Extreme N\τbN Bond Elongation and Facile N-Atom Functionalization Reactions within Two Structurally Versatile New Families of Group 4 Bimetallic "Side-on-Bridged" Dinitrogen Complexes for Zirconium and Hafnium
Masakazu Hirotsu; Philip P. Fontaine; Peter Y. Zavalij; Lawrence R. Sita; Journal of the American Chemical Society 129 (2007) 12690–12692; doi:10.1021/ja0752989

data_4110060
_publ_section_title
;
 Extreme N\\tbN Bond Elongation and Facile N-Atom Functionalization
 Reactions within Two Structurally Versatile New Families of Group 4
 Bimetallic "Side-on-Bridged" Dinitrogen Complexes for Zirconium and
 Hafnium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12690
_journal_page_last               12692
_journal_paper_doi               10.1021/ja0752989
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C34 H60 Hf2 N6'
_chemical_formula_sum            'C34 H60 Hf2 N6'
_chemical_formula_weight         909.86
_chemical_name_common            cmpd_5
_chemical_name_systematic        ?
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.0967(7)
_cell_length_b                   16.0300(8)
_cell_length_c                   31.8146(15)
_cell_measurement_reflns_used    8608
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      29.0
_cell_measurement_theta_min      2.3
_cell_volume                     7699.1(6)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XSHEL (Bruker, 1999)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker Smart1000'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      366,606,606,1206
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'cactus needle'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0215411
_diffrn_orient_matrix_UB_12      -0.0222718
_diffrn_orient_matrix_UB_13      -0.0275237
_diffrn_orient_matrix_UB_21      -0.0494219
_diffrn_orient_matrix_UB_22      -0.0415197
_diffrn_orient_matrix_UB_23      -0.0001750
_diffrn_orient_matrix_UB_31      -0.0384817
_diffrn_orient_matrix_UB_32      0.0408839
_diffrn_orient_matrix_UB_33      -0.0151768
_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  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            70111
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.54
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.418
_exptl_absorpt_correction_T_max  0.805
_exptl_absorpt_correction_T_min  0.213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             3600
_exptl_crystal_id                cmpd_5
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         8849
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.019P)^2^+17.29P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0547
_reflns_number_gt                7364
_reflns_number_total             8849
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0752989si20070716_045144.cif
_cod_data_source_block           cmpd_5
_cod_database_code               4110060