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_4506776
_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(C52 H80 N4 O8), 8(C6 H2 N3 O7), 3(C4 H10 O), 3(C H Cl3), H2 O'
_chemical_formula_sum            'C167 H211 Cl9 N32 O76'
_chemical_formula_weight         4201.73
_chemical_melting_point          ???:???
_chemical_name_systematic
;
 three-butanol solvate di-cloroform solvate monohydrate
;
_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             2010-10-10T19:11:26-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                102.069(6)
_cell_angle_beta                 95.145(6)
_cell_angle_gamma                96.104(6)
_cell_formula_units_Z            2
_cell_length_a                   15.635(2)
_cell_length_b                   19.086(2)
_cell_length_c                   34.414(4)
_cell_measurement_reflns_used    28068
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      63.691
_cell_measurement_theta_min      0.883
_cell_volume                     9919(2)
_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 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.1879
_diffrn_reflns_av_unetI/netI     0.1638
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            122171
_diffrn_reflns_theta_full        63.53
_diffrn_reflns_theta_max         63.53
_diffrn_reflns_theta_min         2.46
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.015
_exptl_absorpt_correction_T_max  0.7523
_exptl_absorpt_correction_T_min  0.6229
_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            yellow
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4396
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.898
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2595
_refine_ls_number_reflns         31484
_refine_ls_number_restraints     244
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.2250
_refine_ls_R_factor_gt           0.1438
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2641P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3655
_refine_ls_wR_factor_ref         0.4294
_reflns_number_gt                13815
_reflns_number_total             31484
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg3008409_si_002.cif
_cod_data_source_block           3a_4H_4Pic
_cod_database_code               4506776