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_4125216
_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 Cl4, C72 H122 O61 Rb, 4(H2 O)'
_chemical_formula_sum            'C72 H130 Au Cl4 O65 Rb'
_chemical_formula_weight         2459.99
_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             2014-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.2619(19)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9510(5)
_cell_length_b                   23.8573(10)
_cell_length_c                   16.0436(6)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.091
_cell_measurement_theta_min      3.333
_cell_volume                     5308.0(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  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.04
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.943
_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  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            99934
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.114
_diffrn_reflns_theta_min         2.771
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    5.010
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0586 before and 0.0459 after correction. The Ratio of minimum to maximum transmission is 0.8258. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             2532
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.071
_refine_diff_density_max         1.473
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Flack x determined using 8548 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.015(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1331
_refine_ls_number_reflns         18015
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0545P)^2^+15.6014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.933
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                17831
_reflns_number_total             18015
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04986_si_006.cif
_cod_data_source_block           n3428
_cod_depositor_comments
'Adding full bibliography for 4125213--4125224.cif.'
_cod_database_code               4125216
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.717
_shelx_estimated_absorpt_t_min   0.462
_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.a Free rotating group:
 O66(H66C,H66D), O62(H62A,H62B), O1A(H1AA,H1AB), O1B(H1BA,H1BB)
2.b Rotating group:
 O61(H61A,H61B)
2.c Ternary CH refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3A), C4(H4A), C5(H5), C7(H7A), C8(H8A), C9(H9A),
 C10(H10), C11(H11), C13(H13A), C14(H14A), C15(H15), C16(H16), C17(H17A),
 C19(H19A), C20(H20), C21(H21), C22(H22A), C23(H23A), C25(H25), C26(H26),
 C27(H27A), C28(H28A), C29(H29A), C31(H31), C32(H32A), C33(H33A), C34(H34A),
 C35(H35), C37(H37A), C38(H38A), C39(H39A), C40(H40), C41(H41), C43(H43A),
 C44(H44A), C45(H45), C46(H46), C47(H47A), C49(H49A), C50(H50), C51(H51),
 C52(H52A), C53(H53A), C55(H55), C56(H56), C57(H57A), C58(H58A), C59(H59A),
 C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C67(H67), C68(H68), C69(H69),
  C70(H70), C71(H71)
2.d Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C30(H30A,H30B),
 C36(H36A,H36B), C42(H42A,H42B), C48(H48A,H48B), C54(H54A,H54B), C60(H60A,H60B),
  C66(H66A,H66B), C72(H72A,H72B)
2.e Tetrahedral OH refined with riding coordinates:
 O12(H12), O14(H14), O24(H24), O27(H27), O33(H33), O34(H34)
2.f Idealised tetrahedral OH refined as rotating group:
 O2(H2), O3(H3), O4(H4), O7(H7), O8(H8), O9(H9), O13(H13), O17(H17), O18(H18),
 O19(H19), O22(H22), O23(H23), O28(H28), O29(H29), O32(H32), O37(H37), O38(H38),
  O39(H39), O42(H42), O43(H43), O44(H44), O47(H47), O48(H48), O49(H49),
 O52(H52), O53(H53), O54(H54), O57(H57), O58(H58), O59(H59)
;
_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 = 743.5 Ang^3^ [14.0%]
Total electron count / cell = 200.7
;
_shelx_res_checksum              82987
_shelx_hkl_checksum              37902