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_7224202
_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         'C36 H36 N4 O10 S4'
_chemical_formula_sum            'C36 H36 N4 O10 S4'
_chemical_formula_weight         812.93
_chemical_melting_point          443.0(10)
_chemical_name_systematic
'25,27-Di[(hydrazinocarbonyl)methoxy]-26,28-di[(ethoxycarbonyl)methoxy]-2,8,14,20-tetrathiacalix[4]arene '
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.046(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9936(9)
_cell_length_b                   18.4615(15)
_cell_length_c                   20.6801(17)
_cell_measurement_reflns_used    5782
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.86
_cell_measurement_theta_min      2.26
_cell_volume                     3805.9(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 0.978
_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  0.0689
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47387
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.498
_diffrn_reflns_theta_min         1.974
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.916
_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
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       plate
_exptl_crystal_F_000             1696
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         9433
_refine_ls_number_restraints     354
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1632
_refine_ls_R_factor_gt           0.0606
_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^)+(0.0878P)^2^+0.2624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1482
_refine_ls_wR_factor_ref         0.1905
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4234
_reflns_number_total             9433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra01730d2.cif
_cod_data_source_block           sample_7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '442-444' was changed to '443.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               7224202
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.878
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              12823