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_4517954
_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         'Au Cl4, 0.5(C36 H36 N24 O12), 3.5(H4 O2)'
_chemical_formula_sum            'C18 H32 Au Cl4 N12 O13'
_chemical_formula_weight         963.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_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                 93.083(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1427(4)
_cell_length_b                   16.3995(4)
_cell_length_c                   12.6960(3)
_cell_measurement_reflns_used    14098
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      33.9460
_cell_measurement_theta_min      2.3430
_cell_volume                     3356.18(14)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101(2)
_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 0.862
_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     -2.00  86.00   0.50    1.39    --   13.12  57.00 -60.00  176
  2  \w     44.00  70.00   0.50    1.39    --   13.12-178.00  60.00   52
  3  \w     46.00  73.00   0.50    1.39    --   13.12-178.00   0.00   54
  4  \w     40.00  65.00   0.50    1.39    --   13.12-178.00-180.00   50
  5  \w    -88.00   0.00   0.50    1.39    --  -13.59 -24.00  33.00  176
  6  \w    -18.00  61.00   0.50    1.39    --  -13.59  24.00-161.00  158
;
_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      -0.0372916000
_diffrn_orient_matrix_UB_12      0.0054945000
_diffrn_orient_matrix_UB_13      0.0262397000
_diffrn_orient_matrix_UB_21      0.0202723000
_diffrn_orient_matrix_UB_22      -0.0133240000
_diffrn_orient_matrix_UB_23      0.0478996000
_diffrn_orient_matrix_UB_31      0.0116635000
_diffrn_orient_matrix_UB_32      0.0407672000
_diffrn_orient_matrix_UB_33      0.0121261000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20967
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.762
_diffrn_reflns_theta_min         2.345
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.779
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.309
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_description       block
_exptl_crystal_F_000             1900
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.189
_refine_diff_density_max         1.127
_refine_diff_density_min         -1.589
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5964
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0343P)^2^+1.1741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5456
_reflns_number_total             5964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c09673_si_002.cif
_cod_data_source_block           cx1758_1
_cod_database_code               4517954
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C36H36N24O12HAuCl4
_shelx_estimated_absorpt_t_max   0.465
_shelx_estimated_absorpt_t_min   0.297
_diffrn_oxdiff_digest_frames
;
01b25794aeaf5707eb01131dad073ec9cb006662cbb
;
_diffrn_oxdiff_digest_hkl
;
01dea8ab6674c649b5b5d278133e0a75f1b274
;
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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 H(H,H) groups, All O(H,H) groups
2. Restrained distances
 O6-H6D
 0.85 with sigma of 0.02
 O6-H6C
 0.85 with sigma of 0.02
 O5-H5A = O5-H5B
 0.85 with sigma of 0.02
 O7-H7A
 0.85 with sigma of 0.02
 O7-H7B
 0.85 with sigma of 0.02
3. Others
 Fixed Sof: H5A(0.5)
4.a Free rotating group:
 O8(H8A,H8B)
4.b Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C8(H8)
4.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C6(H6A,H6B), C9(H9A,H9B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4444
_shelx_hkl_checksum              37072
_shelx_fab_checksum              68110
_olex2_date_sample_data_collection 2019-12-27
_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 cx1758_1
_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 1.369
_oxdiff_exptl_absorpt_empirical_full_min 0.765