Liquid Crystal and Crystal Structure of Octahomotetraoxacalix[4]arenes
Shigeo Kohmoto; Yasunobu Someya; Hyuma Masu; Kentaro Yamaguchi; Keiki Kishikawa; Journal of Organic Chemistry 71 (2006) 4509–4515; doi:10.1021/jo060355m

data_4021735
_publ_contact_author_address
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 Department of Applied Chemistry and Biotechnology,
 Faculty of Engineering, Chiba University,
 1-33, Yayoi-cho, Inage-ku, Chiba 263-8522, Japan
;
_publ_contact_author_email       kohmoto@faculty.chiba-u.jp
_publ_contact_author_name        'Shigeo Kohmoto'
_publ_contact_author_phone       +81-43-290-3420
_publ_section_title
;
 Liquid Crystal and Crystal Structure of Octahomotetraoxacalix[4]arenes
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_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4509
_journal_page_last               4515
_journal_paper_doi               10.1021/jo060355m
_journal_volume                  71
_journal_year                    2006
_chemical_formula_sum            'C68 H96 O16'
_chemical_formula_weight         1169.45
_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                102.227(2)
_cell_angle_beta                 94.988(2)
_cell_angle_gamma                99.295(2)
_cell_formula_units_Z            1
_cell_length_a                   9.7628(9)
_cell_length_b                   12.5244(11)
_cell_length_c                   13.9344(12)
_cell_measurement_reflns_used    2085
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.3575
_cell_measurement_theta_min      2.4505
_cell_volume                     1630.3(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      150
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker Smart1000 CCD'
_diffrn_measurement_method       '\w 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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9851
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.9835
_exptl_absorpt_correction_T_min  0.9754
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.058
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         7111
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0715
_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^)+(0.1120P)^2^+0.5752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1973
_refine_ls_wR_factor_ref         0.2268
_reflns_number_gt                4272
_reflns_number_total             7111
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo060355msi20060221_055154.cif
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4021735