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_4109871
_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         'C86 H88 N8 P2 Zr2'
_chemical_formula_sum            'C86 H88 N8 P2 Zr2'
_chemical_formula_weight         1478.10
_chemical_name_common            {[NPN]*Zr(Py)}2(N2)
_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                 91.7900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6395(7)
_cell_length_b                   19.7497(8)
_cell_length_c                   27.0757(12)
_cell_measurement_reflns_used    5350
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.446
_cell_measurement_theta_min      2.419
_cell_volume                     10496.8(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker Apex'
_diffrn_measurement_method       'area detector'
_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  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            35075
_diffrn_reflns_theta_full        22.48
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.9241
_exptl_absorpt_correction_T_min  0.8580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.935
_exptl_crystal_description       prism
_exptl_crystal_F_000             3080
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         13279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1024P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1630
_reflns_number_gt                9468
_reflns_number_total             13279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja073753vsi20070524_051828.cif
_cod_data_source_block           platon
_cod_database_code               4109871