A Tripyrrolylmethane-Based Macrobicyclic Triazacryptand: X-ray Structure, Size-Selective Anion Binding, and Fluoride-Ion-Mediated Proton-Deuterium Exchange Studies
Tapas Guchhait; Ganesan Mani; Carola Schulzke; Anakuthil Anoop; Inorganic Chemistry 51 (2012) 11635–11644; doi:10.1021/ic301546v

data_4330876
_publ_section_title
;
 A Tripyrrolylmethane-Based Macrobicyclic Triazacryptand: X-ray Structure,
 Size-Selective Anion Binding, and Fluoride-Ion-Mediated Proton-Deuterium
 Exchange Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11635
_journal_page_last               11644
_journal_paper_doi               10.1021/ic301546v
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C53 H85 F N10 O2'
_chemical_formula_weight         913.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 106.130(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2318(16)
_cell_length_b                   17.875(2)
_cell_length_c                   23.693(3)
_cell_measurement_reflns_used    68804
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      1.45
_cell_volume                     5383.2(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker-APEX-II CCD area detector'
_diffrn_measurement_method       hemisphere
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1387
_diffrn_reflns_av_sigmaI/netI    0.1322
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            68804
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.9864
_exptl_absorpt_correction_T_min  0.9807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_description       prism
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         10841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.2233
_refine_ls_R_factor_gt           0.0826
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+0.4611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1818
_reflns_number_gt                4180
_reflns_number_total             10841
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic301546v_si_002_2.cif
_cod_data_source_block           fluoridecomplex
_cod_original_cell_volume        5383.3(11)
_cod_database_code               4330876