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_4110062
_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         'C42 H74 Hf2 N8 Si'
_chemical_formula_sum            'C42 H74 Hf2 N8 Si'
_chemical_formula_weight         1076.16
_chemical_name_common            cmpd_7a
_chemical_name_systematic        ?
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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            16
_cell_length_a                   40.804(2)
_cell_length_b                   45.984(2)
_cell_length_c                   9.8364(5)
_cell_measurement_reflns_used    7130
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      2.5
_cell_volume                     18456.3(15)
_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      606,606,587
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_measurement_specimen_support 'cactus needle'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0143162
_diffrn_orient_matrix_UB_12      -0.0174103
_diffrn_orient_matrix_UB_13      -0.0135823
_diffrn_orient_matrix_UB_21      -0.0183892
_diffrn_orient_matrix_UB_22      0.0129483
_diffrn_orient_matrix_UB_23      -0.0291827
_diffrn_orient_matrix_UB_31      0.0075829
_diffrn_orient_matrix_UB_32      -0.0014677
_diffrn_orient_matrix_UB_33      -0.0964338
_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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            67588
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.51
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.560
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       needle
_exptl_crystal_F_000             8640
_exptl_crystal_id                cmpd_7a
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   0.031(8)
_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     508
_refine_ls_number_reflns         20048
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0367
_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^)+(0.02P)^2^+180.5P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                18208
_reflns_number_total             20048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0752989si20070716_045216.cif
_cod_data_source_block           cmpd_7_a
_cod_original_cell_volume        18456.4(16)
_cod_database_code               4110062