Indenyl Zirconium Dinitrogen Chemistry: N2 Coordination to an Isolated Zirconium Sandwich and Synthesis of Side-on, End-on Dinitrogen Compounds
Doris Pun; Emil Lobkovsky; Paul J. Chirik; Journal of the American Chemical Society 130 (2008) 6047–6054; doi:10.1021/ja801021w

data_4107749
_publ_section_title
;
 Indenyl Zirconium Dinitrogen Chemistry: N2 Coordination to an Isolated
 Zirconium Sandwich and Synthesis of Side-on, End-on Dinitrogen Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6047
_journal_page_last               6054
_journal_paper_doi               10.1021/ja801021w
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C46 H60 N2 Zr2'
_chemical_formula_sum            'C46 H60 N2 Zr2'
_chemical_formula_weight         823.40
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5456(6)
_cell_length_b                   17.1401(8)
_cell_length_c                   18.5216(9)
_cell_measurement_reflns_used    5776
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.37
_cell_measurement_theta_min      2.21
_cell_volume                     4300.2(3)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29880
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  0.9797
_exptl_absorpt_correction_T_min  0.8202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       rod
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.453
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         5342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.1893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                4191
_reflns_number_total             5342
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801021w-file004.cif
_cod_data_source_block           dp7
_cod_database_code               4107749