Reactivity Study of a Pyridyl-1-azaallylgermanium(I) Dimer: Synthesis of Heavier Ether and Ester Analogues of Germanium.
Leung, Wing-Por; Chan, Yuk-Chi; So, Cheuk-Wai; Mak, Thomas C. W.; Inorganic chemistry 55 (2016) 3553–3557; doi:10.1021/acs.inorgchem.6b00026

data_4347335
_publ_section_title
;
 Reactivity Study of a Pyridyl-1-azaallylgermanium(I) Dimer: Synthesis of
 Heavier Ether and Ester Analogues of Germanium.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3553
_journal_page_last               3557
_journal_paper_doi               10.1021/acs.inorgchem.6b00026
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C40 H59 Ge2 N4 O0.5 Si4 Te2'
_chemical_formula_weight         1116.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                84.4139(17)
_cell_angle_beta                 73.5680(15)
_cell_angle_gamma                70.8713(16)
_cell_formula_units_Z            2
_cell_length_a                   11.4954(3)
_cell_length_b                   12.3514(4)
_cell_length_c                   18.8350(5)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      30.3248
_cell_measurement_theta_min      2.1671
_cell_volume                     2423.39(12)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2013)'
_computing_publication_material  'APEX2 (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      103.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            111290
_diffrn_reflns_theta_full        31.07
_diffrn_reflns_theta_max         31.07
_diffrn_reflns_theta_min         2.56
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.551
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1110
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_refine_diff_density_max         1.906
_refine_diff_density_min         -1.909
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         15462
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+3.9783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0777
_reflns_number_gt                12165
_reflns_number_total             15462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00026_si_002.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C40 H59 Ge2 N4 O0.50 Si4 Te2'
_cod_database_code               4347335
_shelx_res_checksum              13343
_shelx_hkl_checksum              57206