Synthesis and Structure of Upper-Rim 1,3-Alternate Tetraoxacalix[2]arene[2]triazine Azacrowns and Change of Cavity in Response to Fluoride Anion
Bao-Yong Hou; De-Xian Wang; Hai-Bo Yang; Qi-Yu Zheng; Mei-Xiang Wang; Journal of Organic Chemistry 72 (2007) 5218–5226; doi:10.1021/jo0706168

data_4023996
_publ_section_title
;
 Synthesis and Structure of Upper-Rim
 1,3-Alternate Tetraoxacalix[2]arene[2]triazine Azacrowns
 and Change of Cavity in Response to Fluoride Anion
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5218
_journal_page_last               5226
_journal_paper_doi               10.1021/jo0706168
_journal_volume                  72
_journal_year                    2007
_chemical_formula_sum            'C48 H50 N8 O14'
_chemical_formula_weight         962.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 119.35(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.154(5)
_cell_length_b                   13.507(3)
_cell_length_c                   18.307(4)
_cell_measurement_reflns_used    5958
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.79
_cell_volume                     5206.0(18)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Raxis Rapid IP'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1402
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5958
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.9900
_exptl_absorpt_correction_T_min  0.9792
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   abscor
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.417
_refine_diff_density_min         -1.878
_refine_diff_density_rms         0.382
_refine_ls_extinction_coef       0.012(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.471
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         5958
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.487
_refine_ls_R_factor_all          0.4487
_refine_ls_R_factor_gt           0.2236
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2750P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5351
_refine_ls_wR_factor_ref         0.6645
_reflns_number_gt                1548
_reflns_number_total             5958
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo0706168si20070324_094451.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4023996