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_4329148
_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         'C136 H160 Ge2 N4 S2 Si6, 2(C6 H14)'
_chemical_formula_sum            'C148 H188 Ge2 N4 S2 Si6'
_chemical_formula_weight         2400.86
_chemical_name_systematic
; 
 ? 
;
_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                62.851(3)
_cell_angle_beta                 66.564(4)
_cell_angle_gamma                83.170(4)
_cell_formula_units_Z            1
_cell_length_a                   15.3279(11)
_cell_length_b                   16.5942(12)
_cell_length_c                   16.8715(13)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.78
_cell_measurement_theta_min      3.00
_cell_volume                     3493.2(5)
_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 0.950
_diffrn_measured_fraction_theta_max 0.933
_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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23551
_diffrn_reflns_theta_full        67.70
_diffrn_reflns_theta_max         70.20
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    1.668
_exptl_absorpt_correction_T_max  0.8699
_exptl_absorpt_correction_T_min  0.7074
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_platon_squeeze_details
; 
Attempts to refine peaks of residual electron density as disordered 
or partial-occupancy solvent hexane carbon atoms were unsuccessful. 
The data were corrected for disordered electron density through use 
of the SQUEEZE procedure (Sluis, P. van der; Spek, A. L. Acta 
Crystallogr. 1990, A46, 194-201) as implemented in PLATON (Spek, 
A. L. Acta Crystallogr. 1990, A46, C34; Spek, A. L. J. Appl. Cryst. 
2003, 36, 7-13.  PLATON - a multipurpose crystallographic tool. 
Utrecht University, Utrecht, The Netherlands).  A total solvent- 
accessible void volume of 591 \%A3 with a total electron count of 89 
(consistent with 2 molecules of solvent hexane, or 1 molecule per 
asymmetric unit) was found in the unit cell. 
;
_refine_diff_density_max         1.279
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         12426
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0722
_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^)+(0.1430P)^2^+0.8975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2076
_refine_ls_wR_factor_ref         0.2328
_reflns_number_gt                8900
_reflns_number_total             12426
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic300495k_si_001_7.cif
_cod_data_source_block           riv1190
_cod_original_cell_volume        3493.2(4)
_cod_database_code               4329148