Regioselective synthesis of 1,2- and 1,3-diaminothiacalix[4]arenes via nucleophilic aromatic substitution and their X-ray structures
Katagiri, Hiroshi; Tanaka, Shinya; Ohkubo, Kazuya; Akahira, Yuki; Morohashi, Naoya; Iki, Nobukiho; Hattori, Tetsutaro; Miyano, Sotaro; RSC Advances 4 (2014) 9608–; doi:10.1039/c3ra47718e

data_7239484
_publ_section_title
;
 Regioselective synthesis of 1,2- and 1,3-diaminothiacalix[4]arenes via
 nucleophilic aromatic substitution and their X-ray structures
;
_journal_issue                   19
_journal_name_full               'RSC Advances'
_journal_page_first              9608
_journal_paper_doi               10.1039/c3ra47718e
_journal_volume                  4
_journal_year                    2014
_chemical_absolute_configuration ' ?'
_chemical_formula_sum            'C42 H53 N3 O2 S4'
_chemical_formula_weight         760.11
_space_group_IT_number           130
_space_group_name_Hall           '-P 4a 2ac'
_space_group_name_H-M_alt        'P 4/n c c :2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3887(16)
_cell_length_b                   15.3887(16)
_cell_length_c                   17.563(3)
_cell_measurement_reflns_used    3362
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.90
_cell_measurement_theta_min      2.65
_cell_volume                     4159.1(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD''
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayered confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0937
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21688
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6023
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'phi and omega scans'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2396
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1084P)^2^+4.7899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2036
_refine_ls_wR_factor_ref         0.2528
_reflns_number_gt                1447
_reflns_number_total             2396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra47718e.txt
_cod_data_source_block           5c_MeCN
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Tetragonal' was changed to
'tetragonal' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        4159.2(9)
_cod_original_sg_symbol_H-M      P4/ncc
_cod_database_code               7239484