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_7224201
_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         'C60 H66 N6 O10 S4, (C O H4)'
_chemical_formula_sum            'C61 H70 N6 O11 S4'
_chemical_formula_weight         1191.47
_chemical_melting_point          471
_chemical_name_common
5,11,17,23-Tetra-tert-butyl-25,27-Di[((2-pyridinylmethylidene)hydrazinocarbonyl)-methoxy]-26,28-di[(hydroxycarbonyl)methoxy]-2,8,14,20-tetrathiacalix[4]arene
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                71.891(12)
_cell_angle_beta                 85.063(18)
_cell_angle_gamma                69.735(12)
_cell_formula_units_Z            2
_cell_length_a                   13.783(13)
_cell_length_b                   15.091(14)
_cell_length_c                   17.68(2)
_cell_measurement_reflns_used    1205
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      16.85
_cell_measurement_theta_min      2.37
_cell_volume                     3278(6)
_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 1.000
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2261
_diffrn_reflns_av_unetI/netI     0.4454
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39008
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.027
_diffrn_reflns_theta_min         1.575
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.829
_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    1.207
_exptl_crystal_description       block
_exptl_crystal_F_000             1260
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH/CH2Cl2'
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.037
_platon_squeeze_details
;
;
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         16924
_refine_ls_number_restraints     690
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.3498
_refine_ls_R_factor_gt           0.1530
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4178
_refine_ls_wR_factor_ref         0.4690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3408
_reflns_number_total             16924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra01730d2.cif
_cod_data_source_block           sample_5
_cod_database_code               7224201
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.978
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              43980