New Side-On Bound Dinitrogen Complexes of Zirconium Supported by an Arene-Bridged Diamidophosphine Ligand and Their Reactivity with Dihydrogen
Erin A. MacLachlan; Fiona M. Hess; Brian O. Patrick; Michael D. Fryzuk; Journal of the American Chemical Society 129 (2007) 10895–10905; doi:10.1021/ja073753v

data_4109870
_publ_section_title
;
 New Side-On Bound Dinitrogen Complexes of Zirconium Supported by an
 Arene-Bridged Diamidophosphine Ligand and Their Reactivity with
 Dihydrogen
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10895
_journal_page_last               10905
_journal_paper_doi               10.1021/ja073753v
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C42 H49 N2 P Si Zr'
_chemical_formula_sum            'C42 H49 N2 P Si Zr'
_chemical_formula_weight         732.11
_chemical_name_common            '[NPN]*ZrTMS'
_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                86.9080(10)
_cell_angle_beta                 78.1770(10)
_cell_angle_gamma                76.0500(10)
_cell_formula_units_Z            2
_cell_length_a                   9.22160(10)
_cell_length_b                   11.5343(2)
_cell_length_c                   19.5329(3)
_cell_measurement_reflns_used    9617
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.966
_cell_measurement_theta_min      2.591
_cell_volume                     1973.54(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43622
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.379
_exptl_absorpt_correction_T_max  0.9701
_exptl_absorpt_correction_T_min  0.8609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       plate
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         9436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.0526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0973
_reflns_number_gt                7340
_reflns_number_total             9436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja073753vsi20070524_051807.cif
_cod_data_source_block           mf643_0m
_cod_database_code               4109870