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_4125221
_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
'0.78(Au Br4), 0.78(Rb), 2(C42 H70 O35), 12(H2 O)'
_chemical_formula_sum            'C84 H164 Au0.78 Br3.1 O82 Rb0.78'
_chemical_formula_weight         2953.06
_chemical_name_systematic
;
 ?
;
_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             2014-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.399(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.8404(4)
_cell_length_b                   24.5602(6)
_cell_length_c                   19.0823(6)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.537
_cell_measurement_theta_min      2.440
_cell_volume                     7044.3(3)
_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      99.95
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            76689
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.778
_diffrn_reflns_theta_min         2.440
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.763
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.5942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0833 before and 0.0720 after correction.
The Ratio of minimum to maximum transmission is 0.7891.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       rod
_exptl_crystal_F_000             3045
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.042
_refine_diff_density_max         2.490
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details
;
 Flack x determined using 9672 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.011(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1623
_refine_ls_number_reflns         24929
_refine_ls_number_restraints     1344
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0690
_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^)+(0.1295P)^2^+6.8543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.1938
_reflns_Friedel_coverage         0.926
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                22261
_reflns_number_total             24929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04986_si_009.cif
_cod_data_source_block           n3450
_cod_depositor_comments
'Adding full bibliography for 4125213--4125224.cif.'
_cod_original_formula_sum        'C84 H164 Au0.78 Br3.10 O82 Rb0.78'
_cod_database_code               4125221
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.858
_shelx_estimated_absorpt_t_min   0.467
_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
 O1W-H1WA = O1W-H1WB = O2W-H2WB = O2W-H2WA = O3W-H3WB = O3W-H3WA = O4W-H4WB =
 O4W-H4WA = O5W-H5WB = O5W-H5WA = O6W-H6WA = O6W-H6WB = O7W-H7WB = O7W-H7WA =
 O8W-H8WA = O8W-H8WB = O9W-H9WB = O9W-H9WA = O10W-H10E = O10W-H10D = O11W-H11B =
  O11W-H11C = O12W-H12E = O12W-H12F
 0.87 with sigma of 0.001
 H1WA-H1WB = H2WA-H2WB = H3WB-H3WA = H4WB-H4WA = H5WA-H5WB = H6WA-H6WB = H7WA-
 H7WB = H8WA-H8WB = H9WB-H9WA = H10E-H10D = H11B-H11C = H12E-H12F
 1.421 with sigma of 0.001
 C30A-C29A \\sim C30B-C29A
 with sigma of 0.02
 O25A-C30A \\sim O25B-C30B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C30A) = Uanis(C30B) = Uanis(O25A) = Uanis(O25B)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O25B)=Sof(H25B)=Sof(H29C)=Sof(C30B)=Sof(H30D)=Sof(H30E)=1-FVAR(1)
 Sof(O25A)=Sof(H25A)=Sof(H29B)=Sof(C30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Sof(Au1)=Sof(Br1)=Sof(Br2)=Sof(Br3)=Sof(Br4)=Sof(Rb1)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3B), C4(H4B), C5(H5B), C7(H7), C8(H8B), C9(H9B),
 C10(H10C), C11(H11), C13(H13C), C14(H14C), C15(H15C), C16(H16), C17(H17),
 C19(H19C), C20(H20C), C21(H21), C22(H22), C23(H23C), C25(H25D), C26(H26),
 C27(H27), C28(H28C), C29(H29D), C31(H31), C32(H32), C33(H33C), C34(H34C),
 C35(H35C), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C1A(H1A),
 C2A(H2A), C3A(H3AA), C4A(H4AA), C5A(H5AA), C7A(H7A), C8A(H8AA), C9A(H9AA),
 C10A(H10B), C11A(H11A), C13A(H13B), C14A(H14B), C15A(H15B), C16A(H16A),
 C17A(H17A), C19A(H19B), C20A(H20B), C21A(H21A), C22A(H22A), C23A(H23B),
 C25A(H25C), C26A(H26A), C27A(H27A), C28A(H28B), C29A(H29B), C29A(H29C),
 C31A(H31A), C32A(H32A), C33A(H33B), C34A(H34B), C35A(H35B), C37A(H37A),
 C38A(H38A), C39A(H39A), C40A(H40A), C41A(H41A)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12C,H12D), C18(H18D,H18E), C24(H24D,H24E), C30(H30F,H30G),
 C36(H36C,H36D), C42(H42C,H42D), C6A(H6AA,H6AB), C12A(H12A,H12B), C18A(H18B,
 H18C), C24A(H24B,H24C), C30A(H30B,H30C), C30B(H30D,H30E), C36A(H36A,H36B),
 C42A(H42A,H42B)
6.c Tetrahedral OH refined with riding coordinates:
 O3(H3), O4(H4), O5(H5), O8(H8), O9(H9), O10(H10), O13(H13), O14(H14),
 O15(H15), O18(H18), O19(H19), O20(H20), O23(H23), O24(H24), O25(H25), O28(H28),
  O29(H29), O30(H30), O33(H33), O34(H34), O35(H35), O3A(H3A), O4A(H4A),
 O5A(H5A), O8A(H8A), O9A(H9A), O10A(H10A), O13A(H13A), O14A(H14A), O15A(H15A),
 O18A(H18A), O19A(H19A), O20A(H20A), O23A(H23A), O24A(H24A), O25A(H25A),
 O25B(H25B), O28A(H28A), O29A(H29A), O30A(H30A), O33A(H33A), O34A(H34A),
 O35A(H35A)
;
_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 = 1493.0 Ang^3^ [21.2%]
Total electron count / cell = 308.4
;
_shelx_res_checksum              43207
_shelx_hkl_checksum              22855