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_1518366
_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+, Cl 1-, C H4 O, C H Cl3'
_chemical_formula_sum            'C74 H77 Cl4 Cs N4 O7'
_chemical_formula_weight         1409.10
_chemical_name_systematic        ksk1818
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc13dwjx
_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                 90.135(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.4416(13)
_cell_length_b                   17.3237(8)
_cell_length_c                   28.5922(14)
_cell_measurement_reflns_used    4168
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      16.7
_cell_measurement_theta_min      2.2
_cell_volume                     14087.7(11)
_computing_cell_refinement       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_collection       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_reduction        'Apex II release 2010, Bruker AXS, Inc.'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/Plus, Siemens Analytical'
_computing_structure_refinement  'Shelxl-2013, Sheldrick, G. M. 2013'
_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      153(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
'Nonius Kappa CCD with Bruker Apex II detector'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2210
_diffrn_reflns_av_unetI/netI     0.2928
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            90097
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.009
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS. Apex II release 2010, Bruker AXS, Inc.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       plates
_exptl_crystal_F_000             5824
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.636
_refine_diff_density_min         -1.330
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.839
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1557
_refine_ls_number_reflns         24546
_refine_ls_number_restraints     1026
_refine_ls_restrained_S_all      1.819
_refine_ls_R_factor_all          0.3235
_refine_ls_R_factor_gt           0.1786
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3976
_refine_ls_wR_factor_ref         0.4448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9383
_reflns_number_total             24546
_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               1518366
_shelxl_version_number           2013-4
_shelx_res_checksum              76331
_shelx_fab_checksum              72615