Hydrometallation of amino-trialkynylsilanes - intramolecular M-N interactions (M = Al, Ga) and potential activation of Si-N bonds.
Uhl, Werner; Bohnemann, Jörg; Kappelt, Benedikt; Hepp, Alexander; Layh, Marcus; Dalton transactions (Cambridge, England : 2003) 43 (2014) 14386–14398; doi:10.1039/c4dt00922c

data_7031277
_publ_section_title
;
 Hydrometallation of amino-trialkynylsilanes - intramolecular M-N
 interactions (M = Al, Ga) and potential activation of Si-N bonds.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14386
_journal_page_last               14398
_journal_paper_doi               10.1039/c4dt00922c
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C22 H31 N Si'
_chemical_formula_weight         337.57
_chemical_melting_point          411
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0207(2)
_cell_length_b                   13.4721(2)
_cell_length_c                   16.8224(3)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      74.56
_cell_measurement_theta_min      4.20
_cell_volume                     2271.02(7)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Diamond 3.2i (Crystal Impact, 2012)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Photon 100 CMOS-detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'Venture Mo multilayer optic'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16167
_diffrn_reflns_theta_full        74.55
_diffrn_reflns_theta_max         74.55
_diffrn_reflns_theta_min         5.26
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  0.9288
_exptl_absorpt_correction_T_min  0.7380
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.987
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.175
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4542
_refine_ls_number_restraints     318
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0450P)^2^+0.4175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0944
_reflns_number_gt                4135
_reflns_number_total             4542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00922c1.cif
_cod_data_source_block           sad
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7031277--7031283.cif.
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_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7031277