Triptycene-Based Expanded Oxacalixarenes: Synthesis, Structure, and Tubular Assemblies in the Solid State
Chun Zhang; Chuan-Feng Chen; Journal of Organic Chemistry 72 (2007) 3880–3888; doi:10.1021/jo0702490

data_4022921
_publ_section_title
;
 Triptycene-Based Expanded Oxacalixarenes: Synthesis,
 Structure, and Tubular Assemblies in the Solid State
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3880
_journal_page_last               3888
_journal_paper_doi               10.1021/jo0702490
_journal_volume                  72
_journal_year                    2007
_chemical_formula_sum            'C52 H30 Cl8 N2 O4'
_chemical_formula_weight         1030.38
_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                95.19(3)
_cell_angle_beta                 93.16(3)
_cell_angle_gamma                96.43(3)
_cell_formula_units_Z            1
_cell_length_a                   8.7116(17)
_cell_length_b                   9.7063(19)
_cell_length_c                   13.761(3)
_cell_measurement_reflns_used    9410
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.49
_cell_volume                     1149.0(4)
_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 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Rigaku raxis Rapid IP'
_diffrn_measurement_method       '\w oscillation'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9410
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  0.9540
_exptl_absorpt_correction_T_min  0.6928
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   abscor
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0729
_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^)+(0.0957P)^2^+1.3546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.2136
_reflns_number_gt                3246
_reflns_number_total             4982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo0702490si20070206_041821.cif
_cod_data_source_block           a
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2018-01-29

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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4022921