Hydrogen bond-assisted solid-state formation of a salt-bridged calix[5]arene pseudo-dimer
Brancatelli, Giovanna; Pappalardo, Sebastiano; Gattuso, Giuseppe; Notti, Anna; Pisagatti, Ilenia; Parisi, Melchiorre F.; Geremia, Silvano; CrystEngComm 16 (2014) 89–; doi:10.1039/c3ce41667d

data_7214087
_publ_section_title
;
 Hydrogen bond-assisted solid-state formation of a salt-bridged
 calix[5]arene pseudo-dimer
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              89
_journal_paper_doi               10.1039/c3ce41667d
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety
'2(C81 H119 O7), 2(C4 H12 N1), 2(C81 H120 O7), 2(C2 H3 N1)'
_chemical_formula_sum            'C336 H508 N4 O28'
_chemical_formula_weight         5051.46
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                90.92(4)
_cell_angle_beta                 88.87(2)
_cell_angle_gamma                74.53(2)
_cell_formula_units_Z            2
_cell_length_a                   21.54(2)
_cell_length_b                   25.710(15)
_cell_length_c                   31.950(10)
_cell_measurement_temperature    100(2)
_cell_volume                     17045(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.888
_diffrn_measured_fraction_theta_max 0.888
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_wavelength     0.77491
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            38444
_diffrn_reflns_theta_full        24.41
_diffrn_reflns_theta_max         24.41
_diffrn_reflns_theta_min         6.36
_exptl_absorpt_coefficient_mu    0.049
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    0.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5552
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0102(6)
_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   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3422
_refine_ls_number_reflns         38444
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.1276
_refine_ls_shift/su_max          0.114
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1302P)^2^+79.9471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3302
_refine_ls_wR_factor_ref         0.3342
_reflns_number_gt                33223
_reflns_number_total             38444
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3ce41667d.txt
_cod_data_source_block           dimer
_cod_original_cell_volume        17045(19)
_cod_database_code               7214087