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_4027543
_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 S4'
_chemical_formula_sum            'C32 H36 N4 S4'
_chemical_formula_weight         604.93
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.263(9)
_cell_angle_beta                 94.180(8)
_cell_angle_gamma                103.759(9)
_cell_formula_units_Z            1
_cell_length_a                   5.4838(8)
_cell_length_b                   9.3179(16)
_cell_length_c                   15.686(2)
_cell_measurement_temperature    100(2)
_cell_volume                     776.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  Platon
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'SMART 6000'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'crossed G\"obel mirrors'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1120
_diffrn_reflns_av_sigmaI/netI    0.0977
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14061
_diffrn_reflns_theta_full        66.60
_diffrn_reflns_theta_max         66.60
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    3.024
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.364
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'WinGX v1.70.01'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       plate
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0821
_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^)+(0.0000P)^2^+4.8533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1960
_refine_ls_wR_factor_ref         0.2032
_reflns_number_gt                2180
_reflns_number_total             2681
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo301321w_si_001_1.cif
_cod_data_source_block           wim152
_cod_original_cell_volume        776.3(2)
_cod_database_code               4027543