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_4110059
_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         'C36 H64 Hf2 N6, (C5 H12)'
_chemical_formula_sum            'C41 H76 Hf2 N6'
_chemical_formula_weight         1010.06
_chemical_name_common            cmpd_4
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 105.0590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9712(10)
_cell_length_b                   22.8383(17)
_cell_length_c                   14.6871(11)
_cell_measurement_reflns_used    8601
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      29.4
_cell_measurement_theta_min      2.3
_cell_volume                     4525.4(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      366,366,366,726,606,606,606
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0385216
_diffrn_orient_matrix_UB_12      0.0368919
_diffrn_orient_matrix_UB_13      0.0191141
_diffrn_orient_matrix_UB_21      0.0201452
_diffrn_orient_matrix_UB_22      -0.0139882
_diffrn_orient_matrix_UB_23      0.0667859
_diffrn_orient_matrix_UB_31      0.0600329
_diffrn_orient_matrix_UB_32      -0.0189855
_diffrn_orient_matrix_UB_33      -0.0120605
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0106
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            48539
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.29
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.617
_exptl_absorpt_correction_T_max  0.228
_exptl_absorpt_correction_T_min  0.159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       pyramid
_exptl_crystal_F_000             2032
_exptl_crystal_id                'Sita/Hirotsu mh140'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         5200
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.02P)^2^+14.6P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0482
_reflns_number_gt                4736
_reflns_number_total             5200
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0752989si20070716_045130.cif
_cod_data_source_block           cmpd_4
_cod_database_code               4110059