N‒H and N‒C Bond Formation with an N2-Derived Dihafnium μ-Nitrido Complex
Semproni, Scott P.; Chirik, Paul J.; Organometallics 33 (2014) 3727–; doi:10.1021/om500393n

data_4083918
_publ_section_title
;
 N--H and N--C Bond Formation with an N2-Derived Dihafnium \m-Nitrido
 Complex
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3727
_journal_paper_doi               10.1021/om500393n
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C39 H56 Hf2 N2 O2'
_chemical_formula_weight         941.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.5040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6695(7)
_cell_length_b                   35.852(3)
_cell_length_c                   10.5549(8)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.26
_cell_volume                     3618.8(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 (Farraguia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            31266
_diffrn_reflns_theta_full        27.65
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    5.768
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamond
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.049
_refine_diff_density_max         1.091
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         8369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+9.3509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0484
_reflns_number_gt                7394
_reflns_number_total             8369
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500393n_si_002.cif
_cod_data_source_block           sps40
_cod_depositor_comments
'Adding full bibliography for 4083916--4083924.cif.'
_cod_original_cell_volume        3618.9(5)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4083918