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_4316986
_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         'C18 H23 Cl N2 Ni O3 Si'
_chemical_formula_sum            'C18 H23 Cl N2 Ni O3 Si'
_chemical_formula_weight         437.61
_chemical_melting_point          170
_chemical_name_common            'amidinate 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
;
2010-07-22 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.24(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.942(3)
_cell_length_b                   11.524(2)
_cell_length_c                   13.737(3)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.104
_cell_measurement_theta_min      3.399
_cell_volume                     2057.2(8)
_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 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Three circle diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36195
_diffrn_reflns_theta_full        65.12
_diffrn_reflns_theta_max         65.12
_diffrn_reflns_theta_min         3.40
_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    3.278
_exptl_absorpt_correction_T_max  0.9680
_exptl_absorpt_correction_T_min  0.4396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3491
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0328P)^2^+1.6002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                3409
_reflns_number_total             3491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101556s_si_001.cif
_cod_data_source_block           atx040
_cod_original_cell_volume        2057.2(7)
_cod_original_formula_sum        'C18 H23 Cl N2 Ni O3 Si '
_cod_database_code               4316986