Supramolecular Gold Stripping from Activated Carbon Using α-Cyclodextrin.
Liu, Wenqi; Jones, Leighton O.; Wu, Huang; Stern, Charlotte L.; Sponenburg, Rebecca A.; Schatz, George C.; Stoddart, J. Fraser; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c11769

data_4135482
_publ_section_title
;
 Supramolecular Gold Stripping from Activated Carbon Using
 \a-Cyclodextrin.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c11769
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C108 H192 K3 O96, 3(C2 Au N2), 15(H2 O)'
_chemical_formula_sum            'C38 H74 Au K N2 O37'
_chemical_formula_weight         1387.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   13.99063(13)
_cell_length_b                   23.4405(2)
_cell_length_c                   51.2967(4)
_cell_measurement_reflns_used    36729
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      77.5960
_cell_measurement_theta_min      3.5900
_cell_volume                     16822.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.967
_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    -21.00  69.00   0.50    1.72    --   47.53 -74.00 -72.00  180
  2  \w    -67.00 -33.00   0.50    6.89    -- -106.00  56.00 -77.00   68
  3  \w   -169.00 -91.00   0.50    6.89    -- -106.00 -96.00  41.00  156
  4  \w   -176.00 -96.00   0.50    6.89    -- -106.00 -56.00 139.00  160
  5  \w     42.00 102.00   0.50    6.89    --  113.25 -74.00 -72.00  120
  6  \w    -15.00  23.00   0.50    1.72    --  -47.53  19.00   0.00   76
  7  \w   -117.00 -83.00   0.50    1.72    --  -47.53-125.00 -30.00   68
  8  \w   -107.00 -82.00   0.50    1.72    --  -47.53-125.00  90.00   50
  9  \w    -13.00  18.00   0.50    1.72    --  -47.53  19.00  60.00   62
 10  \w    -27.00  12.00   0.50    1.72    --   47.53 -19.00 150.00   78
 11  \w    -64.00 -34.00   0.50    6.89    -- -106.00   0.00 120.00   60
 12  \w    -76.00 -42.00   0.50    6.89    -- -106.00   0.00  60.00   68
 13  \w    -71.00 -34.00   0.50    6.89    -- -106.00   0.00 -60.00   74
 14  \w    -75.00 -39.00   0.50    6.89    -- -106.00  61.00  60.00   72
 15  \w    127.00 164.00   0.50    6.89    --  113.25  15.00   0.00   74
 16  \w     44.00  69.00   0.50    6.89    --  113.25 -61.00 120.00   50
 17  \w     43.00  68.00   0.50    6.89    --  113.25 -61.00  60.00   50
 18  \w     45.00  70.00   0.50    6.89    --  113.25 -61.00-120.00   50
 19  \w     83.00 108.00   0.50    6.89    --  113.25-125.00 -60.00   50
 20  \w    142.00 172.00   0.50    6.89    --  113.25  30.00 120.00   60
 21  \w     45.00  70.00   0.50    6.89    --  113.25 -61.00   0.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source 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      -0.0894725000
_diffrn_orient_matrix_UB_12      0.0376825000
_diffrn_orient_matrix_UB_13      -0.0030980000
_diffrn_orient_matrix_UB_21      0.0135490000
_diffrn_orient_matrix_UB_22      0.0225576000
_diffrn_orient_matrix_UB_23      0.0279911000
_diffrn_orient_matrix_UB_31      0.0625770000
_diffrn_orient_matrix_UB_32      0.0489288000
_diffrn_orient_matrix_UB_33      -0.0104707000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            97178
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.292
_diffrn_reflns_theta_min         3.274
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.517
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       needle
_exptl_crystal_F_000             8520
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.015
_refine_diff_density_max         3.413
_refine_diff_density_min         -2.661
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details
;
 Flack x determined using 11919 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2243
_refine_ls_number_reflns         34431
_refine_ls_number_restraints     1832
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+97.8094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1474
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.898
_reflns_number_gt                31036
_reflns_number_total             34431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11769_si_002.cif
