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_4517957
_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 Br1.72 Cl2.28), C36 H36 N24 O12, 7(H4 O2)'
_chemical_formula_sum            'C36 H64 Au2 Br3.43 Cl4.57 N24 O26'
_chemical_formula_weight         2079.14
_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                 93.6000(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.2232(3)
_cell_length_b                   16.5456(3)
_cell_length_c                   12.6850(2)
_cell_measurement_reflns_used    14233
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      37.7880
_cell_measurement_theta_min      2.3050
_cell_volume                     3398.22(10)
_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      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 0.999
_diffrn_measured_fraction_theta_max 0.931
_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    -48.00 -22.00   0.50    2.73    --   24.71 -39.00  19.00   52
  2  \w    -38.00  45.00   0.50    2.73    --  -25.33  39.00 173.00  166
  3  \w     46.00  96.00   0.50    2.73    --   24.71 178.00   0.00  100
  4  \w     46.00  95.00   0.50    2.73    --   24.71 178.00  30.00   98
  5  \w     51.00  77.00   0.50    2.73    --   24.71 178.00 120.00   52
  6  \w    -98.00 -12.00   0.50    2.73    --  -25.33 -39.00  19.00  172
  7  \w     48.00  95.00   0.50    2.73    --   24.71-178.00 -30.00   94
;
_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      -0.0034369000
_diffrn_orient_matrix_UB_12      0.0025999000
_diffrn_orient_matrix_UB_13      -0.0558788000
_diffrn_orient_matrix_UB_21      -0.0380427000
_diffrn_orient_matrix_UB_22      -0.0212491000
_diffrn_orient_matrix_UB_23      -0.0009326000
_diffrn_orient_matrix_UB_31      -0.0215378000
_diffrn_orient_matrix_UB_32      0.0371250000
_diffrn_orient_matrix_UB_33      0.0034028000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26523
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.053
_diffrn_reflns_theta_min         2.331
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.601
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39696
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_description       block
_exptl_crystal_F_000             2023
_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         3.130
_refine_diff_density_min         -4.001
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         8879
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+4.5554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7590
_reflns_number_total             8879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c09673_si_006.cif
_cod_data_source_block           cx1761
_cod_original_cell_volume        3398.25(10)
_cod_database_code               4517957
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C36H36N24O12HAuBr4
_shelx_estimated_absorpt_t_max   0.368
_shelx_estimated_absorpt_t_min   0.215
_diffrn_oxdiff_digest_frames
;
01e398bd2e48f2824f4c72ae5d3b88c14000027cbbb
;
_diffrn_oxdiff_digest_hkl
;
01c078d0a47959393260f65f00ac2905b876aa
;
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_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. Restrained distances
 O5-H5A = O5-H5B
 0.85 with sigma of 0.02
3. Others
 Sof(Br1)=0.5*(1-FVAR(2))
 Sof(Cl1)=0.5*FVAR(2)
 Sof(Br2)=1-FVAR(2)
 Sof(Cl2)=FVAR(2)
 Sof(Br3)=0.5*(1-FVAR(4))
 Sof(Cl3)=0.5*FVAR(4)
 Fixed Sof: H5A(0.5)
4.a Free rotating group:
 O6(H6C,H6D), O7(H7A,H7B), 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)
;
_shelx_res_checksum              80864
_shelx_hkl_checksum              49360
_shelx_fab_checksum              42610
_olex2_date_sample_data_collection 2020-01-01
_olex2_date_sample_submission    2019-12-30
_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 cx1761
_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 1.866
_oxdiff_exptl_absorpt_empirical_full_min 0.746