The First Halogen-Substituted Cyclotrigermenes: A Unique Halogen Walk over the Three-Membered Ring Skeleton and Facial Stereoselectivity in the Diels-Alder Reaction
Akira Sekiguchi; Yutaka Ishida; Norihisa Fukaya; Masaaki Ichinohe; Nozomi Takagi; Shigeru Nagase; Journal of the American Chemical Society 124 (2002) 1158–1159; doi:10.1021/ja012216m

data_4114616
_publ_section_title
;
 The First Halogen-Substituted Cyclotrigermenes: A Unique Halogen Walk
 over the Three-Membered Ring Skeleton and Facial Stereoselectivity in the
 Diels-Alder Reaction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1158
_journal_page_last               1159
_journal_paper_doi               10.1021/ja012216m
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C36 H81 Cl Ge3 Si3'
_chemical_formula_weight         851.52
_chemical_name_systematic
; 
 3-Chloro-1,2,3-tris(tri-tert-butylsilyl)cyclotrigermene 
;
_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                89.037(4)
_cell_angle_beta                 79.917(4)
_cell_angle_gamma                81.937(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6690(7)
_cell_length_b                   12.9930(9)
_cell_length_c                   20.8670(7)
_cell_measurement_reflns_used    23137
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.92
_cell_measurement_theta_min      2.41
_cell_volume                     2291.1(3)
_computing_cell_refinement       'HKL scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        Denzo
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'MacScience DIP2030 Image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23137
_diffrn_reflns_theta_full        27.92
_diffrn_reflns_theta_max         27.92
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    2.114
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       Plate
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         5.916
_refine_diff_density_min         -1.307
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.0112(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         10094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1119P)^2^+7.1922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1828
_refine_ls_wR_factor_ref         0.1992
_reflns_number_gt                7739
_reflns_number_total             10094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja012216m_1.cif
_cod_data_source_block           shelxl
_cod_original_formula_sum        'C36 H81 Cl1 Ge3 Si3'
_cod_database_code               4114616