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_4110058
_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_absolute_configuration ad
_chemical_formula_moiety         'C36 H66 Hf2 N8'
_chemical_formula_sum            'C36 H66 Hf2 N8'
_chemical_formula_weight         967.95
_chemical_name_common            cmpd_3
_chemical_name_systematic        ?
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_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                   17.0487(10)
_cell_length_b                   18.9416(11)
_cell_length_c                   25.4574(16)
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_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      28.6
_cell_measurement_theta_min      2.3
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_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
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_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      606,606,606
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'glass capillary'
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_diffrn_orient_matrix_UB_13      -0.0029945
_diffrn_orient_matrix_UB_21      -0.0042490
_diffrn_orient_matrix_UB_22      0.0029723
_diffrn_orient_matrix_UB_23      0.0391200
_diffrn_orient_matrix_UB_31      0.0048191
_diffrn_orient_matrix_UB_32      0.0525518
_diffrn_orient_matrix_UB_33      -0.0019745
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
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_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.081
_exptl_absorpt_correction_T_max  0.517
_exptl_absorpt_correction_T_min  0.357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             3856
_exptl_crystal_id                cmpd_3
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.718
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   0.506(8)
_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     1119
_refine_ls_number_reflns         18343
_refine_ls_number_restraints     458
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0253
_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^)+(0.025P)^2^+8.35P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0586
_reflns_Friedel_coverage         0.906
_reflns_number_gt                16477
_reflns_number_total             18343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0752989si20070716_045118.cif
_cod_data_source_block           cmpd_3
_cod_original_cell_volume        8221.0(9)
_cod_database_code               4110058