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_4106391
_publ_section_title
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 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_sum            'C41 H62 Hf2 N2 O1.5 Si'
_chemical_formula_weight         991.99
_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                 92.2600(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   41.290(6)
_cell_length_b                   9.5098(13)
_cell_length_c                   19.378(3)
_cell_measurement_reflns_used    8706
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      2.0
_cell_volume                     7603.0(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_radiation_monochromator  'Triumph curved-crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42027
_diffrn_reflns_theta_full        27.65
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    5.525
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       prism
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.094
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         8706
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0175
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+11.2462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0357
_refine_ls_wR_factor_ref         0.0386
_reflns_number_gt                7113
_reflns_number_total             8706
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja2042595_si_001_4.cif
_cod_data_source_block           sps19
_cod_depositor_comments
;

2021-08-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C82 H124 Hf4 N4 O3 Si2'
_cod_original_formula_weight         1983.99
_cod_original_formula_units_Z            4
_cod_original_cell_volume        7603.0(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4106391