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_4083919
_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 H51 F Hf2 N2 O'
_chemical_formula_weight         939.80
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.290(3)
_cell_angle_beta                 93.368(3)
_cell_angle_gamma                92.903(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1858(12)
_cell_length_b                   12.4686(14)
_cell_length_c                   14.8013(16)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.61
_cell_volume                     1730.9(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 (Farraguia, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacavazzo, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.974
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22373
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    6.032
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       diamond
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.025
_refine_diff_density_max         3.973
_refine_diff_density_min         -3.007
_refine_diff_density_rms         0.344
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7751
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0557P)^2^+6.6866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                6888
_reflns_number_total             7751
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500393n_si_002.cif
_cod_data_source_block           sps74
_cod_depositor_comments
'Adding full bibliography for 4083916--4083924.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4083919