Synthesis and Reactivity of New Niobocene Hydride-Stibine and Hydride-Stilbene Complexes. X-ray Crystal Structure of [Nb(η5-C5H4SiMe3)2(H)(trans-η2-C,C-PhCH═CHPh)]
Antiñolo, Antonio; Pérez-Flores, Juan-Carlos; Hervás, Maria Jesús; García-Yuste, Santiago; López-Solera, Maria Isabel; Otero, Antonio; Fernández-Pacheco, Ana Rodríguez; Tercero-Morales, Maria Teresa; Organometallics 32 (2013) 862–; doi:10.1021/om301171j

data_4080009
_publ_section_title
;
 Synthesis and Reactivity of New Niobocene Hydride-Stibine and
 Hydride-Stilbene Complexes. X-ray Crystal Structure of
 [Nb(\h5-C5H4SiMe3)2(H)(trans-\h2-C,C-PhCH&#x2550;CHPh)]
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              862
_journal_paper_doi               10.1021/om301171j
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C30 H39 Nb Si2'
_chemical_formula_sum            'C30 H39 Nb Si2'
_chemical_formula_weight         548.70
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 94.087(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6788(9)
_cell_length_b                   10.9654(8)
_cell_length_c                   19.9135(15)
_cell_measurement_reflns_used    2930
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.864
_cell_measurement_theta_min      2.516
_cell_volume                     2761.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0803
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33336
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.9481
_exptl_absorpt_correction_T_min  0.8861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         6872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0610P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                5004
_reflns_number_total             6872
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301171j_si_001.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4080009