A Dihydrodisilene Transition Metal Complex from an N-Heterocyclic Carbene-Stabilized Silylene Monohydride
Shigeyoshi Inoue; Carsten Eisenhut; Journal of the American Chemical Society 135 (2013) 18315–18318; doi:10.1021/ja410528y

data_4121297
_publ_contact_author_address
;
Institut f\"ur Chemie, Technische Universit\"at Berlin, 
Stra\&se des 17. Juni 135, Sekr. C2, D-10623 Berlin
;
_publ_contact_author_email       shigeyoshi.inoue@tu-berlin.de
_publ_contact_author_fax         49-30-314-29732
_publ_contact_author_name        'Shigeyoshi Inoue'
_publ_contact_author_phone       49-30-314-29734
_publ_section_title
;
 A Dihydrodisilene Transition Metal Complex from an N-Heterocyclic
 Carbene-Stabilized Silylene Monohydride
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18315
_journal_page_last               18318
_journal_paper_doi               10.1021/ja410528y
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C38 H80 N4 Ni Si4'
_chemical_formula_weight         764.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.5259(3)
_cell_length_b                   23.4672(7)
_cell_length_c                   31.3977(9)
_cell_measurement_reflns_used    6349
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.6722
_cell_measurement_theta_min      3.1204
_cell_volume                     9229.3(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S Sapphire'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            35403
_diffrn_reflns_theta_full        67.49
_diffrn_reflns_theta_max         67.49
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    1.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_description       rod
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         8301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0432P)^2^+2.2739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                7139
_reflns_number_total             8301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja410528y_si_001_2.cif
_cod_data_source_block           c:\compound3
_cod_database_code               4121297