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_4125222
_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
'C192 H320 Na O160, 2(C48 H80 O40), 2(Au0.5 Cl2), O'
_chemical_formula_sum            'C288 H480 Au Cl4 Na O241'
_chemical_formula_weight         8160.45
_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
_audit_creation_date             2015-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   23.761(12)
_cell_length_b                   23.761(12)
_cell_length_c                   22.836(17)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.594
_cell_measurement_theta_min      2.162
_cell_volume                     12893(13)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_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, 2015)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.03
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'QuazarTM optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            180452
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.047
_diffrn_reflns_theta_min         0.892
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1138 before and 0.0713 after correction.
The Ratio of minimum to maximum transmission is 0.7820.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.051
_exptl_crystal_description       block
_exptl_crystal_F_000             4294
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.442
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 4762 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.049(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         18893
_refine_ls_number_restraints     958
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0810
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1714P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2361
_refine_ls_wR_factor_ref         0.2521
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                12856
_reflns_number_total             18893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04986_si_014.cif
_cod_data_source_block           cx0597
_cod_depositor_comments
'Adding full bibliography for 4125213--4125224.cif.'
_cod_original_cell_volume        12893(16)
_cod_database_code               4125222
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.905
_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. Shared sites
{Na1, O1S}
3. Restrained distances
 O30-H30
 0.87 with sigma of 0.01
 O5-H5
 0.87 with sigma of 0.01
 C36-H30
 1.898121 with sigma of 0.02
 Na1-H30
 3.518381 with sigma of 0.02
 C6-H5
 1.953758 with sigma of 0.02
 Na1-H5
 3.411941 with sigma of 0.02
 Au1-Cl1A \\sim Au1-Cl1
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(Na1) = Uanis(O1S)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Sof(Cl1A)=0.5*(1-FVAR(2))
 Sof(Cl1)=0.5*FVAR(2)
 Fixed Sof: Na1(0.125) Au1(0.125)
7.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3A), C4(H4), C5(H5A), C7(H7A), C8(H8A), C9(H9),
 C10(H10A), C11(H11), C25(H25A), C26(H26), C27(H27A), C28(H28A), C29(H29),
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C13(H13A), C14(H14),
 C15(H15A), C16(H16), C17(H17A), C19(H19), C20(H20A), C21(H21), C22(H22A),
 C23(H23A)
7.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C30(H30A,H30B), C36(H36A,H36B), C18(H18A,H18B),
 C24(H24A,H24B)
7.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O3(H3), O7(H7), O8(H8), O10(H10), O22(H22), O23(H23), O25(H25),
 O27(H27), O28(H28), O12(H12), O13(H13), O15(H15), O17(H17), O18(H18), O20(H20)
;
_smtbx_masks_special_details
;
Total solvent accessible volume / cell = 4895.7 Ang^3^ [38.0%]
Total electron count / cell = 307.1

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.
;
_shelx_res_checksum              30530
_shelx_hkl_checksum              71945
_olex2_date_sample_data_collection 2015-10-26
_olex2_date_sample_submission    2015-10-23
_olex2_submission_original_sample_id cx0597
_olex2_submission_special_instructions 'No special instructions were received'