Formation of Zirconocenes Containing Vinyl-imine and Keteniminate Species from Zirconacycles and Diphenylacetonitrile
Zhao, Jing; Zhang, Shaoguang; Zhang, Wen-Xiong; Xi, Zhenfeng; Organometallics 30 (2011) 3464–; doi:10.1021/om200404p

data_4064905
_publ_section_title
;
 Formation of Zirconocenes Containing Vinyl-imine and Keteniminate Species
 from Zirconacycles and Diphenylacetonitrile
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3464
_journal_paper_doi               10.1021/om200404p
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C44 H44 N2 Si Zr'
_chemical_formula_sum            'C44 H44 N2 Si Zr'
_chemical_formula_weight         720.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 122.930(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.560(4)
_cell_length_b                   18.179(5)
_cell_length_c                   17.708(5)
_cell_measurement_reflns_used    10472
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      1.12
_cell_volume                     3663.8(18)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0758
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15959
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.9173
_exptl_absorpt_correction_T_min  0.8382
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         7438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+5.5398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1511
_reflns_number_gt                6475
_reflns_number_total             7438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200404p_si_002.cif
_cod_data_source_block           3b
_cod_original_cell_volume        3663.8(17)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4064905