Triple C-H Bond Activation of a Nickel-Bound Methyl Group: Synthesis and X-Ray Structure of a Carbide Cluster (NiCp)6(μ6-C)
Włodzimierz Buchowicz; Beata Herbaczyńska; Lucjan B. Jerzykiewicz; Tadeusz Lis; Stanisław Pasynkiewicz; Antoni Pietrzykowski; Inorganic Chemistry 51 (2012) 8292–8297; doi:10.1021/ic3008409

data_4329870
_publ_contact_author_address
;
Faculty of Chemistry
Warsaw University of Technology
Noakowskiego 3, 00-664 Warsaw, Poland
;
_publ_contact_author_email       anpietr@ch.pw.edu.pl
_publ_contact_author_fax         '+48 22 234 5462'
_publ_contact_author_name        'Antoni Pietrzykowski'
_publ_contact_author_phone       '+48 22 234 7116'
_publ_section_title
;
 Triple C-H Bond Activation of a Nickel-Bound Methyl Group: Synthesis and
 X-Ray Structure of a Carbide Cluster (NiCp)6(\m6-C)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8292
_journal_page_last               8297
_journal_paper_doi               10.1021/ic3008409
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C31 H30 Ni6, 2(C H2 Cl2)'
_chemical_formula_sum            'C33 H34 Cl4 Ni6'
_chemical_formula_weight         924.66
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 98.50(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.814(3)
_cell_length_b                   9.298(3)
_cell_length_c                   17.857(4)
_cell_measurement_reflns_used    19378
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37
_cell_measurement_theta_min      4
_cell_volume                     1611.6(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'KUMA KM4 \k-geometry diffractometer with Saphire CCD camera'
_diffrn_measurement_method       \w
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            40283
_diffrn_reflns_theta_full        37.50
_diffrn_reflns_theta_max         37.50
_diffrn_reflns_theta_min         4.53
_exptl_absorpt_coefficient_mu    3.789
_exptl_absorpt_correction_T_max  0.552
_exptl_absorpt_correction_T_min  0.332
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2003)'
_exptl_crystal_colour            reddish
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_description       column
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.71
_refine_diff_density_min         -1.21
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         8462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.084P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1513
_reflns_number_gt                5596
_reflns_number_total             8462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3008409_si_002_1.cif
_cod_data_source_block           CCDC867932
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4329870