Reactivity of LGe‒NR2 and LGe(E)‒NR2 over LGe‒Cl and LGe(E)‒Cl toward Me3SiX (L = Aminotroponiminate; NR2 = N(SiMe3)2/NC4H4; E = S/Se; X = Br/CN)
Siwatch, Rahul Kumar; Karwasara, Surendar; Sharma, Mahendra Kumar; Mondal, Santigopal; Mukherjee, Goutam; Rajaraman, Gopalan; Nagendran, Selvarajan; Organometallics 35 (2016) 429–; doi:10.1021/acs.organomet.5b00643

data_4087848
_publ_section_title
;
 Reactivity of LGe--NR2 and LGe(E)--NR2 over LGe--Cl and LGe(E)--Cl toward
 Me3SiX (L = Aminotroponiminate; NR2 = N(SiMe3)2/NC4H4; E = S/Se; X =
 Br/CN)
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              429
_journal_paper_doi               10.1021/acs.organomet.5b00643
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C16 H23 Ge N3'
_chemical_formula_sum            'C16 H23 Ge N3'
_chemical_formula_weight         329.98
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.281(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.187(3)
_cell_length_b                   16.231(4)
_cell_length_c                   7.8031(19)
_cell_measurement_reflns_used    855
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.68
_cell_measurement_theta_min      2.51
_cell_volume                     1669.7(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0642
_diffrn_reflns_av_sigmaI/netI    0.0911
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7064
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    1.830
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             688.0
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0648P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1382
_reflns_number_gt                2109
_reflns_number_total             2945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00643_si_001.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4087848