Exhaustively methylated azacalix[4]arene: preparation, conformation, and crystal structure with exclusively CH/pi-controlled crystal architecture.
Tsue, Hirohito; Ishibashi, Koichi; Takahashi, Hiroki; Tamura, Rui; Organic letters 7 (2005) 2165–2168; doi:10.1021/ol050493i

data_1506561
_publ_section_title
;
 Exhaustively methylated azacalix[4]arene: preparation, conformation, and
 crystal structure with exclusively CH/pi-controlled crystal architecture.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2165
_journal_page_last               2168
_journal_paper_doi               10.1021/ol050493i
_journal_volume                  7
_journal_year                    2005
_chemical_formula_moiety         'C48 H68 N4 O4 '
_chemical_formula_sum            'C48 H68 N4 O4'
_chemical_formula_weight         765.09
_chemical_melting_point_gt       300
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_cell_angle_alpha                90
_cell_angle_beta                 116.40(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.64(1)
_cell_length_b                   16.890(6)
_cell_length_c                   12.682(5)
_cell_measurement_reflns_used    15498
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      3.0
_cell_volume                     4536(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.6.0'
_computing_structure_refinement  CRYSTALS
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9987
_diffrn_measured_fraction_theta_max 0.9987
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.099
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25100
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1664.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.38
_refine_diff_density_min         -2.26
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     340
_refine_ls_number_reflns         6370
_refine_ls_R_factor_gt           0.0920
_refine_ls_shift/su_max          0.2290
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[0.0101Fo^2^ + 1.0000\s(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1360
_reflns_number_gt                6370
_reflns_number_total             25100
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol050493isi20050308_023523.cif
_cod_data_source_block           '_NMe-ACA4-OMe'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '>300' was changed to
'300' - it should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4535(3)
_cod_original_formula_sum        'C48 H68 N4 O4 '
_cod_database_code               1506561