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_7224199
_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, 2(H4 N2)'
_chemical_formula_sum            'C48 H68 N8 O10 S4'
_chemical_formula_weight         1045.34
_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           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 108.104(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.723(8)
_cell_length_b                   13.121(3)
_cell_length_c                   25.422(6)
_cell_measurement_reflns_used    2427
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.20
_cell_measurement_theta_min      2.68
_cell_volume                     11326(5)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.971
_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_unetI/netI     0.3002
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13275
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.990
_diffrn_reflns_theta_min         2.376
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.912
_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. 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       plate
_exptl_crystal_F_000             4448
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH/CH2Cl2'
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.751
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         13275
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      0.763
_refine_ls_R_factor_all          0.2839
_refine_ls_R_factor_gt           0.0952
_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^)+(0.1389P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2080
_refine_ls_wR_factor_ref         0.2684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3458
_reflns_number_total             13275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra01730d2.cif
_cod_data_source_block           sample_4_af
_cod_original_cell_volume        11326(4)
_cod_database_code               7224199
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.913
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              92072