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_4125223
_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
'0.89(Au Br4), 1.1(Cs), 0.22(Br), 2(C36 H60 O30), 9.5(H2 O)'
_chemical_formula_sum            'C72 H139 Au0.89 Br3.76 Cs1.1 O69.5'
_chemical_formula_weight         2738.19
_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     direct
_audit_creation_date             2014-05-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.021(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.3326(7)
_cell_length_b                   14.2587(6)
_cell_length_c                   23.6886(9)
_cell_measurement_reflns_used    9684
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.142
_cell_measurement_theta_min      2.705
_cell_volume                     5516.6(4)
_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    'XT (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 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            96588
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.169
_diffrn_reflns_theta_min         1.865
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    7.558
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0882 before and 0.0646 after correction.
The Ratio of minimum to maximum transmission is 0.6634.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             2778
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.364
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.160
_refine_ls_abs_structure_details
;
 Flack x determined using 8723 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.004(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1485
_refine_ls_number_reflns         18605
_refine_ls_number_restraints     1185
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0979P)^2^+34.4085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1582
_refine_ls_wR_factor_ref         0.1583
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    0.941
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                18575
_reflns_number_total             18605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04986_si_004.cif
_cod_data_source_block           n3511a
_cod_depositor_comments
'Adding full bibliography for 4125213--4125224.cif.'
_cod_original_formula_sum        'C72 H139.0 Au0.89 Br3.76 Cs1.10 O69.50'
_cod_database_code               4125223
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.490
_shelx_estimated_absorpt_t_min   0.158
_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
 O8-H8
 0.87 with sigma of 0.01
 O13-H13
 0.87 with sigma of 0.01
 H8WB-H8WA = H5WA-H5WB = H13D-H13E = H1WA-H1WB = H12E-H12F = H9WA-H9WB = H4WB-
 H4WA = H11C-H11B = H6WB-H6WA = H2WA-H2WB = H7WB-H7WA = H3WB-H3WA = H10D-H10E
 1.421 with sigma of 0.0005
 O12W-H12E = O12W-H12F = O8W-H8WB = O8W-H8WA = O5W-H5WA = O5W-H5WB = O13W-H13D
 = O13W-H13E = O9W-H9WA = O9W-H9WB = O4W-H4WB = O4W-H4WA = O11W-H11C = O11W-
 H11B = O1W-H1WA = O1W-H1WB = O6W-H6WB = O6W-H6WA = O2W-H2WB = O2W-H2WA = O7W-
 H7WB = O7W-H7WA = O10W-H10D = O10W-H10E = O3W-H3WA = O3W-H3WB
 0.87 with sigma of 0.0005
3. Uiso/Uaniso restraints and constraints
Uanis(Au1) = Uanis(Br2) = Uanis(Br4) = Uanis(Br1) = Uanis(Br3) = Uanis(Br2A) =
Uanis(Br4A) = Uanis(Br1A) = Uanis(Br3A)
Uanis(Cs2) = Uanis(Cs1)
Uanis(Cs3) = Uanis(Cs4) = Uanis(Br5)
Uanis(O7W) = Uanis(O8W)
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
 1*[Sof(Br1)+Sof(Br2)+Sof(Br3)+Sof(Br4)]+1*[Sof(Br1A)+Sof(Br2A)+Sof(Br3A)+
 Sof(Br4A)]-1*[Sof(Au1)]=0 with esd of 0.0001
 1*[Sof(Cs3)+Sof(O8W)+Sof(H8WA)+Sof(H8WB)]+1*[Sof(Cs4)]-1*[Sof(Br5)]=0 with
 esd of 0.00001
 1*[Sof(Cs2)+Sof(O12W)+Sof(H12E)+Sof(H12F)]+1*[Sof(Cs1)+Sof(O7W)+Sof(H7WA)+
 Sof(H7WB)]-1*[Sof(Au1)]=0 with esd of 0.0001
 Sof(Br1)=Sof(Br2)=Sof(Br3)=Sof(Br4)=FVAR(1)
 Sof(Br1A)=Sof(Br2A)=Sof(Br3A)=Sof(Br4A)=FVAR(2)
 Sof(O12W)=Sof(H12E)=Sof(H12F)=1-FVAR(4)
 Sof(Cs2)=FVAR(4)
 Sof(O7W)=Sof(H7WA)=Sof(H7WB)=1-FVAR(5)
 Sof(Cs1)=FVAR(5)
 Sof(O8W)=Sof(H8WA)=Sof(H8WB)=1-FVAR(6)
 Sof(Cs3)=FVAR(6)
 Fixed Sof: O5W(0.75) H5WA(0.75) H5WB(0.75) O6W(0.75) H6WA(0.75) H6WB(0.75)
 O9W(0.5) H9WA(0.5) H9WB(0.5) O10W(0.5) H10D(0.5) H10E(0.5) O11W(0.5) H11B(0.5)
 H11C(0.5) O13W(0.5) H13D(0.5) H13E(0.5)
6.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(H33), C34(H34),
 C35(H35), 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(H33A), C34A(H34A), C35A(H35A)
6.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), C6A(H6AA,H6AB), C12A(H12C,H12D), C18A(H18D,H18E), C24A(H24D,
 H24E), C30A(H30D,H30E), C36A(H36C,H36D)
6.c Tetrahedral OH refined with riding coordinates:
 O23(H23), O3A(H3AA)
6.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4), O5(H5), O9(H9), O10(H10), O14(H14), O15(H15), O18(H18),
 O19(H19), O20(H20), O24(H24), O25(H25), O28(H28), O29(H29), O30(H30),
 O4A(H4AA), O5A(H5AA), O8A(H8AA), O9A(H9AA), O10A(H10B), O13A(H13B), O14A(H14B),
  O15A(H15B), O18A(H18C), O19A(H19B), O20A(H20B), O23A(H23B), O24A(H24C),
 O25A(H25B), O28A(H28B), O29A(H29B), O30A(H30C)
;
_shelx_res_checksum              28898
_shelx_hkl_checksum              29999