Selective isolation of gold facilitated by second-sphere coordination with alpha-cyclodextrin
Zhichang Liu; Marco Frasconi; Juying Lei; Zachary J. Brown; Zhixue Zhu; Dennis Cao; Julien Iehl; Guoliang Liu; Albert C. Fahrenbach; Youssry Y. Botros; Omar K. Farha; Joseph T. Hupp; Chad A. Mirkin; J. Fraser Stoddart; Nature Communications 4 (2013) 1855–; doi:10.1038/ncomms2891

data_1548331
_publ_section_title
;
 Selective isolation of gold facilitated by second-sphere coordination
 with alpha-cyclodextrin
;
_journal_name_full               'Nature Communications'
_journal_page_first              1855
_journal_paper_doi               10.1038/ncomms2891
_journal_volume                  4
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Au Br4, C84 H143 K O72'
_chemical_formula_sum            'C84 H143 Au Br4 K O72'
_chemical_formula_weight         2860.69
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 108.4010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.8246(4)
_cell_length_b                   24.5009(6)
_cell_length_c                   19.0924(5)
_cell_measurement_reflns_used    9035
_cell_measurement_temperature    109(2)
_cell_measurement_theta_max      66.58
_cell_measurement_theta_min      3.03
_cell_volume                     7024.0(3)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XM, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      109.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            86562
_diffrn_reflns_theta_full        67.05
_diffrn_reflns_theta_max         67.05
_diffrn_reflns_theta_min         1.80
_diffrn_source                   microsource
_diffrn_source_current           0.64
_diffrn_source_power             0.0285824
_diffrn_source_voltage           44.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.357
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.5839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0919 before and 0.0778 after correction.
The Ratio of minimum to maximum transmission is 0.7755.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2922
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.081
_refine_diff_density_max         3.619
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.073(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1526
_refine_ls_number_reflns         23851
_refine_ls_number_restraints     1524
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1643P)^2^+16.2172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2180
_refine_ls_wR_factor_ref         0.2225
_reflns_number_gt                22244
_reflns_number_total             23851
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ncomms2891-s4.cif
_cod_data_source_block           n1374
_cod_database_code               1548331
_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.  Only the
atoms used in the refinement model are reported in the formula here.

Total solvent accessible volume / cell = 1973.0 Ang^3^ [28.1%]
Total electron count / cell = 394.1
;