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_4110063
_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 H66 N6 Hf2, (H ), (N2 H)'
_chemical_formula_sum            'C36 H68 Hf2 N8'
_chemical_formula_weight         969.96
_chemical_name_common            cmpd_8a
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.2330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2318(7)
_cell_length_b                   11.8589(7)
_cell_length_c                   31.064(2)
_cell_measurement_reflns_used    8654
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      29.2
_cell_measurement_theta_min      2.2
_cell_volume                     4113.2(4)
_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
_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      0.0535192
_diffrn_orient_matrix_UB_12      0.0077252
_diffrn_orient_matrix_UB_13      0.0277447
_diffrn_orient_matrix_UB_21      -0.0712055
_diffrn_orient_matrix_UB_22      -0.0051708
_diffrn_orient_matrix_UB_23      0.0166305
_diffrn_orient_matrix_UB_31      0.0093282
_diffrn_orient_matrix_UB_32      -0.0838114
_diffrn_orient_matrix_UB_33      0.0015271
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            48579
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.51
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.078
_exptl_absorpt_correction_T_max  0.530
_exptl_absorpt_correction_T_min  0.390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             1936
_exptl_crystal_id                cmpd_8a
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         9445
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0194
_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^)+(0.011P)^2^+5.96P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0407
_refine_ls_wR_factor_ref         0.0423
_reflns_number_gt                8435
_reflns_number_total             9445
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0752989si20070716_045231.cif
_cod_data_source_block           cmpd_8a
_cod_database_code               4110063