High-Efficiency Gold Recovery Using Cucurbit[6]uril.
Wu, Huang; Jones, Leighton O.; Wang, Yu; Shen, Dengke; Liu, Zhichang; Zhang, Long; Cai, Kang; Jiao, Yang; Stern, Charlotte L.; Schatz, George C.; Stoddart, J. Fraser; ACS applied materials & interfaces  (2020) –; doi:10.1021/acsami.0c09673

data_4517955
_publ_section_title
;
 High-Efficiency Gold Recovery Using Cucurbit[6]uril.
;
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_paper_doi               10.1021/acsami.0c09673
_journal_year                    2020
_chemical_formula_moiety         '2(Au Br4), 2(C36 H36 N24 O12), 0.25(H8 O4)'
_chemical_formula_sum            'C72 H74 Au2 Br8 N48 O25'
_chemical_formula_weight         3045.00
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-02
_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            4
_cell_length_a                   14.4358(2)
_cell_length_b                   14.4358(2)
_cell_length_c                   58.4604(11)
_cell_measurement_reflns_used    18475
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.1820
_cell_measurement_theta_min      2.0900
_cell_volume                     12182.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(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 0.892
_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  41.28   0.38   85.09    --    2.99  77.00  60.00  156
  2  \w     19.00  60.04   0.38   85.09    --   -3.53  77.00 -30.00  108
  3  \w    -26.00  15.04   0.38   85.09    --   -3.53  77.00 -30.00  108
  4  \w    -26.00  10.10   0.38   85.09    --   -3.53  77.00 -90.00   95
  5  \w    -25.00  24.02   0.38   85.09    --   -3.53  77.00 120.00  129
;
_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      -0.0066990000
_diffrn_orient_matrix_UB_12      -0.0423570000
_diffrn_orient_matrix_UB_13      0.0059204000
_diffrn_orient_matrix_UB_21      0.0076469500
_diffrn_orient_matrix_UB_22      -0.0247737500
_diffrn_orient_matrix_UB_23      -0.0103040500
_diffrn_orient_matrix_UB_31      0.0480886000
_diffrn_orient_matrix_UB_32      -0.0019711000
_diffrn_orient_matrix_UB_33      0.0024583000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       80
_diffrn_reflns_limit_l_min       -79
_diffrn_reflns_number            47505
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.313
_diffrn_reflns_theta_min         2.113
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.110
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_description       block
_exptl_crystal_F_000             5920
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.877
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.189
_refine_ls_abs_structure_details
;
 Flack x determined using 2253 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.177(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         7636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0901
_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^)+(0.1900P)^2^+44.4967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2526
_refine_ls_wR_factor_ref         0.2663
_reflns_Friedel_coverage         0.728
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.765
_reflns_number_gt                6113
_reflns_number_total             7636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c09673_si_004.cif
_cod_data_source_block           cx1759_1b
_cod_original_cell_volume        12182.7(4)
_cod_database_code               4517955
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C36H36N24O12HAuBr4
_shelx_estimated_absorpt_t_max   0.685
_shelx_estimated_absorpt_t_min   0.307
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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,H) groups
2. Others
 Fixed Sof: Au1(0.33333) Br1(0.33333) Br2(0.33333) Br3(0.33333) Br4(0.33333)
 Au2(0.16667) Br5(0.33333) Br6(0.33333) H7C(0.25) H7D(0.25)
3.a Everything fixed:
 H7C, H7D
3.b Ternary CH refined with riding coordinates:
 C5(H5), C6(H6), C9(H9), C10(H10), C14(H14), C16(H16)
3.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C7(H7A,H7B), C11(H11A,H11B), C13(H13A,H13B),
 C18(H18A,H18B)
;
_shelx_res_checksum              51008
_shelx_hkl_checksum              8453
_shelx_fab_checksum              98226
_olex2_date_sample_data_collection 2020-01-29
_olex2_date_sample_submission    2019-12-26
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder'
_olex2_submission_original_sample_id cx1759
_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 2.008
_oxdiff_exptl_absorpt_empirical_full_min 0.688