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_4329147
_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         'C58 H78 Ge N2 Si4'
_chemical_formula_sum            'C58 H78 Ge N2 Si4'
_chemical_formula_weight         988.17
_chemical_name_common            12
_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                 116.4250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.6549(5)
_cell_length_b                   16.2623(4)
_cell_length_c                   21.0055(5)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.60
_cell_measurement_theta_min      2.64
_cell_volume                     5706.7(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.976
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28066
_diffrn_reflns_theta_full        67.80
_diffrn_reflns_theta_max         69.44
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    1.800
_exptl_absorpt_correction_T_max  0.6939
_exptl_absorpt_correction_T_min  0.5381
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.846
_refine_diff_density_min         -1.623
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         10446
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+6.8177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1791
_refine_ls_wR_factor_ref         0.1928
_reflns_number_gt                8581
_reflns_number_total             10446
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic300495k_si_001_6.cif
_cod_data_source_block           riv1194
_cod_original_cell_volume        5706.7(2)
_cod_database_code               4329147