Triptycene-derived oxacalixarene with expanded cavity: synthesis, structure and its complexation with fullerenes C60 and C70
Hu, Shu-Zhen; Chen, Chuan-Feng; Chemical Communications 46 (2010) 4199–4201; doi:10.1039/c002944k

data_7111625
_publ_section_title
;
 Triptycene-derived oxacalixarene with expanded cavity: synthesis,
 structure and its complexation with fullerenes C60 and C70
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              4199
_journal_page_last               4201
_journal_paper_doi               10.1039/c002944k
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C56 H32 N4 O4'
_chemical_formula_weight         824.86
_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                90.79(3)
_cell_angle_beta                 105.31(3)
_cell_angle_gamma                107.40(3)
_cell_formula_units_Z            4
_cell_length_a                   16.802(3)
_cell_length_b                   18.474(4)
_cell_length_c                   18.656(4)
_cell_measurement_reflns_used    13670
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.14
_cell_volume                     5303(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics
;
Mercury: visualization and analysis of crystal structures, C. F. Macrae,
P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006.
;
_computing_publication_material  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELX-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELX-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'MM007HF + CCD (Saturn724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            71916
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.9928
_exptl_absorpt_correction_T_min  0.9883
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.033
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
;
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.582
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1190
_refine_ls_number_reflns         24266
_refine_ls_number_restraints     1075
_refine_ls_restrained_S_all      1.562
_refine_ls_R_factor_all          0.1450
_refine_ls_R_factor_gt           0.1101
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3047
_refine_ls_wR_factor_ref         0.3191
_reflns_number_gt                14468
_reflns_number_total             24266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002944ksup1.cif
_cod_data_source_block           mx379
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111625