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_4107748
_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         'C25 H34 Zr'
_chemical_formula_sum            'C25 H34 Zr'
_chemical_formula_weight         425.74
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   12.4012(3)
_cell_length_b                   16.6358(6)
_cell_length_c                   10.2988(3)
_cell_measurement_reflns_used    2785
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.39
_cell_measurement_theta_min      2.33
_cell_volume                     2124.68(11)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14465
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.9257
_exptl_absorpt_correction_T_min  0.8180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         3320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.6623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                2576
_reflns_number_total             3320
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801021w-file003.cif
_cod_data_source_block           dp10
_cod_database_code               4107748