Ion pair-induced conformational motion in calix[4]arene-strapped calix[4]pyrroles
Kim, Sung Kuk; Lynch, Vincent M.; Hay, Benjamin P.; Kim, Jong Seung; Sessler, Jonathan L.; Chem. Sci. 6 (2015) 1404–; doi:10.1039/C4SC03272A

data_1518367
_publ_section_title
;
 Ion pair-induced conformational motion in calix[4]arene-strapped
 calix[4]pyrroles
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              1404
_journal_paper_doi               10.1039/C4SC03272A
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C72 H72 N4 O6, Cs 1+, F 1-, C H Cl3, C H4 O'
_chemical_formula_sum            'C74 H77 Cl3 Cs F N4 O7'
_chemical_formula_weight         1392.65
_chemical_name_systematic        ksk1823
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc13dwky
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-09-21 deposited with the CCDC.
2014-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.129(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1643(12)
_cell_length_b                   20.2720(15)
_cell_length_c                   20.1109(15)
_cell_measurement_reflns_used    24275
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     6909.0(9)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            70835
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.071
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.676
_refine_diff_density_min         -1.723
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         12132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0740
_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^)+(0.1069P)^2^+16.7082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1865
_refine_ls_wR_factor_ref         0.2053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8861
_reflns_number_total             12132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc03272a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 1518360--1518368.cif.'
_cod_database_code               1518367
_shelx_estimated_absorpt_t_min   0.883
_shelx_estimated_absorpt_t_max   0.932
_shelxl_version_number           2013-4
_shelx_res_checksum              4325
_shelx_fab_checksum              3516