Novel calixarene hemisphere synthesized via pinacol rearrangement of [2.1.2.1]metacyclophane.
Sawada, Tsuyoshi; Nishiyama, Yousuke; Tabuchi, Wataru; Ishikawa, Makoto; Tsutsumi, Emi; Kuwahara, Yutaka; Shosenji, Hideto; Organic letters 8 (2006) 1995–1997; doi:10.1021/ol060286y

data_1505914
_publ_section_title
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 Novel calixarene hemisphere synthesized via pinacol rearrangement of
 [2.1.2.1]metacyclophane.
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_journal_issue                   10
_journal_name_full               'Organic letters'
_journal_page_first              1995
_journal_page_last               1997
_journal_paper_doi               10.1021/ol060286y
_journal_volume                  8
_journal_year                    2006
_chemical_formula_moiety         'C46 H52 O4, C2 H3 N '
_chemical_formula_sum            'C48 H55 N O4'
_chemical_formula_weight         709.93
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.365(5)
_cell_length_b                   21.338(6)
_cell_length_c                   16.49(2)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    298.1
_cell_measurement_theta_max      12.09
_cell_measurement_theta_min      7.20
_cell_volume                     3999(5)
_computing_cell_refinement       WinAFC
_computing_data_collection       WinAFC
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.6.0'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7448
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.90
_diffrn_standards_decay_%        -1.25
_diffrn_standards_interval_count 0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1528.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.22
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4708
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1045P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2440
_reflns_number_gt                2934
_reflns_number_total             4708
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol060286ysi20060202_101212.cif
_cod_data_source_block           '_calixarene5a'
_cod_depositor_comments
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The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_formula_sum        'C48 H55 N O4 '
_cod_database_code               1505914