Highly Electrophilic Half-Sandwich Group 4 Metallacarborane Alkyls. C−H/C−O Activation and Alkyne Insertion Reactions at Neutral Metal Complexes
Cheung, Mak-Shuen; Chan, Hoi-Shan; Xie, Zuowei; Organometallics 24 (2005) 5217–; doi:10.1021/om050658r

data_4076149
_publ_section_title
;
 Highly Electrophilic Half-Sandwich Group 4 Metallacarborane Alkyls.
 C&#x2212;H/C&#x2212;O Activation and Alkyne Insertion Reactions at
 Neutral Metal Complexes
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5217
_journal_paper_doi               10.1021/om050658r
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C14 H38 B9 Hf N O Si'
_chemical_formula_weight         540.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 96.0340(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.5013(15)
_cell_length_b                   10.6833(6)
_cell_length_c                   18.5513(10)
_cell_measurement_temperature    293(2)
_cell_volume                     5420.3(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14718
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    3.897
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6878
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.635
_refine_diff_density_min         -1.300
_refine_diff_density_rms         0.283
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.215
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+21.4644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1733
_reflns_number_gt                3696
_reflns_number_total             4770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050658rsi20050730_045551.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4076149