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_4506777
_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         '2(C56 H96 N4 O8 4+), 8(N O3 1-), 5 (C2 H3 N)'
_chemical_formula_sum            'C138 H207 N21 O40'
_chemical_formula_weight         2800.25
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-05-27T13:05:44-00:00
_audit_creation_method           'WinGX routine-INITIALISE'
_cell_angle_alpha                100.1500(10)
_cell_angle_beta                 107.610(2)
_cell_angle_gamma                111.825(2)
_cell_formula_units_Z            2
_cell_length_a                   18.8851(6)
_cell_length_b                   21.7869(6)
_cell_length_c                   21.9992(7)
_cell_measurement_reflns_used    17940
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      90
_cell_measurement_theta_min      0.883
_cell_volume                     7570.7(4)
_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    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker-Nonius Kappa Apex II Diffractometer'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.586935E-1
_diffrn_orient_matrix_UB_12      0.143877E-1
_diffrn_orient_matrix_UB_13      0.45784E-2
_diffrn_orient_matrix_UB_21      -0.208918E-1
_diffrn_orient_matrix_UB_22      -0.329597E-1
_diffrn_orient_matrix_UB_23      -0.463826E-1
_diffrn_orient_matrix_UB_31      -0.14799E-2
_diffrn_orient_matrix_UB_32      0.379805E-1
_diffrn_orient_matrix_UB_33      -0.193156E-1
_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  0.0992
_diffrn_reflns_av_sigmaI/netI    0.1104
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            64681
_diffrn_reflns_theta_full        63.31
_diffrn_reflns_theta_max         63.31
_diffrn_reflns_theta_min         2.31
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.7523
_exptl_absorpt_correction_T_min  0.6191
_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    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             3004
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.590
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.00123(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1867
_refine_ls_number_reflns         23725
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1296
_refine_ls_R_factor_gt           0.0933
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2174P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2676
_refine_ls_wR_factor_ref         0.3007
_reflns_number_gt                15077
_reflns_number_total             23725
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg3008409_si_003.cif
_cod_data_source_block           4b_4H_4NO3_MeCN
_cod_database_code               4506777