Structural Characterization of a Cationic Zirconocene Dimethylaniline Complex and Related Catalytically Relevant Species
Wilson, Polly A.; Wright, Joseph A.; Oganesyan, Vasily S.; Lancaster, Simon J.; Bochmann, Manfred; Organometallics 27 (2008) 6371–; doi:10.1021/om800783h

data_4072339
_publ_section_title
;
 Structural Characterization of a Cationic Zirconocene Dimethylaniline
 Complex and Related Catalytically Relevant Species
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6371
_journal_paper_doi               10.1021/om800783h
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C30 H32 N Zr, C24 B F20, 2(C7 H8)'
_chemical_formula_structural     '[(IPCF)ZrMe(NMe2Ph)][B(C6F5)4].2(C7H8)'
_chemical_formula_sum            'C68 H48 B F20 N Zr'
_chemical_formula_weight         1361.10
_chemical_name_common            'Compound 2'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                113.805(5)
_cell_angle_beta                 91.394(5)
_cell_angle_gamma                110.625(5)
_cell_formula_units_Z            2
_cell_length_a                   13.368(5)
_cell_length_b                   14.468(5)
_cell_length_c                   17.283(5)
_cell_measurement_reflns_used    12173
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2807.6(17)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
 SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999)
 and enCIFer (Allen <i>et al.</i>, 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1993)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_sigmaI/netI    0.1014
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45780
_diffrn_reflns_theta_full        27.67
_diffrn_reflns_theta_max         27.67
_diffrn_reflns_theta_min         3.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  0.9877
_exptl_absorpt_correction_T_min  0.7487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS 2007/2; Sheldrick, 2007)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.265
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         12835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.1569
_refine_ls_R_factor_gt           0.0883
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+12.1109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1697
_reflns_number_gt                8090
_reflns_number_total             12835
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800783h_si_001.cif
_cod_data_source_block           2
_cod_original_cell_volume        2807.6(16)
_cod_database_code               4072339