Synthesis, structure and coordinating properties of novel bifunctional carboxylic derivatives of 1,3-alternate tetrathiacalix[4]arene
Podyachev, Sergey Nicolaevich; Gimazetdinova, Gulnaz; Gubaidullin, Aidar Timergalievich; Syakaev, Victor Vasil'evich; Sudakova, Svetlana; Gabidullin, Bulat; Ivanov, Vladimir Timofeevich; Gogolashvili, Edward Lavrentievich; Konovalov, Alexander Ivanovich; RSC Adv.  (2016) –; doi:10.1039/C6RA01730D

data_7224198
_publ_section_title
;
 Synthesis, structure and coordinating properties of novel bifunctional
 carboxylic derivatives of 1,3-alternate tetrathiacalix[4]arene
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA01730D
_journal_year                    2016
_chemical_formula_moiety         'C48 H60 N4 O10 S4, C2 H6 O S'
_chemical_formula_sum            'C50 H66 N4 O11 S5'
_chemical_formula_weight         1059.36
_chemical_melting_point          545
_chemical_name_systematic
'5,11,17,23-Tetra-tert-butyl-25,27-di[(hydrazinocarbonyl)methoxy]-26,28-di[(hydroxycarbonyl)methoxy]- 2,8,14,20-tetrathiacalix[4]arene'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-17 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.473(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.163(5)
_cell_length_b                   29.199(11)
_cell_length_c                   15.137(5)
_cell_measurement_reflns_used    3329
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17.12
_cell_measurement_theta_min      2.46
_cell_volume                     5816(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.1259
_diffrn_reflns_av_unetI/netI     0.1996
_diffrn_reflns_laue_measured_fraction_full 0.987
_diffrn_reflns_laue_measured_fraction_max 0.873
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            67104
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.536
_diffrn_reflns_theta_min         1.697
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 G.M. Sheldrick (1998a). SADABS v.2.01, Bruker.
 Siemens Area Detector Absorption Correction Program.
 Bruker AXS. Madison. Wisconsin. USA

 The maximum experimental transmission factor Tmax is equal to the 
 one estimated by SHELX. The minimum experimental transmission factor 
 Tmin is calculated as a product of Tmax and the Tmin-to-Tmax-ratio, 
 evaluated by SADABS.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       prism
_exptl_crystal_F_000             2248
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMSO'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.070
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.6670
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         15532
_refine_ls_number_restraints     447
_refine_ls_restrained_S_all      0.875
_refine_ls_R_factor_all          0.2629
_refine_ls_R_factor_gt           0.1075
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1693P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2694
_refine_ls_wR_factor_ref         0.3323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4474
_reflns_number_total             15532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra01730d2.cif
_cod_data_source_block           sample_4_ae
_cod_database_code               7224198
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.939
_shelx_estimated_absorpt_t_max   0.982
_shelx_res_checksum              1925