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_4075090
_publ_section_title
;
 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
;
_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            'C86 H80 Ge4 Li O3.5'
_chemical_formula_weight         1466.80
_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                 99.8000(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4011(7)
_cell_length_b                   24.5315(11)
_cell_length_c                   21.9725(10)
_cell_measurement_temperature    293(2)
_cell_volume                     8180.3(6)
_computing_cell_refinement       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_collection       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_reduction        'BRUKER SMART CCD DIFFRACTOMETER'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER SMART CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA SCAN'
_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  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0894
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43596
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    1.500
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.570132
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3020
_exptl_crystal_size_max          1.01
_exptl_crystal_size_mid          0.86
_exptl_crystal_size_min          0.64
_refine_diff_density_max         0.862
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         14397
_refine_ls_number_restraints     583
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0658
_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^)+(0.1270P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.2129
_reflns_number_gt                6621
_reflns_number_total             14397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060032gsi20060323_041416.cif
_cod_data_source_block           scw212
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C86 H80 Ge4 Li O3.50'
_cod_database_code               4075090