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_4125218
_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         'Au Br4, Na1, 2(C36 H60 O30), H2 O'
_chemical_formula_sum            'C72 H122 Au Br4 Na O61'
_chemical_formula_weight         2503.29
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2014-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.7683(16)
_cell_length_b                   14.1475(9)
_cell_length_c                   16.2856(11)
_cell_measurement_reflns_used    9600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.136
_cell_measurement_theta_min      3.123
_cell_volume                     5476.2(6)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0456
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            71662
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.237
_diffrn_reflns_theta_min         2.713
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    5.125
_exptl_absorpt_correction_T_max  0.6807
_exptl_absorpt_correction_T_min  0.4989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1241 before and 0.0736 after correction.
The Ratio of minimum to maximum transmission is 0.7329.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.134
_refine_diff_density_max         1.581
_refine_diff_density_min         -1.298
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details
;
 Flack x determined using 4278 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.015(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         9940
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0915P)^2^+17.5643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1542
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                9774
_reflns_number_total             9940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04986_si_002.cif
_cod_data_source_block           n3423
_cod_depositor_comments
'Adding full bibliography for 4125213--4125224.cif.'
_cod_database_code               4125218
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.547
_shelx_estimated_absorpt_t_min   0.343
_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
 H1SB-H1SA
 1.421 with sigma of 0.0001
 C36A-C35 \\sim C36-C35
 with sigma of 0.02
 O30A-C36A \\sim O30-C36
 with sigma of 0.02
 O1S-H1SA \\sim O1S-H1SB
 with sigma of 0.02
 C34-C33A \\sim C34-C33 \\sim C33-C32 \\sim C33A-C32A \\sim C32A-C31 \\sim
C32-C31
 with sigma of 0.02
 O27A-C33A \\sim O27-C33 \\sim O26A-C32A \\sim O26-C32
 with sigma of 0.02
 C12A-C11 \\sim C12-C11
 with sigma of 0.02
 O14A-C12A \\sim O14-C12
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Na1) = Uanis(Na2)
Uanis(C36A) = Uanis(C36) = Uanis(O30A) = Uanis(O30)
Uanis(C33A) = Uanis(C33) = Uanis(C32A) = Uanis(C32) = Uanis(O27A) = Uanis(O27)
= Uanis(O26A) = Uanis(O26)
Uanis(C12) = Uanis(C12A) = Uanis(O14A) = Uanis(O14)
4. Others
 1*[Sof(Na1)]+1*[Sof(Na2)]=0.5 with esd of 0.0001
 Sof(O30A)=Sof(H30A)=Sof(H35A)=Sof(C36A)=Sof(H36C)=Sof(H36D)=1-FVAR(3)
 Sof(O30)=Sof(H30)=Sof(H35)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(3)
 Sof(H31A)=Sof(H34A)=Sof(C33A)=Sof(H33A)=Sof(O27A)=Sof(H27B)=Sof(C32A)=
 Sof(H32A)=Sof(O26A)=Sof(H26B)=1-FVAR(4)
 Sof(O26)=Sof(H26)=Sof(O27)=Sof(H27)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=
 Sof(H33)=Sof(H34)=FVAR(4)
 Sof(H11B)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(O14A)=Sof(H14B)=1-FVAR(5)
 Sof(O14)=Sof(H14)=Sof(H11A)=Sof(C12)=Sof(H12A)=Sof(H12B)=FVAR(5)
 Fixed Sof: Br1(0.5) Br2(0.5) Br3(0.5) Br4(0.5) O1S(0.5) H1SA(0.5) H1SB(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C7(H7A), C8(H8A), C9(H9A), C10(H10A),
 C11(H11A), C11(H11B), C13(H13A), C14(H14A), C15(H15A), C16(H16), C17(H17),
 C19(H19), C20(H20), C21(H21), C22(H22A), C23(H23A), C25(H25A), C26(H26A),
 C27(H27A), C28(H28A), C29(H29A), C31(H31), C31(H31A), C32(H32), C33(H33),
 C34(H34), C34(H34A), C35(H35), C35(H35A), C33A(H33A), C32A(H32A)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C30(H30B,H30C),
 C36(H36A,H36B), C36A(H36C,H36D), C12A(H12C,H12D)
5.c Tetrahedral OH refined with riding coordinates:
 O7(H7)
5.d Tetrahedral OH refined as rotating group:
 O8(H8), O12(H12), O14(H14), O30(H30), O30A(H30A), O14A(H14B)
5.e Idealised tetrahedral OH refined as rotating group:
 O9(H9), O10(H10), O11(H11), O13(H13), O15(H15), O22(H22), O23(H23), O24(H24),
 O25(H25), O26(H26), O27(H27), O28(H28), O29(H29), O27A(H27B), O26A(H26B)
;
_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 = 984.5 Ang^3^ [18.0%]
Total electron count / cell = 237.5
;
_shelx_res_checksum              14337
_shelx_hkl_checksum              58735