Synthesis, structure, and extraction behavior of 4,5′,4″,5‴-tetra-tert-butyltetrabenzo-24-crown-8 †‡
Levitskaia, Tatiana G.; Sachleben, Richard A.; Bryan, Jeffrey C.; Moyer, Bruce A.; Journal of the Chemical Society, Perkin Transactions 2  (2001) 808–; doi:10.1039/b008603g

data_7213445
_publ_section_title
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 Synthesis, structure, and extraction behavior of
 4,5&#x2032;,4&#x2033;,5&#x2034;-tetra-tert-butyltetrabenzo-24-crown-8&#x200A;&#x2020;&#x2021;
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_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              808
_journal_paper_doi               10.1039/b008603g
_journal_year                    2001
_chemical_formula_moiety         'C48 H64 O8'
_chemical_formula_sum            'C48 H64 O8'
_chemical_formula_weight         768.99
_chemical_name_common
;
tetra(t-butylbenzo)-24-crown-8
;
_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                76.083(14)
_cell_angle_beta                 82.120(12)
_cell_angle_gamma                89.600(13)
_cell_formula_units_Z            1
_cell_length_a                   5.8214(8)
_cell_length_b                   10.7769(19)
_cell_length_c                   17.258(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.4
_cell_measurement_theta_min      10.1
_cell_volume                     1040.6(3)
_computing_cell_refinement       'CAD4-PC (Enraf-Nonius, 1993)'
_computing_data_collection       'CAD4-PC (Enraf-Nonius, 1993)'
_computing_data_reduction        'XCAD4 (Harms, 1995)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Nonius CAD4'
_diffrn_measurement_method       Omega-scans
_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  0.023
_diffrn_reflns_av_sigmaI/netI    0.039
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5827
_diffrn_reflns_theta_full        27.0
_diffrn_reflns_theta_max         27.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        6
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            fragment
_exptl_crystal_density_diffrn    1.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       colorless
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.42
_refine_diff_density_min         -0.26
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.068
_refine_ls_R_factor_gt           0.047
_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^)+(0.0766P)^2^+0.3047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.126
_refine_ls_wR_factor_ref         0.137
_reflns_number_gt                3514
_reflns_number_total             4533
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008603gsup1.cif
_cod_data_source_block           tbb4
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7213445