Dinitrogen Silylation and Cleavage with a Hafnocene Complex
Scott P. Semproni; Emil Lobkovsky; Paul J. Chirik; Journal of the American Chemical Society 133 (2011) 10406–10409; doi:10.1021/ja2042595

data_4106388
_publ_section_title
;
 Dinitrogen Silylation and Cleavage with a Hafnocene Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10406
_journal_page_last               10409
_journal_paper_doi               10.1021/ja2042595
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C32 H44 Hf2 N2, C6 H5 F'
_chemical_formula_sum            'C38 H49 F Hf2 N2'
_chemical_formula_weight         909.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4976(9)
_cell_length_b                   14.9955(11)
_cell_length_c                   17.1276(12)
_cell_measurement_reflns_used    7808
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.09
_cell_measurement_theta_min      2.72
_cell_volume                     3466.7(4)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16896
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.018
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.2654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.298
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         4258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0199
_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^)+(0.0190P)^2^+4.8299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0467
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                3486
_reflns_number_total             4258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2042595_si_001_1.cif
_cod_data_source_block           sps2
_cod_database_code               4106388