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_4329871
_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, 3(C4 H8 O)'
_chemical_formula_sum            'C43 H54 Ni6 O3'
_chemical_formula_weight         971.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           186
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      186
_symmetry_space_group_name_Hall  'P 6c -2c'
_symmetry_space_group_name_H-M   'P 63 m c'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   15.637(4)
_cell_length_b                   15.637(4)
_cell_length_c                   9.351(3)
_cell_measurement_reflns_used    3358
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      35
_cell_measurement_theta_min      2
_cell_volume                     1980.1(10)
_computing_cell_refinement
;
CrysAlis CCD. Version 1.171.33 (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis CCD. Version 1.171.33 (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis CCD. Version 1.171.33 (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
' DIAMOND. Version 3.1f. (Brandenburg, K.  2007)'
_computing_publication_material  'SHELXTL. Version 6.14 (Bruker, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1150
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17515
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.61
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    2.833
_exptl_absorpt_correction_T_max  0.8713
_exptl_absorpt_correction_T_min  0.3621
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2003)'
_exptl_crystal_colour            reddish
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       needle
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1520
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0682
_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^)+(0.0990P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1804
_reflns_number_gt                864
_reflns_number_total             1520
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3008409_si_002_2.cif
_cod_data_source_block           CCDC867930
_cod_database_code               4329871