μ-[Bis(3,3-dimethylbut-1-ynyl)diphenylsilane]bis[(cycloocta-1,5-diene)nickel(II)](<i>Ni{—</i>Ni})
Imhof, Wolfgang; Klettke, Thomas; Walther, Dirk; Acta Crystallographica Section E 63 (2007) m2567–m2567; doi:10.1107/S1600536807045825

data_2215407
_publ_section_title
\m-[Bis(3,3-dimethylbut-1-ynyl)diphenylsilane]bis[(cycloocta-1,5-diene)nickel(II)](<i>Ni{---</i>Ni})
_journal_coeditor_code           CF2141
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2567
_journal_page_last               m2567
_journal_paper_doi               10.1107/S1600536807045825
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ni2 (C24 H28 Si) (C8 H12)2]'
_chemical_formula_moiety         'C40 H52 Ni2 Si'
_chemical_formula_sum            'C40 H52 Ni2 Si'
_chemical_formula_weight         678.31
_chemical_name_systematic
;
\m-[Bis(3,3-dimethylbut-1-ynyl)diphenylsilane]bis[(cycloocta-1,5-
diene)nickel(II)](<i>Ni---Ni</i>)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.167(2)
_cell_length_b                   9.617(2)
_cell_length_c                   18.110(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      13.4
_cell_volume                     1764.8(6)
_computing_cell_refinement       'SET4 (de Boer & Duisenberg, 1984)'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'MoLEN (Fair, 1990)'
_computing_molecular_graphics    'XP (Siemens, 1990)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4489
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        0.13
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.134
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.318
_refine_ls_abs_structure_details 'Flack (1983), with 4 Friedel pairs'
_refine_ls_abs_structure_Flack   0.006(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         4246
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0315P)^2^+0.65P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                3931
_reflns_number_total             4246
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf2141.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2215407
_cod_database_fobs_code          2215407