Synthetic and Structural Exploration of [24]Tetrathiacalix[2]arene[2]pyrimidines
Mahendra P. Sonawane; Kristof Van Hecke; Jeroen Jacobs; Joice Thomas; Luc Van Meervelt; Wim Dehaen; Wim Van Rossom; Journal of Organic Chemistry 77 (2012) 8444–8450; doi:10.1021/jo301321w

data_4027545
_publ_section_title
;
 Synthetic and Structural Exploration of
 [24]Tetrathiacalix[2]arene[2]pyrimidines
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8444
_journal_page_last               8450
_journal_paper_doi               10.1021/jo301321w
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C32 H36 N4 O8 S4'
_chemical_formula_sum            'C32 H36 N4 O8 S4'
_chemical_formula_weight         732.93
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 90.2749(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.17209(14)
_cell_length_b                   18.4260(3)
_cell_length_c                   18.4308(3)
_cell_measurement_reflns_used    19775
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.4810
_cell_measurement_theta_min      2.3953
_cell_volume                     3454.46(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_publication_material  Platon
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2474
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) x-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11976
_diffrn_reflns_theta_full        66.59
_diffrn_reflns_theta_max         66.59
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    3.000
_exptl_absorpt_correction_T_max  0.8324
_exptl_absorpt_correction_T_min  0.7434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.552
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     881
_refine_ls_number_reflns         11976
_refine_ls_number_restraints     592
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0991P)^2^+3.0097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                11441
_reflns_number_total             11976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo301321w_si_001_3.cif
_cod_data_source_block           exp_102
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4027545