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_4125219
_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_formula_moiety
'(C48 H80 Na O40), 2(C48 H80 O40), (Au Br4), 3(O), 12(H2 O)'
_chemical_formula_sum            'C144 H264 Au Br4 Na O135'
_chemical_formula_weight         4695.10
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           90
_space_group_name_Hall           'P 4ab 2ab'
_space_group_name_H-M_alt        'P 4 21 2'
_symmetry_space_group_name_Hall  'P 4ab 2ab'
_symmetry_space_group_name_H-M   'P 4 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2013-03-28
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.6486(4)
_cell_length_b                   23.6486(4)
_cell_length_c                   22.7925(5)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      63.43
_cell_measurement_theta_min      4.21
_cell_volume                     12746.8(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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXD, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.97
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.995
_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  0.1508
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            79552
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.01
_diffrn_reflns_theta_min         1.87
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.658
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0993 before and 0.0817 after correction.
The Ratio of minimum to maximum transmission is 0.7583.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       plate
_exptl_crystal_F_000             4876
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.671
_refine_diff_density_min         -1.478
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.055(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         10807
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0613
_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^)+(0.1077P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1688
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.928
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                7230
_reflns_number_total             10807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04986_si_012.cif
_cod_data_source_block           n2568
_cod_depositor_comments
'Adding full bibliography for 4125213--4125224.cif.'
_cod_original_cell_volume        12746.9(5)
_cod_database_code               4125219
_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. Shared sites
{Na1, O}
3. Restrained distances
 Au1B-Br2B \\sim Au1B-Br1B \\sim Au1-Br2 \\sim Au1-Br1 \\sim Au1A-Br1A \\sim Au1A-Br2A
 with sigma of 0.02
4. Restrained planarity
 Au1B, Br1B_$1, Br2B, Br1B, Br1B_$2, Br1B_$5, Br2B_$2, Br2B_$5, Br2B_$1
 with sigma of 0.1
5. Rigid bond restraints
 Au1A, Au1, Au1B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br2A, Br1A, Br2, Br1, Br2B, Br1B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
Au1A \\sim Au1 \\sim Au1B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Br2A \\sim Br1A \\sim Br2 \\sim Br1 \\sim Br2B \\sim Br1B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Br2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na1) = Uanis(O)
7. Others
 1*[Sof(Au1B)+Sof(Br1B)+Sof(Br2B)]+1*[Sof(Au1)+Sof(Br1)+Sof(Br2)]+1*[Sof(Au1A)+
 Sof(Br1A)+Sof(Br2A)]=1 with esd of 0.0001
 Sof(Au1A)=Sof(Br1A)=Sof(Br2A)
 Sof(Au1)=Sof(Br1)=Sof(Br2)
 Sof(Au1B)=Sof(Br1B)=Sof(Br2B)
 Fixed Sof: Na1(0.25) O(0.75)
8.a Free rotating group:
 O9(H9C,H9D), O13(H13A,H13B)
8.b Rotating group:
 O12(H12A,H12B)
8.c Ternary CH refined with riding coordinates:
 C1(H1A), C1A(H1AA), C2(H2), C2A(H2A), C3(H3B), C3A(H3AA), C4(H4B), C4A(H4AA),
 C5(H5), C5A(H5AA), C7(H7), C7A(H7A), C8(H8B), C8A(H8AA), C9(H9), C9A(H9A),
 C10(H10B), C10A(H10C), C11(H11B), C11A(H11C), C1B(H1B), C2B(H2B), C3B(H3BB),
 C4B(H4BB), C5B(H5BA), C7B(H7B), C8B(H8BB), C9B(H9BA), C10B(H10E), C11B(H11D)
8.d Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C6A(H6AA,H6AB), C12(H12C,H12D), C12A(H12E,H12F), C6B(H6BA,H6BB),
 C12B(H12G,H12H)
8.e Tetrahedral OH refined with riding coordinates:
 O5(H1), O10A(H10A), O10B(H10D)
8.f Idealised tetrahedral OH refined as rotating group:
 O3(H3), O3A(H3A), O4(H4), O4A(H4A), O5A(H5A), O8(H8), O8A(H8A), O10(H10),
 O11(H11), O11A(H11A), O3B(H3BA), O4B(H4BA), O5B(H5B), O8B(H8BA), O9B(H9B)
;
_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 = 3708.9 Ang^3^ [29.1%]
Total electron count / cell = 895.5
;
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.706
_shelx_hkl_checksum              81608
_shelx_res_checksum              48912
_shelxl_version_number           2012-9