Diazene Dehydrogenation Follows H2 Addition to Coordinated Dinitrogen in anansa-Zirconocene Complex
Tamara E. Hanna; Ivan Keresztes; Emil Lobkovsky; Paul J. Chirik; Inorganic Chemistry 46 (2007) 1675–1683; doi:10.1021/ic0620539

data_4307554
_publ_section_title
;
Diazene Dehydrogenation Follows H2 Addition to Coordinated Dinitrogen in
anansa-Zirconocene Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1675
_journal_page_last               1683
_journal_paper_doi               10.1021/ic0620539
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C40 H60 N2 Si2 Zr2'
_chemical_formula_weight         807.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 96.7670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2903(6)
_cell_length_b                   26.3223(15)
_cell_length_c                   13.6173(8)
_cell_measurement_temperature    173(2)
_cell_volume                     4018.7(4)
_computing_cell_refinement       SAINT+
_computing_data_collection       APEX2
_computing_data_reduction        SAINT+
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32633
_diffrn_reflns_theta_full        29.23
_diffrn_reflns_theta_max         29.23
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.9703
_exptl_absorpt_correction_T_min  0.8883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.611
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         10699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.099
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+9.8767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1273
_reflns_number_gt                7952
_reflns_number_total             10699
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0620539si20061026_021515.cif
_cod_data_source_block           th11
_cod_database_code               4307554