Synthesis of tetraazacalix[2]arene[2]triazines: tuning the cavity by the substituents on the bridging nitrogen atoms.
Wang, Qi-Qiang; Wang, De-Xian; Ma, Hong-Wei; Wang, Mei-Xiang; Organic letters 8 (2006) 5967–5970; doi:10.1021/ol062441e

data_1506306
_publ_section_title
;
 Synthesis of tetraazacalix[2]arene[2]triazines: tuning the cavity by the
 substituents on the bridging nitrogen atoms.
;
_journal_issue                   26
_journal_name_full               'Organic letters'
_journal_page_first              5967
_journal_page_last               5970
_journal_paper_doi               10.1021/ol062441e
_journal_volume                  8
_journal_year                    2006
_chemical_formula_sum            'C33.5 H27.5 Cl2 N10.5 O2.5'
_chemical_formula_weight         688.06
_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                76.66(3)
_cell_angle_beta                 89.07(3)
_cell_angle_gamma                88.22(3)
_cell_formula_units_Z            4
_cell_length_a                   13.477(3)
_cell_length_b                   15.305(3)
_cell_length_c                   16.878(3)
_cell_measurement_reflns_used    29318
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.24
_cell_volume                     3385.6(12)
_computing_cell_refinement       'Rapid Auto(Rigaku 2001)'
_computing_data_collection       'Rapid Auto(Rigaku 2001)'
_computing_data_reduction        'Rapid Auto(Rigaku 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  '\w oscillation'
_diffrn_measurement_method       'Rigaku Raxis Rapid IP Area Detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_sigmaI/netI    0.0826
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29318
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  0.9265
_exptl_absorpt_correction_T_min  0.8729
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Abscor
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       trunk
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         12807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1802
_refine_ls_R_factor_gt           0.1191
_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^)+(0.1356P)^2^+16.3978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3283
_refine_ls_wR_factor_ref         0.3646
_reflns_number_gt                7438
_reflns_number_total             12807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol062441esi20061004_092712.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3385.5(12)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C33.50 H27.50 Cl2 N10.50 O2.50'
_cod_database_code               1506306