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_4072340
_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         'C42 H36 F2 Zr2, 2(C24 B F20), 2(C7 H8)'
_chemical_formula_structural     '[{(IPCF)Zr(\m-F)}2][B(C6F5)4]2.2(C7H8)'
_chemical_formula_sum            'C104 H52 B2 F42 Zr2'
_chemical_formula_weight         2303.52
_chemical_name_common            'Compound 5'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.183(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.045(2)
_cell_length_b                   12.697(2)
_cell_length_c                   26.825(5)
_cell_measurement_reflns_used    746
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      18.94
_cell_measurement_theta_min      4.66
_cell_volume                     4442.1(13)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2004)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2004)'
_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    'SIR-92  (Altomare <i>et al.</i>, 1993)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'fine-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 16.2smx'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.79770
_diffrn_reflns_av_R_equivalents  0.1090
_diffrn_reflns_av_sigmaI/netI    0.1206
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16371
_diffrn_reflns_theta_full        24.82
_diffrn_reflns_theta_max         24.82
_diffrn_reflns_theta_min         4.63
_diffrn_standards_decay_%        5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.9634
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Bruker SADABS; Bruker, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         5381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0488P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                3198
_reflns_number_total             5381
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800783h_si_001.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4072340