Synthesis of cyclic bis- and trismelamine derivatives and their complexation properties with barbiturates.
Kondo, Shin-Ichi; Hayashi, Tomohiro; Sakuno, Yuichi; Takezawa, Yoko; Yokoyama, Takashi; Unno, Masafumi; Yano, Yumihiko; Organic & biomolecular chemistry 5 (2007) 907–916; doi:10.1039/b615537e

data_7151058
_publ_section_title
;
 Synthesis of cyclic bis- and trismelamine derivatives and their
 complexation properties with barbiturates.
;
_journal_issue                   6
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              907
_journal_page_last               916
_journal_paper_doi               10.1039/b615537e
_journal_volume                  5
_journal_year                    2007
_chemical_formula_moiety         'C69 H100 N22 O6 '
_chemical_formula_sum            'C69 H100 N22 O6'
_chemical_formula_weight         1333.69
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                68.348(10)
_cell_angle_beta                 71.330(10)
_cell_angle_gamma                88.860(10)
_cell_formula_units_Z            2
_cell_length_a                   14.995(2)
_cell_length_b                   15.949(2)
_cell_length_c                   17.6433(4)
_cell_measurement_reflns_used    20400
_cell_measurement_temperature    113.1
_cell_measurement_theta_max      32.6
_cell_measurement_theta_min      1.4
_cell_volume                     3692.2(8)
_computing_cell_refinement       PROCESS
_computing_data_collection       PROCESS
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.730
_diffrn_measurement_device_type  'Rigaku RAXIS-IV++'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.1245
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39399
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1432.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.0018(4)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.830
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     885
_refine_ls_number_reflns         15745
_refine_ls_R_factor_all          0.1391
_refine_ls_R_factor_gt           0.0836
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2003
_refine_ls_wR_factor_ref         0.2368
_reflns_number_gt                5059
_reflns_number_total             15745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b615537e.txt
_cod_data_source_block           '__Host-guest'
_cod_original_formula_sum        'C69 H100 N22 O6 '
_cod_database_code               7151058