Synthesis, crystal structures and reactions of sila- and germa-β-diketiminates
Farwell, James D.; Fernandes, Manuel A.; Hitchcock, Peter B.; Lappert, Michael F.; Layh, Marcus; Omondi, Bernard; Dalton Transactions  (2003) 1719–; doi:10.1039/b300817g

data_7012748
_publ_section_title
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 Synthesis, crystal structures and reactions of sila- and
 germa-\b-diketiminates
;
_journal_issue                   9
_journal_name_full               'Dalton Transactions'
_journal_page_first              1719
_journal_paper_doi               10.1039/b300817g
_journal_year                    2003
_chemical_formula_moiety         'C46 H74 Ge2 N4 Si6'
_chemical_formula_sum            'C46 H74 Ge2 N4 Si6'
_chemical_formula_weight         996.81
_chemical_name_systematic
;
(Trimethylsilyl)-bis[(trimethylsilyl)imino-(phenyl)methyl]digermane
;
_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                114.225(2)
_cell_angle_beta                 109.868(2)
_cell_angle_gamma                92.296(2)
_cell_formula_units_Z            1
_cell_length_a                   10.2204(13)
_cell_length_b                   12.0349(15)
_cell_length_c                   13.3254(17)
_cell_measurement_temperature    293(2)
_cell_volume                     1374.6(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8262
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.257
_exptl_absorpt_correction_T_max  0.6892
_exptl_absorpt_correction_T_min  0.3976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS: Area-Detector Absorption 
Correction. (1996)  Siemens Industrial Automation, Inc.: Madison, WI.. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'pearl shape'
_exptl_crystal_F_000             526
_exptl_crystal_preparation       'grown from hexane at -60 C'
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.841
_refine_diff_density_min         -1.463
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1102
_reflns_number_gt                4640
_reflns_number_total             5346
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300817g.txt
_cod_data_source_block           f:\marcus\pdgeket\work\soln\pdgeket
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012748