Synthesis and Characterization of β-Diketiminate Germanium(II) Compounds
Ying Yang; Na Zhao; Yile Wu; Hongping Zhu; Herbert W. Roesky; Inorganic Chemistry 51 (2012) 2425–2431; doi:10.1021/ic202388d

data_4328396
_publ_contact_author
;
Herbert W. ROESKY
;
_publ_contact_author_address
;
Institut fuer Anorganische Chemie
Universitaet Goettingen
Tammannstrasse 4, 37077 Goettingen (Germany)
;
_publ_contact_author_email       hroesky@gwdg.de
_publ_section_title
;
 Synthesis and Characterization of \b-Diketiminate Germanium(II) Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2425
_journal_page_last               2431
_journal_paper_doi               10.1021/ic202388d
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C33 H50 Ge N2 O'
_chemical_formula_weight         563.34
_chemical_name_common            LGeOtBu
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 107.07(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.341(3)
_cell_length_b                   16.611(3)
_cell_length_c                   15.085(3)
_cell_measurement_reflns_used    22644
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      55.00
_cell_measurement_theta_min      6.08
_cell_volume                     3195.7(12)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_data_reduction
;
CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30657
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_T_max  0.8126
_exptl_absorpt_correction_T_min  0.5897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       Block
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         7307
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.5500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0823
_reflns_number_gt                5839
_reflns_number_total             7307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202388d_si_001_2.cif
_cod_data_source_block           yy256
_cod_original_cell_volume        3195.7(11)
_cod_database_code               4328396