Intramolecular iodoetherification of ene or diene ketals: facile synthesis of spiroketals.
Fujioka, Hiromichi; Nakahara, Kenji; Hirose, Hideki; Hirano, Kie; Oki, Tomohiro; Kita, Yasuyuki; Chemical communications (Cambridge, England) 47 (2011) 1060–1062; doi:10.1039/c0cc03933k

data_7112676
_publ_section_title
;
 Intramolecular iodoetherification of ene or diene ketals: facile
 synthesis of spiroketals.
;
_journal_issue                   3
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1060
_journal_page_last               1062
_journal_paper_doi               10.1039/c0cc03933k
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C24 H30 O3 '
_chemical_formula_sum            'C24 H30 O3'
_chemical_formula_weight         366.50
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_cell_angle_alpha                90
_cell_angle_beta                 95.628(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.207(2)
_cell_length_b                   5.884(1)
_cell_length_c                   18.682(2)
_cell_measurement_reflns_used    11336
_cell_measurement_temperature    291.1
_cell_measurement_theta_max      68.3
_cell_measurement_theta_min      4.6
_cell_volume                     2101.1(5)
_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
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9458
_diffrn_measured_fraction_theta_max 0.9458
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5419
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11374
_diffrn_reflns_theta_full        68.21
_diffrn_reflns_theta_max         68.21
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.599
_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    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             792.00
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.48
_refine_ls_extinction_coef       50(8)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3416
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.0150
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0026Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1360
_reflns_number_gt                3258
_reflns_number_total             3416
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c0cc03933k.txt
_cod_data_source_block           '_051207'
_cod_original_cell_volume        2101.0(5)
_cod_original_formula_sum        'C24 H30 O3 '
_cod_database_code               7112676