A bis(disulfide)-linked offset cryptophane
Marc A. Little; Malcolm A. Halcrow; Michaele J. Hardie; Chemical communications (Cambridge, England) 49 (2013) 1512–1514; doi:10.1039/c3cc38768b

data_7108849
_publ_section_title
;
 A bis(disulfide)-linked offset cryptophane
;
_journal_issue                   15
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1512
_journal_page_last               1514
_journal_paper_doi               10.1039/c3cc38768b
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C48 H44 O8 S4, C3 H6 N O, C4 H10 O,'
_chemical_formula_sum            'C55 H61 N O10 S4'
_chemical_formula_weight         1024.29
_chemical_name_common            bis(disulfide)-cryptophane-0.0
_chemical_name_systematic
;
bis(disulfide)-cryptophane-0.0
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.075(5)
_cell_angle_beta                 104.370(5)
_cell_angle_gamma                103.986(11)
_cell_formula_units_Z            2
_cell_length_a                   11.768(7)
_cell_length_b                   15.158(8)
_cell_length_c                   15.531(8)
_cell_measurement_temperature    150(2)
_cell_volume                     2599(2)
_computing_cell_refinement       'CrystalClear-SM Expert2.0(Rigaku, 2009)'
_computing_data_collection       'CrystalClear-SM Expert2.0 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert2.0(Rigaku, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
Number of images: 175
Slice: -60.0000 - 115.0000
Image width: 1.0000
Exp time: 1.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 0.0000
Phi: 0.0000
XTD: 59.7553
2theta: 30.0294
scan:
Number of images: 120
Slice: -60.0000 - 60.0000
Image width: 1.0000
Exp time: 1.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: -50.0000
Phi: 0.0000
XTD: 59.7553
2theta: 30.0294
scan:
Number of images: 120
Slice: -60.0000 - 60.0000
Image width: 1.0000
Exp time: 1.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: -50.0000
Phi: 120.0000
XTD: 59.7553
2theta: 30.0294
scan:
Number of images: 120
Slice: -60.0000 - 60.0000
Image width: 1.0000
Exp time: 1.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: -50.0000
Phi: 240.0000
XTD: 59.7553
2theta: 30.0294
scan:
Number of images: 120
Slice: -10.0000 - 110.0000
Image width: 1.0000
Exp time: 1.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 50.0000
Phi: 0.0000
XTD: 59.7553
2theta: 30.0294
scan:
Number of images: 120
Slice: -10.0000 - 110.0000
Image width: 1.0000
Exp time: 1.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 50.0000
Phi: 120.0000
XTD: 59.7553
2theta: 30.0294
scan:
Number of images: 120
Slice: -10.0000 - 110.0000
Image width: 1.0000
Exp time: 1.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 50.0000
Phi: 240.0000
XTD: 59.7553
2theta: 30.0294
;
_diffrn_measurement_device       'CrystalLogic Kappa (3 circle)'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_source         Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41458
_diffrn_reflns_theta_full        26.64
_diffrn_reflns_theta_max         26.64
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  0.9809
_exptl_absorpt_correction_T_min  0.9354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
See Sheldrick, G. M. (2002). SADABS.
University of Gottingen, Germany.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         11619
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0939P)^2^+2.0428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1804
_refine_ls_wR_factor_ref         0.1821
_reflns_number_gt                11134
_reflns_number_total             11619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc38768b.txt
_cod_data_source_block           compound_3
_cod_original_cell_volume        2598(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7108849