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_4125220
_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
'2(Au0.5 Br2), C192 H328 O168 Rb2, 2(C48 H80 O40)'
_chemical_formula_sum            'C288 H488 Au Br4 O248 Rb2'
_chemical_formula_weight         8606.35
_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             2014-04-18
_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            1
_cell_length_a                   23.7386(6)
_cell_length_b                   23.7386(6)
_cell_length_c                   22.7883(6)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      63.739
_cell_measurement_theta_min      2.688
_cell_volume                     12841.7(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  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.95
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.992
_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  0.0768
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.913
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44769
_diffrn_reflns_point_group_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         64.078
_diffrn_reflns_theta_min         1.939
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.910
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.5890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0783 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.7828.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_description       block
_exptl_crystal_F_000             4493
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.076
_refine_diff_density_max         1.010
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 3056 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.099(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         10602
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1586P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2044
_refine_ls_wR_factor_ref         0.2172
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.903
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                8085
_reflns_number_total             10602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04986_si_013.cif
_cod_data_source_block           n3451
_cod_depositor_comments
'Adding full bibliography for 4125213--4125224.cif.'
_cod_original_cell_volume        12841.7(7)
_cod_database_code               4125220
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.752
_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
2. Restrained distances
 O17-H17
 0.87 with sigma of 0.01
 O8-H8
 0.87 with sigma of 0.01
 C21-H17
 1.892516 with sigma of 0.02
 Rb1-H17
 4.159596 with sigma of 0.02
 C9-H8
 1.869408 with sigma of 0.02
 Rb1-H8
 3.553834 with sigma of 0.02
 Au1A-Br1A \\sim Au1A-Br2A \\sim Au1-Br2 \\sim Au1-Br1
 with sigma of 0.01
3. Rigid bond restraints
 Au1A, Au1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br1, Br2, Br1A, Br2A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Rb1, Rb1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Au1A \\sim Au1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Br1 \\sim Br2 \\sim Br1A \\sim Br2A: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Rb1 \\sim Rb1A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(Au1A) \\sim Ueq, Uanis(Br2A) \\sim Ueq, Uanis(Br1A) \\sim Ueq, Uanis(Au1)
\\sim Ueq, Uanis(Br2) \\sim Ueq, Uanis(Br1) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Others
 1*[Sof(Rb1)]+1*[Sof(Rb1A)]=0.25 with esd of 0.000001
 Fixed Sof: Au1(0.0625) Br1(0.125) Br2(0.125) Au1A(0.0625) Br1A(0.125)
 Br2A(0.125)
6.a Ternary CH refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3), C4(H4), C5(H5A), C6(H6A), C7(H7), C8(H8A),
 C10(H10A), C11(H11A), C13(H13), C14(H14A), C15(H15A), C16(H16), C17(H17A),
 C18(H18), C19(H19), C20(H20A), C22(H22), C23(H23), C25(H25), C26(H26A),
 C27(H27), C28(H28A), C29(H29), C30(H30A), C31(H31), C33(H33), C34(H34),
 C35(H35)
6.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C12(H12A,H12B), C21(H21A,H21B), C24(H24A,H24B), C32(H32A,H32B),
 C36(H36A,H36B)
6.c Tetrahedral OH refined with riding coordinates:
 O5(H5), O1A(H1AA)
6.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O6(H6), O10(H10), O11(H11), O12(H12), O14(H14), O15(H15),
 O20(H20), O21(H21), O23(H23A), O24(H24), O26(H26), O28(H28), O30(H30)
;
_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 = 4282.0 Ang^3^ [33.3%]
Total electron count / cell = 1283.5
;
_shelx_res_checksum              24194
_shelx_hkl_checksum              78782