Reversible Addition of the Si–H Bond of Phenylsilane to the Sc–N Bond of a Scandium Terminal Imido Complex
Chu, Jiaxiang; Lu, Erli; Chen, Yaofeng; Leng, Xuebing; Organometallics 32 (2013) 1137–1140; doi:10.1021/om3010349

data_4080115
_publ_section_title
;
 Reversible Addition of the Si--H Bond of Phenylsilane to the Sc--N Bond
 of a Scandium Terminal Imido Complex
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1137
_journal_page_last               1140
_journal_paper_doi               10.1021/om3010349
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C58 H83 N6 Sc Si'
_chemical_formula_weight         937.35
_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                84.042(3)
_cell_angle_beta                 74.078(3)
_cell_angle_gamma                82.847(3)
_cell_formula_units_Z            2
_cell_length_a                   13.543(2)
_cell_length_b                   14.400(2)
_cell_length_c                   14.572(2)
_cell_measurement_reflns_used    3537
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.23
_cell_volume                     2704.3(7)
_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      140(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21366
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_T_max  0.9649
_exptl_absorpt_correction_T_min  0.9517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         12284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1578
_reflns_number_gt                8078
_reflns_number_total             12284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3010349_si_002.cif
_cod_data_source_block           mo_dm12564_0m
_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 1891 2012-01-12 08:04:46Z andrius 

 Adding the _journal_page_last data item.
;
_cod_original_cell_volume        2704.5(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4080115