Preparation, Structural Characterization, and Photochemical Reactions of Silyl- and Germylborates
Nanjo, Masato; Matsudo, Kazuhiko; Kurihara, Mari; Nakamura, Sayaka; Sakaguchi, Yoshio; Hayashi, Hisaharu; Mochida, Kunio; Organometallics 25 (2006) 832–; doi:10.1021/om050733y

data_4074661
_publ_section_title
;
 Preparation, Structural Characterization, and Photochemical Reactions of
 Silyl- and Germylborates
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              832
_journal_paper_doi               10.1021/om050733y
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C24 H30 B Ge Li'
_chemical_formula_weight         408.82
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.114(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1640(12)
_cell_length_b                   11.3280(5)
_cell_length_c                   16.1220(14)
_cell_measurement_temperature    293(2)
_cell_volume                     2187.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3066
_diffrn_reflns_theta_full        23.33
_diffrn_reflns_theta_max         23.33
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    1.405
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0052(11)
_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   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                2647
_reflns_number_total             3066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050733ysi20050825_031322.cif
_cod_data_source_block           shelxl
_cod_database_code               4074661