Reactivity of Pyridyl-1-azaallyl Germanium(II) Chloride: Synthesis of Novel Lithium Germinate [{(PhC⋮C)3Ge}3GeLi(Et2O)3] and Ge(II)−M(I) (M = Cu and Au) Adducts
Leung, Wing-Por; So, Cheuk-Wai; Chong, Kim-Hung; Kan, Kwok-Wai; Chan, Hoi-Shan; Mak, Thomas C. W.; Organometallics 25 (2006) 2851–; doi:10.1021/om060032g

data_4075086
_publ_section_title
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 Reactivity of Pyridyl-1-azaallyl Germanium(II) Chloride:&#x00A0;
 Synthesis of Novel Lithium Germinate [{(PhC&#x22EE;C)3Ge}3GeLi(Et2O)3]
 and Ge(II)&#x2212;M(I) (M = Cu and Au) Adducts
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_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2851
_journal_paper_doi               10.1021/om060032g
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C27 H32 Ge N2 Si2'
_chemical_formula_weight         513.32
_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                107.28(3)
_cell_angle_beta                 90.39(3)
_cell_angle_gamma                100.47(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3622(17)
_cell_length_b                   11.227(2)
_cell_length_c                   16.899(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1486.6(6)
_computing_cell_refinement       'BIOTEX RIGAKU'
_computing_data_collection       'RAXIS-IIC RIGAKU'
_computing_data_reduction        'BIOTEX RIGAKU'
_computing_molecular_graphics    'SIEMENS SHELXTL'
_computing_publication_material  'SIEMENS SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.837
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_device_type  'RAXIS-IIC RIGAKU'
_diffrn_measurement_method       IP
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4499
_diffrn_reflns_theta_full        25.23
_diffrn_reflns_theta_max         25.23
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  0.8061
_exptl_absorpt_correction_T_min  0.6029
_exptl_absorpt_correction_type   ABSCOR
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4499
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+0.5071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1486
_reflns_number_gt                4191
_reflns_number_total             4499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060032gsi20060111_015917.cif
_cod_data_source_block           ckh48
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1486.6(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075086