Rim-functionalized cryptophane-111 derivatives via heterocapping, and their xenon complexes
Akil I. Joseph; Gracia El-Ayle; Celine Boutin; Estelle Leonce; Patrick Berthault; K. Travis Holman; Chem.Commun. 50 (2014) 15905–; doi:10.1039/C4cc08001G

data_7116138
_publ_section_title
;
 Rim-functionalized cryptophane-111 derivatives via heterocapping, and
 their xenon complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              15905
_journal_paper_doi               10.1039/C4cc08001G
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety
'0.018 (C45 H30 Br6 O6), 0.982 (C45 H33 Br3 O6)'
_chemical_formula_sum            'C45 H32.94 Br3.06 O6'
_chemical_formula_weight         913.78
_chemical_name_common            trisbromo-cryptophane-111
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.9160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6375(10)
_cell_length_b                   30.647(3)
_cell_length_c                   11.2147(10)
_cell_measurement_reflns_used    6910
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.079
_cell_measurement_theta_min      2.259
_cell_volume                     3636.6(6)
_computing_cell_refinement       'SAINT, Bruker-AXS'
_computing_data_collection       'APEX, Bruker-AXS'
_computing_data_reduction        'SAINT, Bruker-AXS'
_computing_molecular_graphics
'X-SEED, L. Barbour (1999); http://x-seed.net/'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97, G. Sheldrick (1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Siemens SMART, Bruker APEXII CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28012
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.94
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.441
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick (1999)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1831
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Nitrobenzene'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0538P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                6427
_reflns_number_total             8291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc08001g2.cif
_cod_data_source_block           13037
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7116138