The first structurally characterised σ-bonded organonickel(i) compound. Crystal structures of [Ni{C(SiMe3)2(SiMe2C5H4N-2)}(PPh3)], [Ni{C(SiMe3)(SiMe2C5H4N-2)(SiMe2O)}]2 and [Pd(μ-Cl){C(SiMe3)2(SiMe2C5H4N-2)}]2
Eaborn, Colin; Hill, Michael S.; Hitchcock, Peter B.; Smith, J. David; Chemical Communications  (2000) 691–; doi:10.1039/b000374n

data_7115154
_publ_section_title
;
 The first structurally characterised \s-bonded organonickel(i) compound.
 Crystal structures of [Ni{C(SiMe3)2(SiMe2C5H4N-2)}(PPh3)],
 [Ni{C(SiMe3)(SiMe2C5H4N-2)(SiMe2O)}]2 and
 [Pd(\m-Cl){C(SiMe3)2(SiMe2C5H4N-2)}]2
;
_journal_issue                   8
_journal_name_full               'Chemical Communications'
_journal_page_first              691
_journal_paper_doi               10.1039/b000374n
_journal_year                    2000
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C26 H50 N2 Ni2 O2 Si6'
_chemical_formula_structural     'C26 H50 N2 Ni2 O2 Si6'
_chemical_formula_sum            'C26 H50 N2 Ni2 O2 Si6'
_chemical_formula_weight         708.64
_chemical_name_common            '[{Ni{C(SiMe3)(SiMe2O)(SiMe2C5H4N)}}2]'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             1999-10-04T16:20:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                91.437(6)
_cell_angle_beta                 111.283(7)
_cell_angle_gamma                92.595(5)
_cell_formula_units_Z            1
_cell_length_a                   8.8600(8)
_cell_length_b                   10.1220(10)
_cell_length_c                   10.6164(11)
_cell_measurement_reflns_used    15870
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      4.246
_cell_measurement_wavelength     0.71073
_cell_volume                     885.36(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.97
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.071
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8262
_diffrn_reflns_theta_full        25.17
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         4.37
_exptl_absorpt_coefficient_mu    1.291
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.079
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+6.3900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1599
_reflns_number_gt                2618
_reflns_number_total             3091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b000374n.txt
_cod_data_source_block           oct199
_cod_original_cell_volume        885.36(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7115154