comments          'Adding full bibliography for 7133433.cif.'
_cod_original_cell_volume        1688.41(11)
_cod_database_code               7133433
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C18 H19 N3 O4'
_chemical_oxdiff_usercomment     'David Husbands DRH 04 35'
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.800
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              51950
_shelx_hkl_checksum              56708
_olex2_date_sample_data_collection 2024-01-12
_olex2_date_sample_submission    2024-01-11
_olex2_exptl_crystal_mounting_method '200 micrometer micromount'
_olex2_submission_original_sample_id cew24001
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.994
_oxdiff_exptl_absorpt_empirical_full_min 0.505