Conformational mobility of 7,16-bis(4-methoxybenzyl)-1,4,10,13-tetraoxa-7,16-diazacyclooctadecane in molecular and proton-transfer complexes: X-ray and DFT studies
Fonari, Marina S.; Ganin, Eduard V.; Chumakov, Yurii M.; Botoshansky, Mark M.; Suwinska, Kinga; Basok, Stepan S.; Simonov, Yurii A.; New Journal of Chemistry 33 (2009) 1646–; doi:10.1039/b902953b

data_7051706
_publ_section_title
;
 Conformational mobility of
 7,16-bis(4-methoxybenzyl)-1,4,10,13-tetraoxa-7,16-diazacyclooctadecane
 in molecular and proton-transfer complexes: X-ray and DFT studies
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1646
_journal_paper_doi               10.1039/b902953b
_journal_volume                  33
_journal_year                    2009
_chemical_formula_moiety         'C28 H44 N2 O6, 2(Ta F6), 2(H2 O)'
_chemical_formula_sum            'C28 H48 F12 N2 O8 Ta2'
_chemical_formula_weight         1130.58
_chemical_name_common
;
7,16-bis(4-methoxybenzyl)-1,4,10,13-tetraoxa-7,16-
diazoniacyclooctadecane dihexafluorotantalate dihydrate
;
_chemical_name_systematic
;
7,16-bis(4-methoxybenzyl)-1,4,10,13-tetraoxa-7,16-
diazoniacyclooctadecane dihexafluorotantalate dihydrate
;
_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                105.873(9)
_cell_angle_beta                 101.336(9)
_cell_angle_gamma                106.175(6)
_cell_formula_units_Z            1
_cell_length_a                   6.8062(11)
_cell_length_b                   11.3381(18)
_cell_length_c                   14.098(2)
_cell_measurement_temperature    293(2)
_cell_volume                     960.2(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker CCD diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5444
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    5.797
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.290
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            light-brown
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.751
_refine_diff_density_min         -1.973
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3640
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1169P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1874
_reflns_number_gt                2021
_reflns_number_total             3640
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b902953b.txt
_cod_data_source_block           ych1
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2016-12-29
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7051706