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_4125214
_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
'0.75(Au Cl4), Cl1, C36 H66 Na O33, C36 H60 O30, 2(H2 O)'
_chemical_formula_sum            'C72 H130 Au0.75 Cl4 Na O65'
_chemical_formula_weight         2348.27
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2014-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                93.585(2)
_cell_angle_beta                 89.976(2)
_cell_angle_gamma                118.8786(17)
_cell_formula_units_Z            1
_cell_length_a                   13.6582(7)
_cell_length_b                   13.9202(7)
_cell_length_c                   15.6235(9)
_cell_measurement_reflns_used    9102
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.385
_cell_measurement_theta_min      2.836
_cell_volume                     2594.4(2)
_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      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.977
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32512
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.152
_diffrn_reflns_theta_min         2.835
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.954
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0894 before and 0.0683 after correction.
The Ratio of minimum to maximum transmission is 0.8129.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       plate
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.051
_refine_diff_density_max         4.167
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details
;
 Flack x determined using 6331 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.012(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1363
_refine_ls_number_reflns         17248
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0936
_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^)+(0.1801P)^2^+9.0530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2476
_refine_ls_wR_factor_ref         0.2555
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    0.850
_reflns_Friedel_fraction_max     0.843
_reflns_number_gt                15575
_reflns_number_total             17248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04986_si_005.cif
_cod_data_source_block           n3389b
_cod_depositor_comments
'Adding full bibliography for 4125213--4125224.cif.'
_cod_database_code               4125214
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.824
_shelx_estimated_absorpt_t_min   0.659
_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
 O29-H29
 0.87 with sigma of 0.01
 O14-H14
 0.87 with sigma of 0.01
 C36-H29
 1.91273 with sigma of 0.02
 Na2-H29
 3.264709 with sigma of 0.02
 C18-H14
 1.898005 with sigma of 0.02
 Na1-H14
 3.426755 with sigma of 0.02
3. Rigid bond restraints
 Cl6, Cl5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl3, Cl2, Cl4, Cl1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl6 \\sim Cl5: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Cl3 \\sim Cl2 \\sim Cl4 \\sim Cl1: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(Cl5)=1-FVAR(1)
 Sof(Cl6)=FVAR(1)
 Fixed Sof: Au1(0.75) Cl1(0.75) Cl2(0.75) Cl3(0.75) Cl4(0.75) Na1(0.5) Na2(0.5)
6.a Free rotating group:
 O64(H64A,H64B), O65(H65A,H65B), O63(H63A,H63B)
6.b Rotating group:
 O61(H61A,H61B), O62(H62A,H62B)
6.c Ternary CH refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3), C4(H4A), C5(H5), C7(H7A), C8(H8), C9(H9A), C10(H10),
  C11(H11A), C13(H13), C14(H14A), C15(H15), C16(H16A), C17(H17A), C19(H19A),
 C20(H20), C21(H21A), C22(H22A), C23(H23), C25(H25), C26(H26A), C27(H27A),
 C28(H28), C29(H29A), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
 C37(H37A), C38(H38), C39(H39A), C40(H40), C41(H41A), C43(H43), C44(H44A),
 C45(H45), C46(H46A), C47(H47A), C49(H49A), C50(H50), C51(H51A), C52(H52A),
 C53(H53), C55(H55), C56(H56A), C57(H57A), C58(H58), C59(H59A), C61(H61),
 C62(H62), C63(H63), C64(H64), C65(H65), C67(H67), C68(H68), C69(H69), C70(H70),
  C71(H71)
6.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)
6.e Tetrahedral OH refined with riding coordinates:
 O4(H4), O9(H9), O19(H19), O24(H24)
6.f Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O6(H6), O7(H7), O11(H11), O12(H12), O16(H16), O17(H17),
 O21(H21), O22(H22), O26(H26), O27(H27), O31(H31A), O32(H32A), O34(H34A),
 O36(H36), O37(H37), O39(H39), O41(H41), O42(H42), O44(H44), O46(H46), O47(H47),
  O49(H49), O51(H51), O52(H52), O54(H54), O56(H56), O57(H57), 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 = 265.1 Ang^3^ [10.2%]
Total electron count / cell = 55.9
;
_shelx_res_checksum              78699
_shelx_hkl_checksum              28969