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_4135483
_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
'C72 H120 K O60, Ag0.91 C2 N2, 0.09(Ag), 2(C2 H6 O), 8(H2 O)'
_chemical_formula_sum            'C78 H148 Ag K N2 O70'
_chemical_formula_weight         2380.95
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                86.135(4)
_cell_angle_beta                 86.215(3)
_cell_angle_gamma                60.269(4)
_cell_formula_units_Z            1
_cell_length_a                   13.7332(5)
_cell_length_b                   13.7848(5)
_cell_length_c                   15.6408(7)
_cell_measurement_reflns_used    8728
_cell_measurement_temperature    99.98(17)
_cell_measurement_theta_max      29.5540
_cell_measurement_theta_min      2.0640
_cell_volume                     2563.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (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      99.98(17)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.852
_diffrn_measured_fraction_theta_max 0.637
_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    -18.00  33.00   0.50   75.27    --    1.25 -99.00 120.00  102
  2  \w    -13.00  67.00   0.50   75.27    --   -1.72  37.00 -30.00  160
  3  \w     -9.00  16.00   0.50   75.27    --   -1.72  57.00  30.00   50
  4  \w    -28.00   9.00   0.50   75.27    --   -1.72 -57.00 120.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0213123000
_diffrn_orient_matrix_UB_12      0.0350729000
_diffrn_orient_matrix_UB_13      -0.0170380000
_diffrn_orient_matrix_UB_21      -0.0544982000
_diffrn_orient_matrix_UB_22      0.0472082000
_diffrn_orient_matrix_UB_23      0.0035925000
_diffrn_orient_matrix_UB_31      0.0108774000
_diffrn_orient_matrix_UB_32      0.0076162000
_diffrn_orient_matrix_UB_33      0.0420203000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.852
_diffrn_reflns_Laue_measured_fraction_max 0.637
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17511
_diffrn_reflns_point_group_measured_fraction_full 0.573
_diffrn_reflns_point_group_measured_fraction_max 0.415
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.718
_diffrn_reflns_theta_min         2.075
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
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    1.542
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1256
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.179
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Flack x determined using 2391 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.039(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1444
_refine_ls_number_reflns         12082
_refine_ls_number_restraints     1204
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+13.5852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1968
_refine_ls_wR_factor_ref         0.1988
_reflns_Friedel_coverage         0.302
_reflns_Friedel_fraction_full    0.294
_reflns_Friedel_fraction_max     0.192
_reflns_number_gt                11318
_reflns_number_total             12082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11769_si_004.cif
_cod_data_source_block           cx1988
_cod_original_cell_volume        2563.54(19)
_cod_database_code               4135483
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C38H60AgKN2O30
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.961
_reflns_odcompleteness_completeness 86.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O18-H18
 0.87 with sigma of 0.01
 O28A-H28A
 0.87 with sigma of 0.01
 O19-H19
 0.87 with sigma of 0.01
 O29A-H29A
 0.87 with sigma of 0.01
 C20-H18
 1.895976 with sigma of 0.02
 C32A-H28A
 1.890032 with sigma of 0.02
 C21-H19
 1.90253 with sigma of 0.02
 C33A-H29A
 1.890509 with sigma of 0.02
 K1-H18
 3.365932 with sigma of 0.02
 K1-H28A
 3.68048 with sigma of 0.02
 K1-H19
 3.4451 with sigma of 0.02
 K1-H29A
 3.478837 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C31A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
Uanis(Ag3) = Uanis(Ag1) = Uanis(Ag2)
4. 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
5. Others
 1*[Sof(Ag3)]+1*[Sof(Ag1)]+1*[Sof(Ag2)]=1 with esd of 0.000001
6.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,
 H5WB), O6W(H6WA,H6WB), O7W(H7WA,H7WB), O8W(H8WA,H8WB)
6.b Ternary CH refined with riding coordinates:
 C1(H1), C1A(H1A), C2(H2), C2A(H2A), C3(H3B), C3A(H3AA), C4(H4B), C4A(H4AA),
 C5(H5B), C5A(H5AA), C7(H7), C7A(H7A), C8(H8B), C8A(H8AA), C9(H9B), C9A(H9AA),
 C10(H10B), C10A(H10C), C11(H11), C11A(H11A), C13(H13B), C13A(H13C), C14(H14B),
 C14A(H14C), C15(H15B), C15A(H15C), C16(H16), C16A(H16A), C17(H17), C17A(H17A),
 C19(H19B), C19A(H19C), C20(H20B), C20A(H20C), C21(H21), C21A(H21A), C22(H22),
 C22A(H22A), C23(H23B), C23A(H23C), C25(H25B), C25A(H25C), C26(H26), C26A(H26A),
  C27(H27), C27A(H27A), C28(H28B), C28A(H28C), C29(H29B), C29A(H29C), C31(H31),
 C31A(H31A), C32(H32), C32A(H32A), C33(H33), C33A(H33A), C34(H34), C34A(H34A),
 C35(H35), C35A(H35A)
6.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C6A(H6AA,H6AB), C12(H12A,H12B), C12A(H12C,H12D), C18(H18B,H18C),
 C18A(H18D,H18E), C24(H24B,H24C), C24A(H24D,H24E), C30(H30B,H30C), C30A(H30D,
 H30E), C36(H36A,H36B), C36A(H36C,H36D), C1S(H1SA,H1SB), C3S(H3SA,H3SB)
6.d Me refined with riding coordinates:
 C4S(H4SA,H4SB,H4SC)
6.e Tetrahedral OH refined with riding coordinates:
 O5A(H5A), O8A(H8A), O9A(H9A), O15A(H15A), O29(H29)
6.f Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC)
6.g Idealised tetrahedral OH refined as rotating group:
 O3(H3), O3A(H3A), O4(H4), O4A(H4A), O5(H5), O8(H8), O9(H9), O10(H10),
 O10A(H10A), O13(H13), O13A(H13A), O14(H14), O14A(H14A), O15(H15), O18A(H18A),
 O19A(H19A), O20(H20), O20A(H20A), O23(H23), O23A(H23A), O24(H24), O24A(H24A),
 O25(H25), O25A(H25A), O28(H28), O30(H30), O30A(H30A), O1S(H1S), O2S(H2S)
;
_shelx_res_checksum              84140
_shelx_hkl_checksum              78589
_olex2_date_sample_data_collection 2020-08-14
_olex2_date_sample_submission    2020-08-11
_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 cx1988
_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 1.264
_oxdiff_exptl_absorpt_empirical_full_min 0.843