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_7115155
_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         'C100 H116 Cl2 N2 P4 Pd2 Si6'
_chemical_formula_structural     'C100 H116 CL2 N2 P4 PD2 SI6'
_chemical_formula_sum            'C28 H56 Cl2 N2 Pd2 Si6'
_chemical_formula_weight         872.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_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_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             1999-07-28T15:21:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.465(5)
_cell_length_b                   23.390(12)
_cell_length_c                   25.032(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      8.5
_cell_measurement_theta_min      7.5
_cell_measurement_wavelength     0.71073
_cell_volume                     7884(6)
_computing_cell_refinement       'CAD4  (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4  (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_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_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.45622E-1
_diffrn_orient_matrix_UB_12      0.29072E-1
_diffrn_orient_matrix_UB_13      -0.16062E-1
_diffrn_orient_matrix_UB_21      0.24193E-1
_diffrn_orient_matrix_UB_22      0.29147E-1
_diffrn_orient_matrix_UB_23      0.02621
_diffrn_orient_matrix_UB_31      0.53384E-1
_diffrn_orient_matrix_UB_32      0.11624E-1
_diffrn_orient_matrix_UB_33      -0.25523E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1279
_diffrn_reflns_av_sigmaI/netI    0.1508
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            13619
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.22
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        5
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.251
_exptl_absorpt_correction_T_max  0.9754
_exptl_absorpt_correction_T_min  0.7053
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   2
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.369
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6907
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1539
_refine_ls_R_factor_gt           0.0824
_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^)+(0.1108P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.2264
_reflns_number_gt                3750
_reflns_number_total             6907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b000374n.txt
_cod_data_source_block           jul1399
_cod_database_code               7115155
_exptl_absorpt_factor_mur        0.015
_exptl_absorpt_correction_t_ave  0.7807
_diffrn_standards_decay_corr_max 2.742
_diffrn_standards_decay_corr_min 0.921