Binding Modes of Nonspherical Anions toN-Alkylammonium Resorcinarenes in the Solid State
Beyeh, N. Kodiah; Cetina, Mario; Rissanen, Kari; Crystal Growth & Design 12 (2012) 4919–; doi:10.1021/cg3008409

data_4506779
_publ_section_title
;
 Binding Modes of Nonspherical Anions toN-Alkylammonium Resorcinarenes in
 the Solid State
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4919
_journal_paper_doi               10.1021/cg3008409
_journal_volume                  12
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'C64 H96 N4 O8, 2.85(C F3 O3 S), 2(C H Cl3), 1.15(Cl)'
_chemical_formula_sum            'C68.85 H98 Cl7.15 F8.55 N4 O16.55 S2.85'
_chemical_formula_weight         1753.8
_chemical_name_systematic        'di-dichloromethane solvate'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-10-07T18:23:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 128.9170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.4470(9)
_cell_length_b                   24.8056(9)
_cell_length_c                   25.2165(8)
_cell_measurement_reflns_used    13077
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.368
_cell_measurement_theta_min      0.883
_cell_volume                     16278.1(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker-Nonius Kappa Apex II Diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1142
_diffrn_reflns_av_unetI/netI     0.0917
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            58807
_diffrn_reflns_theta_full        63.43
_diffrn_reflns_theta_max         63.43
_diffrn_reflns_theta_min         2.51
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.687
_exptl_absorpt_correction_T_max  0.7523
_exptl_absorpt_correction_T_min  0.6109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. SADABS 2008/2; University of G\"ottingen: G\"ottingen,
        Germany, 2008.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7325
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.078
_refine_diff_density_min         -2.034
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1001
_refine_ls_number_reflns         13188
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1747
_refine_ls_R_factor_gt           0.1367
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.4018P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.419
_refine_ls_wR_factor_ref         0.4653
_reflns_number_gt                8437
_reflns_number_total             13188
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg3008409_si_005.cif
_cod_data_source_block           5b_4H_3OTf_Cl
_cod_database_code               4506779