Synthesis of a Dialuminum-Substituted Silicotungstate and the Diastereoselective Cyclization of Citronellal Derivatives
Yuji Kikukawa; Syuhei Yamaguchi; Yoshinao Nakagawa; Kazuhiro Uehara; Sayaka Uchida; Kazuya Yamaguchi; Noritaka Mizuno; Journal of the American Chemical Society 130 (2008) 15872–15878; doi:10.1021/ja8014154

data_4108702
_publ_contact_author_email       tmizuno@mail.ecc.u-tokyo.ac.jp
_publ_contact_author_fax         +81-3-5841-7220
_publ_contact_author_name        'Professor Noritaka Mizuno'
_publ_contact_author_phone       +81-3-5841-7272
_publ_section_title
;
 Synthesis of a Dialuminum-Substituted Silicotungstate and the
 Diastereoselective Cyclization of Citronellal Derivatives
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15872
_journal_page_last               15878
_journal_paper_doi               10.1021/ja8014154
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C65 H129 Al2 N7 O38 Si W10 '
_chemical_formula_sum            'C65 H129 Al2 N7 O38 Si W10'
_chemical_formula_weight         3537.31
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_audit_creation_date             2008-02-15
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   24.7994(2)
_cell_length_b                   14.58220(10)
_cell_length_c                   26.8752(3)
_cell_measurement_temperature    153.2
_cell_volume                     9718.87(15)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS97
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            13393
_diffrn_reflns_theta_full        29.35
_diffrn_reflns_theta_max         29.35
_exptl_absorpt_coefficient_mu    11.907
_exptl_absorpt_correction_T_max  0.3826
_exptl_absorpt_correction_T_min  0.1995
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.417
_exptl_crystal_description       block
_exptl_crystal_F_000             6608.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.79
_refine_diff_density_min         -3.74
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_number_parameters     556
_refine_ls_number_reflns         13393
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.0130
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0915P)^2^+333.4876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1963
_reflns_number_gt                11602
_reflns_number_total             13393
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja8014154_si_003.cif
_cod_data_source_block           '_Template_texray.inf'
_cod_original_formula_sum        'C65 H129 Al2 N7 O38 Si W10 '
_cod_database_code               4108702