Cation-Dependent Gold Recovery with α-Cyclodextrin Facilitated by Second-Sphere Coordination.
Liu, Zhichang; Samanta, Avik; Lei, Juying; Sun, Junling; Wang, Yuping; Stoddart, J. Fraser; Journal of the American Chemical Society 138 (2016) 11643–11653; doi:10.1021/jacs.6b04986

data_4125217
_publ_section_title
;
 Cation-Dependent Gold Recovery with \a-Cyclodextrin Facilitated by
 Second-Sphere Coordination.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11643
_journal_page_last               11653
_journal_paper_doi               10.1021/jacs.6b04986
_journal_volume                  138
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety
'0.8(Au Cl4), 0.8(Na), C42 H72 O36, C42 H70 O35, 5(H2 O)'
_chemical_formula_sum            'C84 H152 Au0.8 Cl3.2 Na0.8 O76'
_chemical_formula_weight         2667.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2014-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.952(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.7324(9)
_cell_length_b                   24.3405(13)
_cell_length_c                   19.2739(12)
_cell_measurement_reflns_used    9156
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.157
_cell_measurement_theta_min      4.368
_cell_volume                     6980.5(7)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_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    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            134887
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.279
_diffrn_reflns_theta_min         2.424
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.013
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0802 before and 0.0632 after correction.
The Ratio of minimum to maximum transmission is 0.7657.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       block
_exptl_crystal_F_000             2781
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.958
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 10822 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.002(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1557
_refine_ls_number_reflns         23461
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0819P)^2^+9.8729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1284
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_full    0.913
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                23045
_reflns_number_total             23461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04986_si_010.cif
_cod_data_source_block           n3492
_cod_depositor_comments
'Adding full bibliography for 4125213--4125224.cif.'
_cod_original_formula_sum        'C84 H152 Au0.80 Cl3.20 Na0.80 O76'
_cod_database_code               4125217
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.449
_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) groups, All O(H,H) groups
2. Restrained distances
 O5W-H5WA = O5W-H5WB = O4W-H4WB = O4W-H4WA = O2W-H2WA = O2W-H2WB = O6W-H6WB =
 O6W-H6WA = O3W-H3WA = O3W-H3WB = O1W-H1WB = O1W-H1WA
 0.87 with sigma of 0.001
 H1WB-H1WA = H3WB-H3WA = H6WA-H6WB = H4WB-H4WA = H5WA-H5WB = H2WA-H2WB
 1.421 with sigma of 0.001
3. Others
 Fixed Sof: Au1(0.8) Cl1(0.8) Cl2(0.8) Cl3(0.8) Cl4(0.8) Na1(0.8)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C4(H4A), C5(H5A), C7(H7), C8(H8A), C9(H9A),
 C10(H10A), C11(H11), C13(H13A), C14(H14A), C15(H15A), C16(H16), C17(H17),
 C19(H19A), C20(H20A), C21(H21), C22(H22), C23(H23A), C25(H25A), C26(H26),
 C27(H27), C28(H28A), C29(H29A), C31(H31), C32(H32), C33(H33A), C34(H34A),
 C35(H35A), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C1A(H1A),
 C2A(H2A), C3A(H3AB), C4A(H4AB), C5A(H5AB), C7A(H7A), C8A(H8AB), C9A(H9AB),
 C10A(H10C), C11A(H11A), C13A(H13C), C14A(H14C), C15A(H15C), C16A(H16A),
 C17A(H17A), C19A(H19C), C20A(H20C), C21A(H21A), C22A(H22A), C23A(H23C),
 C25A(H25C), C26A(H26A), C27A(H27A), C28A(H28C), C29A(H29C), C31A(H31A),
 C32A(H32A), C33A(H33C), C34A(H34C), C35A(H35C), C37A(H37A), C38A(H38A),
 C39A(H39A), C40A(H40A), C41A(H41A)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C30(H30A,H30B),
 C36(H36A,H36B), C42(H42A,H42B), C6A(H6AA,H6AB), C12A(H12C,H12D), C18A(H18D,
 H18E), C24A(H24D,H24E), C30A(H30D,H30E), C36A(H36C,H36D), C42A(H42C,H42D)
4.c Tetrahedral OH refined with riding coordinates:
 O3(H3), O4(H4), O8(H8), O9(H9), O13(H13), O14(H14), O18(H18), O19(H19),
 O23(H23), O24(H24), O28(H28), O34(H34), O19A(H19B), O23A(H23B), O24A(H24C),
 O28A(H28B)
4.d Idealised tetrahedral OH refined as rotating group:
 O5(H5), O10(H10), O15(H15), O20(H20), O25(H25), O29(H29), O30(H30), O33(H33),
 O35(H35), O3A(H3AA), O4A(H4AA), O5A(H5AA), O8A(H8AA), O9A(H9AA), O10A(H10B),
 O13A(H13B), O14A(H14B), O15A(H15B), O18A(H18C), O20A(H20B), O25A(H25B),
 O29A(H29B), O30A(H30C), O33A(H33B), O34A(H34B), O35A(H35B)
;
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.

Total solvent accessible volume / cell = 1897.1 Ang^3^ [27.2%]
Total electron count / cell = 514.2
;
_shelx_res_checksum              92177
_shelx_hkl_checksum              98633