Study of host-guest interactions in benzodiazacoronands by means of solid state NMR spectroscopy, X-ray diffraction and quantum mechanical computations.
Nowicka, Katarzyna; Bujacz, Anna; Paluch, Piotr; Sobczuk, Adam; Jeziorna, Agata; Ciesielski, Włodzimierz; Bujacz, Grzegorz D.; Jurczak, Janusz; Potrzebowski, Marek J.; Physical chemistry chemical physics : PCCP 13 (2011) 6423–6433; doi:10.1039/c0cp02401e

data_7205902
_publ_section_title
;
 Study of host-guest interactions in benzodiazacoronands by means of
 solid state NMR spectroscopy, X-ray diffraction and quantum mechanical
 computations.
;
_journal_issue                   14
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              6423
_journal_page_last               6433
_journal_paper_doi               10.1039/c0cp02401e
_journal_volume                  13
_journal_year                    2011
_chemical_absolute_configuration n/a
_chemical_formula_moiety         '4(C27 H27 N3 O7), 5(H2 O)'
_chemical_formula_sum            'C108 H118 N12 O33'
_chemical_formula_weight         2112.14
_chemical_name_common            benzodiazacoronand
_chemical_name_systematic
;
N-(4,19-Dioxo-2,8,15,21-tetraoxa-5,18-diazatricyclohexacosa-
-1(25),9(14),10,12,22(26),23-hexaen-26-yl)-benzamide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.868(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.375(2)
_cell_length_b                   27.574(2)
_cell_length_c                   23.898(3)
_cell_measurement_temperature    100(2)
_cell_volume                     10148(2)
_computing_cell_refinement       DENZO-SCALEPACK
_computing_data_collection       MAR-CCD
_computing_data_reduction        SCALEPACK
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'single axis goniomether with CCD detector'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  'Si111 crystal'
_diffrn_radiation_source         'DESY Hamburg X13'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80880
_diffrn_reflns_av_R_equivalents  0.0094
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            46172
_diffrn_reflns_theta_full        32.65
_diffrn_reflns_theta_max         32.65
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4456
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0072(3)
_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   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1852
_refine_ls_number_reflns         23305
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0806P)^2^+2.9851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1331
_reflns_number_gt                21525
_reflns_number_total             25231
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cp02401e.txt
_cod_data_source_block           eter_cor_H20
_cod_original_cell_volume        10148.2(19)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7205902
_exptl_crystal_f_000'            4455.29