Reactivity Control of an Allylsilane Bearing a 2-(Phenylazo)phenyl Group by Photoswitching of the Coordination Number of Silicon
Naokazu Kano; Masaki Yamamura; Takayuki Kawashima; Journal of the American Chemical Society 126 (2004) 6250–6251; doi:10.1021/ja037404m

data_4112582
_publ_contact_author_address
;
Department of Chemistry, Graduate School of Science,
The University of Tokyo,
7-3-1 Hongo, Bunkyo-ku, Tokyo, 113-0033, Japan
;
_publ_contact_author_email       takayuki@chem..s.u-tokyo.ac.jp
_publ_contact_author_fax         +81-5800-6899
_publ_contact_author_name        'Takayuki Kawashima'
_publ_contact_author_phone       +81-5800-6899
_publ_section_title
;
 Reactivity Control of an Allylsilane Bearing a 2-(Phenylazo)phenyl Group
 by Photoswitching of the Coordination Number of Silicon
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6250
_journal_page_last               6251
_journal_paper_doi               10.1021/ja037404m
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C27 H39 F4 K N2 O6 Si, 2(C H Cl3)'
_chemical_formula_sum            'C29 H41 Cl6 F4 K N2 O6 Si'
_chemical_formula_weight         869.53
_chemical_name_common
;
potassium 
tetrafluoro{2-[2-phenyl-1-(2-propenyl)-hydrazino]phenyl}silicate,
 18-crown-6
;
_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                86.45(3)
_cell_angle_beta                 76.75(3)
_cell_angle_gamma                67.67(2)
_cell_formula_units_Z            2
_cell_length_a                   9.522(5)
_cell_length_b                   11.167(5)
_cell_length_c                   20.225(10)
_cell_measurement_reflns_used    6437
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      13.7
_cell_measurement_theta_min      1.7
_cell_volume                     1935.6(17)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        YadokariXG
_computing_molecular_graphics    'ORTEP-III ver. 1.0.3'
_computing_publication_material  YadokariXG
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14714
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  0.9097
_exptl_absorpt_correction_T_min  0.6798
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.138
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         8309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+1.8745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0883
_reflns_number_gt                7694
_reflns_number_total             8309
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja037404msi20030719_090519.cif
_cod_data_source_block           allylsilicate
_cod_original_cell_volume        1935.6(16)
_cod_database_code               4112582