Factors driving the self-assembling of water-soluble calix[4]arene and gemini guests: a combined solution, computational and solid-state study
Bonaccorso, Carmela; Brancatelli, Giovanna; Forte, Giuseppe; Arena, Giuseppe; Geremia, Silvano; Sciotto, Domenico; Sgarlata, Carmelo; RSC Adv.  (2014) –; doi:10.1039/C4RA09353D

data_7218425
_publ_section_title
;
 Factors driving the self-assembling of water-soluble calix[4]arene and
 gemini guests: a combined solution, computational and solid-state study
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA09353D
_journal_year                    2014
_chemical_formula_sum            'C168 H215.67 Cl6 N12 O46 S6'
_chemical_formula_weight         3544.24
_space_group_crystal_system      trigonal
_space_group_IT_number           145
_space_group_name_Hall           'P 32'
_space_group_name_H-M_alt        'P 32'
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   35.50(2)
_cell_length_b                   35.50(2)
_cell_length_c                   14.800(10)
_cell_measurement_temperature    100(2)
_cell_volume                     16153(17)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Dectris Pilatus 2M'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38600
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.352
_diffrn_source
'synchrotron, Elettra synchrotron Trieste (Italy)'
_exptl_absorpt_coefficient_mu    0.194
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_F_000             5621
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 15604 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.09(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2208
_refine_ls_number_reflns         38600
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0820
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.042
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1751P)^2^+1.3615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2123
_refine_ls_wR_factor_ref         0.2202
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                35651
_reflns_number_total             38600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra09353d2.cif
_cod_data_source_block           bsc2_3
_cod_original_cell_volume        16153(21)
_cod_database_code               7218425
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.971
_shelxl_version_number           2013-4
_shelx_res_checksum              87231
_shelx_fab_checksum              12689