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_4517956
_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         'C36 H36 K0.5 N24 O12.5, Au Br4'
_chemical_formula_sum            'C36 H36 Au Br4 K0.5 N24 O12.5'
_chemical_formula_weight         1541.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                66.228(7)
_cell_angle_beta                 88.468(7)
_cell_angle_gamma                89.781(7)
_cell_formula_units_Z            2
_cell_length_a                   14.3299(14)
_cell_length_b                   14.3772(11)
_cell_length_c                   15.9853(12)
_cell_measurement_reflns_used    3543
_cell_measurement_temperature    100.01(12)
_cell_measurement_theta_max      24.6240
_cell_measurement_theta_min      2.1240
_cell_volume                     3012.8(5)
_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      100.01(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.932
_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     -4.00  64.00   0.50  193.88    --    2.83  77.00 -60.00  136
  2  \w     -1.00  52.00   0.50  193.88    --   -3.30  77.00   0.00  106
  3  \w    -19.00  65.00   0.50  193.88    --    2.83  77.00-120.00  168
;
_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      -0.0120345000
_diffrn_orient_matrix_UB_12      -0.0460076000
_diffrn_orient_matrix_UB_13      0.0375716000
_diffrn_orient_matrix_UB_21      -0.0099433000
_diffrn_orient_matrix_UB_22      -0.0229541000
_diffrn_orient_matrix_UB_23      -0.0306166000
_diffrn_orient_matrix_UB_31      0.0469845000
_diffrn_orient_matrix_UB_32      -0.0162219000
_diffrn_orient_matrix_UB_33      0.0017399000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0996
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15237
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         2.094
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.200
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74826
_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    1.699
_exptl_crystal_description       block
_exptl_crystal_F_000             1497
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.023
_refine_diff_density_max         2.586
_refine_diff_density_min         -1.493
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.410
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         15237
_refine_ls_number_restraints     1758
_refine_ls_restrained_S_all      1.373
_refine_ls_R_factor_all          0.2244
_refine_ls_R_factor_gt           0.1468
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3994
_refine_ls_wR_factor_ref         0.4354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7954
_reflns_number_total             15237
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9229\% 
 around [0.00 0.00 1.00] (reciprocal) or [-0.02 -0.41 0.91] (direct)
;
_cod_data_source_file            am0c09673_si_005.cif
_cod_data_source_block           cx1754_sq
_cod_original_formula_sum        'C36 H36 Au Br4 K0.50 N24 O12.50'
_cod_database_code               4517956
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C36H36N24O12KAuBr4
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.685(3)
 0.315(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 N15-C23 \\sim N16-C24 \\sim N18-C24 \\sim N22-C31 \\sim N21-C31 \\sim N21-C29
\\sim N22-C30 \\sim N22-C33
 \\sim N24-C33 \\sim N24-C34 \\sim N23-C34 \\sim N23-C32 \\sim N19-C29 \\sim
N20-C30 \\sim N20-C28 \\sim N18-
 C27 \\sim N18-C25 \\sim N17-C25 \\sim N17-C23 \\sim N17-C26 \\sim N16-C21
\\sim N14-C21 \\sim N14-C19 ~
 N13-C19 \\sim N13-C20 \\sim N15-C20 \\sim N15-C22 \\sim N16-C22 \\sim N20-C27
\\sim N19-C26 \\sim N21-C32
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(Au2) \\sim Ueq, Uanis(Br5) \\sim Ueq, Uanis(Br6) \\sim Ueq, Uanis(Br7)
\\sim Ueq, Uanis(Br8) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. 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
6. Others
 Fixed Sof: O13(0.5) Au1(0.66667) Br1(0.66667) Br2(0.66667) Br3(0.66667)
 Br4(0.66667) Au2(0.33333) Br5(0.33333) Br6(0.33333) Br7(0.33333) Br8(0.33333)
7.a Free rotating group:
 Au2(Br5,Br6,Br7,Br8)
7.b Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16), C19(H19), C22(H22),
 C25(H25), C28(H28), C31(H31), C34(H34)
7.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C8(H8A,H8B), C9(H9A,H9B), C14(H14A,H14B), C15(H15A,
 H15B), C23(H23A,H23B), C24(H24A,H24B), C29(H29A,H29B), C30(H30A,H30B),
 C35(H35A,H35B), C36(H36A,H36B)
;
_shelx_res_checksum              29912
_shelx_hkl_checksum              62071
_shelx_fab_checksum              22126
_platon_squeeze_void_probe_radius 1.20
_olex2_date_sample_data_collection 2020-01-02
_olex2_date_sample_submission    2019-12-22
_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 cx1754
_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 1.367
_oxdiff_exptl_absorpt_empirical_full_min 0.674
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2