Facile Syntheses of Silylene Nickel Carbonyl Complexes from Lewis Base Stabilized Chlorosilylenes
Gašper Tavčar; Sakya S. Sen; Ramachandran Azhakar; Andrea Thorn; Herbert W. Roesky; Inorganic Chemistry 49 (2010) 10199–10202; doi:10.1021/ic101556s

data_4316987
_publ_contact_author_address
;
'Department of Structural Chemistry, Tammannstrasse 4, 37077 Goettingen'
;
_publ_contact_author_email       andrea.thorn@web.de
_publ_contact_author_fax         '+49 551 3922582'
_publ_contact_author_name        'Andrea Thorn'
_publ_contact_author_phone       '+49 551 393059'
_publ_section_title
;
 Facile Syntheses of Silylene Nickel Carbonyl Complexes from Lewis Base
 Stabilized Chlorosilylenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10199
_journal_page_last               10202
_journal_paper_doi               10.1021/ic101556s
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C36 H72 Cl4 N4 Ni O2 Si2, C7 H8'
_chemical_formula_sum            'C63 H80 Cl4 N4 Ni O2 Si2'
_chemical_formula_weight         1182.00
_chemical_melting_point          170
_chemical_name_common
'dipp carbene silylene nickel carbony complex'
_chemical_name_systematic
; 
could not be determined
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2010-07-21 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.46(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.072(3)
_cell_length_b                   17.701(4)
_cell_length_c                   24.500(5)
_cell_measurement_reflns_used    1186790
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.761
_cell_measurement_theta_min      2.944
_cell_volume                     6507(2)
_computing_cell_refinement       'Bruker AXS SAINT (v 7.33A, Bruker 2006)'
_computing_data_collection       'Proteum2 (v 2.2-RC7, Bruker 2006)'
_computing_data_reduction        'Bruker AXS SAINT (v 7.33A, Bruker 2006)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (v 6.12)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.602
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Three circle diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC multilayer optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            101205
_diffrn_reflns_theta_full        65.10
_diffrn_reflns_theta_max         65.10
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_type              'Bruker SMART 6000'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.624
_exptl_absorpt_correction_T_max  0.9023
_exptl_absorpt_correction_T_min  0.6943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.061
_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     958
_refine_ls_number_reflns         11010
_refine_ls_number_restraints     1623
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0668P)^2^+3.4517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                9292
_reflns_number_total             11010
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101556s_si_002.cif
_cod_data_source_block           atx036
_cod_database_code               4316987