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_7205901
_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_formula_moiety         '2(C27 H27 N3 O7), C3 H6 O, 5(H2 O)'
_chemical_formula_sum            'C57 H70 N6 O20'
_chemical_formula_weight         1159.19
_chemical_melting_point          506.84
_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           2
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.24(3)
_cell_angle_beta                 72.99(3)
_cell_angle_gamma                72.58(3)
_cell_formula_units_Z            2
_cell_length_a                   11.932(2)
_cell_length_b                   16.268(3)
_cell_length_c                   16.358(3)
_cell_measurement_temperature    100(2)
_cell_volume                     2866.0(11)
_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 0.856
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'single axis goniometer with CCD detector'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  'Si111 crystal'
_diffrn_radiation_source         'BESY Berlin BL14.2'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82657
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14226
_diffrn_reflns_theta_full        33.44
_diffrn_reflns_theta_max         33.44
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         '1.062 H32C 1.45'
_refine_diff_density_min         '-1.127 O3W 0.33'
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     997
_refine_ls_number_reflns         12182
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+2.7338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1505
_reflns_number_gt                11552
_reflns_number_total             14226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cp02401e.txt
_cod_data_source_block           eter_cor_aceton
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '233.69 oC' was changed to '506.84' -
it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        2866.0(10)
_cod_database_code               7205901
_exptl_crystal_f_000'            1227.81