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_4125224
_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         'C72 H124 O62 Rb, Au Br4, C2 H6 O, 6(H2 O)'
_chemical_formula_sum            'C74 H142 Au Br4 O69 Rb'
_chemical_formula_weight         2737.95
_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             2014-04-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.259(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.3791(10)
_cell_length_b                   14.2585(8)
_cell_length_c                   23.6538(13)
_cell_measurement_reflns_used    9567
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.092
_cell_measurement_theta_min      6.232
_cell_volume                     5524.1(5)
_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      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.988
_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  0.0325
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            89002
_diffrn_reflns_point_group_measured_fraction_full 0.930
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.132
_diffrn_reflns_theta_min         1.868
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    5.671
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0646 before and 0.0494 after correction.
The Ratio of minimum to maximum transmission is 0.8081.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       block
_exptl_crystal_F_000             2788
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.136
_refine_diff_density_max         3.384
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details
;
 Flack x determined using 8774 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.021(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1455
_refine_ls_number_reflns         18593
_refine_ls_number_restraints     1283
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0805P)^2^+27.2857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1424
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.925
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                18529
_reflns_number_total             18593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04986_si_003.cif
_cod_data_source_block           n3438
_cod_depositor_comments
'Adding full bibliography for 4125213--4125224.cif.'
_cod_database_code               4125224
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.513
_shelx_estimated_absorpt_t_min   0.349
_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 C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O52-H52
 0.87 with sigma of 0.01
 O51-H51
 0.87 with sigma of 0.01
 O16-H16
 0.87 with sigma of 0.01
 O17-H17
 0.87 with sigma of 0.01
 C63-H52
 1.874318 with sigma of 0.02
 Rb1-H52
 3.464094 with sigma of 0.02
 C62-H51
 1.884118 with sigma of 0.02
 Rb1-H51
 3.667195 with sigma of 0.02
 C20-H16
 1.911582 with sigma of 0.02
 Rb1-H16
 3.209211 with sigma of 0.02
 C21-H17
 1.894768 with sigma of 0.02
 Rb1-H17
 4.253243 with sigma of 0.02
3. Rigid bond restraints
 Rb2, Rb3, Rb1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Br2A, Br1, Br3A, Br1A, Br3, Br2, Br4, Br4A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Rb2 \\sim Rb3 \\sim Rb1: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Br2A \\sim Br1 \\sim Br3A \\sim Br1A \\sim Br3 \\sim Br2 \\sim Br4 \\sim Br4A:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(Rb2)]+1*[Sof(Rb1)]+1*[Sof(Rb3)]=1 with esd of 0.00001
 Sof(Br1A)=Sof(Br2A)=Sof(Br3A)=Sof(Br4A)=1-FVAR(3)
 Sof(Br1)=Sof(Br2)=Sof(Br3)=Sof(Br4)=FVAR(3)
7.a Free rotating group:
 O64(H64A,H64B), O65(H65A,H65B), O66(H66C,H66D), O68(H68A,H68B), O69(H69A,H69B)
7.b Rotating group:
 O61(H61A,H61B), O62(H62A,H62B), O63(H63A,H63B)
7.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(H31A), C32(H32A), C33(H33), C34(H34A), 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)
7.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), C73(H73A,H73B)
7.e Tetrahedral OH refined with riding coordinates:
 O4(H4), O14(H14), O24(H24), O34(H34), O37(H37), O39(H39), O41(H41), O54(H54),
 O56(H56)
7.f Idealised Me refined as rotating group:
 C74(H74A,H74B,H74C)
7.g Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O6(H6), O7(H7), O9(H9), O11(H11), O12(H12), O19(H19),
 O21(H21), O22(H22), O26(H26), O27(H27), O29(H29), O31(H31), O32(H32), O36(H36),
  O42(H42), O44(H44), O46(H46), O47(H47), O49(H49), O57(H57), O59(H59),
 O70(H70A)
;
_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 = 417.5 Ang^3^ [7.6%]
Total electron count / cell = 75.0
;
_shelx_res_checksum              53464
_shelx_hkl_checksum              48639