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_4347334
_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            'C38 H54 Ge2 N4 Se2 Si4'
_chemical_formula_weight         982.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 93.6396(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0939(4)
_cell_length_b                   16.1868(4)
_cell_length_c                   19.7136(5)
_cell_measurement_reflns_used    6507
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      22.9266
_cell_measurement_theta_min      2.2229
_cell_volume                     4488.3(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      103.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0984
_diffrn_reflns_av_unetI/netI     0.0933
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47419
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    3.099
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.697
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     925
_refine_ls_number_reflns         9209
_refine_ls_number_restraints     2474
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1288
_refine_ls_R_factor_gt           0.0648
_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^)+30.9022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1430
_reflns_number_gt                5626
_reflns_number_total             9209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00026_si_002.cif
_cod_data_source_block           I
_cod_database_code               4347334
_shelx_res_checksum              94230
_shelx_hkl_checksum              96009