_cod_data_source_block           cx2044
_cod_original_cell_volume        16822.6(3)
_cod_database_code               4135482
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C38H60AuKN2O30
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.407
_diffrn_oxdiff_digest_frames
;
019400236024167b1168fad422c2e3c3a601676619f
;
_diffrn_oxdiff_digest_hkl
;
018ed2113fb10266362b51f3155022e454733c
;
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 O3B-H3BA
 0.87 with sigma of 0.01
 O4B-H4BA
 0.87 with sigma of 0.01
 O8A-H8AA
 0.87 with sigma of 0.01
 O9A-H9AA
 0.87 with sigma of 0.01
 O15A-H15B
 0.87 with sigma of 0.01
 O23A-H23B
 0.87 with sigma of 0.01
 O24A-H24C
 0.87 with sigma of 0.01
 O21W-H21C = O21W-H21D
 0.87 with sigma of 0.02
 C2B-H3BA
 1.910172 with sigma of 0.02
 K2-H3BA
 3.639354 with sigma of 0.02
 C3B-H4BA
 1.903837 with sigma of 0.02
 K2-H4BA
 3.443427 with sigma of 0.02
 C8A-H8AA
 1.897074 with sigma of 0.02
 K3-H8AA
 3.492367 with sigma of 0.02
 C9A-H9AA
 1.896562 with sigma of 0.02
 K3-H9AA
 3.565945 with sigma of 0.02
 C18A-H15B
 1.922644 with sigma of 0.02
 K1-H15B
 3.343829 with sigma of 0.02
 C26A-H23B
 1.92164 with sigma of 0.02
 K2-H23B
 3.953299 with sigma of 0.02
 C27A-H24C
 1.898986 with sigma of 0.02
 K2-H24C
 3.499847 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Everything fixed:
 H12G, H12H, H15F, H15G, H18I, H18J
4.b Free rotating group:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O6W(H6WA,H6WB), O7W(H7WA,
 H7WB), O8W(H8WA,H8WB), O11W(H11C,H11D), O13W(H13F,H13G), O14W(H14F,H14G),
 O16W(H16C,H16D), O19W(H19F,H19G), O20W(H20F,H20G)
4.c Rotating group:
 O1W(H1WA,H1WB), O5W(H5WA,H5WB), O9W(H9WA,H9WB), O17W(H17C,H17D), O10W(H10F,
 H10G), O21W(H21C,H21D)
4.d Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10),
 C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20),
  C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28),
 C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C1A(H1A), C1B(H1B),
  C2A(H2A), C2B(H2B), C3A(H3A), C3B(H3B), C4A(H4A), C4B(H4B), C5A(H5A),
 C5B(H5B), C7A(H7A), C7B(H7B), C8A(H8A), C8B(H8B), C9A(H9A), C9B(H9B),
 C10A(H10A), C10B(H10C), C11A(H11A), C11B(H11B), C13A(H13A), C13B(H13C),
 C14A(H14A), C14B(H14C), C15A(H15A), C15B(H15C), C16A(H16A), C16B(H16B),
 C17A(H17A), C17B(H17B), C19A(H19A), C19B(H19C), C20A(H20A), C20B(H20C),
 C21A(H21A), C21B(H21B), C22A(H22A), C22B(H22B), C23A(H23A), C23B(H23C),
 C25A(H25A), C25B(H25C), C26A(H26A), C26B(H26B), C27A(H27A), C27B(H27B),
 C28A(H28A), C28B(H28C), C29A(H29A), C29B(H29C), C31A(H31A), C31B(H31B),
 C32A(H32A), C32B(H32B), C33A(H33A), C33B(H33B), C34A(H34A), C34B(H34B),
 C35A(H35A), C35B(H35B)
4.e Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12E,H12F), C18(H18G,H18H), C24(H24G,H24H), C30(H30G,H30H),
 C36(H36E,H36F), C6A(H6AA,H6AB), C6B(H6BA,H6BB), C12A(H12A,H12B), C12B(H12C,
 H12D), C18A(H18A,H18B), C18B(H18D,H18E), C24A(H24A,H24B), C24B(H24D,H24E),
 C30A(H30A,H30B), C30B(H30D,H30E), C36A(H36A,H36B), C36B(H36C,H36D)
4.f Tetrahedral OH refined with riding coordinates:
 O5A(H5AA)
4.g Idealised tetrahedral OH refined as rotating group:
 O3(H3C), O4(H4C), O5(H5C), O8(H8C), O9(H9C), O10(H10E), O13(H13E), O14(H14E),
 O15(H15E), O18(H18), O19(H19E), O20(H20E), O23(H23E), O24(H24), O25(H25E),
 O28(H28E), O29(H29E), O30(H30), O3A(H3AA), O4A(H4AA), O5B(H5BA), O8B(H8BA),
 O9B(H9BA), O10A(H10B), O10B(H10D), O13A(H13B), O13B(H13D), O14A(H14B),
 O14B(H14D), O15B(H15D), O18A(H18C), O18B(H18F), O19A(H19B), O19B(H19D),
 O20A(H20B), O20B(H20D), O23B(H23D), O24B(H24F), O25A(H25B), O25B(H25D),
 O28A(H28B), O28B(H28D), O29A(H29B), O29B(H29D), O30A(H30C), O30B(H30F)
;
_shelx_res_checksum              19159
_shelx_hkl_checksum              3251
_shelx_fab_checksum              163
_olex2_date_sample_data_collection 2020-09-23
_olex2_date_sample_submission    2020-09-23
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder with Paratone oil'
_olex2_submission_original_sample_id cx2044
_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 1.496
_oxdiff_exptl_absorpt_empirical_full_min 0.716