Expanding the Steric Coverage Offered by Bis(amidosilyl) Chelates: Isolation of Low-Coordinate N-Heterocyclic Germylene Complexes
Sean K. Liew; S. M. Ibrahim Al-Rafia; James T. Goettel; Paul A. Lummis; Sean M. McDonald; Leah J. Miedema; Michael J. Ferguson; Robert McDonald; Eric Rivard; Inorganic Chemistry 51 (2012) 5471–5480; doi:10.1021/ic300495k

data_4329144
_publ_contact_author_address
;
Department of Chemistry
University of Alberta
Edmonton
AB T6G 2G2
CANADA
;
_publ_contact_author_email       ERIVARD@UALBERTA.CA
_publ_contact_author_name        'E. Rivard'
_publ_section_title
;
 Expanding the Steric Coverage Offered by Bis(amidosilyl) Chelates:
 Isolation of Low-Coordinate N-Heterocyclic Germylene Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5471
_journal_page_last               5480
_journal_paper_doi               10.1021/ic300495k
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C56 H92 Ge2 N4 S2 Si4, C7 H8, C4 H8 O'
_chemical_formula_sum            'C67 H108 Ge2 N4 O S2 Si4'
_chemical_formula_weight         1307.23
_chemical_name_common            4
_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                102.871(3)
_cell_angle_beta                 93.857(3)
_cell_angle_gamma                107.097(2)
_cell_formula_units_Z            1
_cell_length_a                   9.960(2)
_cell_length_b                   14.101(3)
_cell_length_c                   15.228(3)
_cell_measurement_reflns_used    5998
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.34
_cell_measurement_theta_min      2.16
_cell_volume                     1972.5(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w 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  0.0641
_diffrn_reflns_av_sigmaI/netI    0.0873
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14188
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  0.9363
_exptl_absorpt_correction_T_min  0.7569
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_description       rod
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.865
_refine_diff_density_min         -1.461
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7124
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0870
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1643P)^2^+3.9378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2477
_refine_ls_wR_factor_ref         0.2703
_reflns_number_gt                5240
_reflns_number_total             7124
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic300495k_si_001_3.cif
_cod_data_source_block           riv1142
_cod_original_cell_volume        1972.6(8)
_cod_database_code               4329144