Synthesis and structures of (dialkylsilylene)bis(phosphine)-nickel, palladium, and platinum complexes and (η(6)-arene)(dialkylsilylene)nickel complexes.
Watanabe, Chieko; Inagawa, Yuichiro; Iwamoto, Takeaki; Kira, Mitsuo; Dalton transactions (Cambridge, England : 2003) 39 (2010) 9414–9420; doi:10.1039/c0dt00415d

data_7026433
_publ_section_title
;
 Synthesis and structures of (dialkylsilylene)bis(phosphine)-nickel,
 palladium, and platinum complexes and
 (\h(6)-arene)(dialkylsilylene)nickel complexes.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9414
_journal_page_last               9420
_journal_paper_doi               10.1039/c0dt00415d
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C23 H48 Ni Si5'
_chemical_formula_weight         523.77
_chemical_name_systematic
;
?
;
_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                73.590(4)
_cell_angle_beta                 74.064(4)
_cell_angle_gamma                70.214(4)
_cell_formula_units_Z            2
_cell_length_a                   9.386(3)
_cell_length_b                   10.766(4)
_cell_length_c                   16.176(6)
_cell_measurement_reflns_used    5015
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.35
_cell_volume                     1446.1(9)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 '
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16070
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  0.9165
_exptl_absorpt_correction_T_min  0.7180
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.775
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         6437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0925P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1504
_reflns_number_gt                5112
_reflns_number_total             6437
_reflns_threshold_expression     >2sigma
_cod_data_source_file            c0dt00415d.txt
_cod_data_source_block           (silylene)(toluene)Ni_cw19
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1446.2(9)
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               7026433