Low-Coordinate Germylene and Stannylene Heterocycles featuring Sterically Tunable Bis(amido)silyl Ligands
S. M. Ibrahim Al-Rafia; Paul A. Lummis; Michael J. Ferguson; Robert McDonald; Eric Rivard; Inorganic Chemistry 49 (2010) 9709–9717; doi:10.1021/ic101485a

data_4316857
_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
;
 Low-Coordinate Germylene and Stannylene Heterocycles featuring Sterically
 Tunable Bis(amido)silyl Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9709
_journal_page_last               9717
_journal_paper_doi               10.1021/ic101485a
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C60 H96 Ge2 N4 O2 Si2, 2(C4 H10 O)'
_chemical_formula_sum            'C68 H116 Ge2 N4 O4 Si2'
_chemical_formula_weight         1255.01
_chemical_name_common            'Compound 7'
_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                82.9780(10)
_cell_angle_beta                 78.9340(10)
_cell_angle_gamma                79.3030(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8221(6)
_cell_length_b                   15.7103(7)
_cell_length_c                   19.1054(9)
_cell_measurement_reflns_used    4920
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.45
_cell_volume                     3696.4(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 0.998
_diffrn_measured_fraction_theta_max 0.979
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16911
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_T_max  0.8992
_exptl_absorpt_correction_T_min  0.6687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         16911
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+2.2226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                13235
_reflns_number_total             16911
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic101485a_si_001_08.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               4316857