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_4072342
_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         'C45 H45 Zr2, C19 H3 B F15'
_chemical_formula_structural     '[{(IPCF)ZrMe}2(\m-Me)][MeB(C6F5)3]'
_chemical_formula_sum            'C64 H48 B F15 Zr2'
_chemical_formula_weight         1295.27
_chemical_name_common            'Compound 7'
_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                 98.682(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.885(2)
_cell_length_b                   13.8749(14)
_cell_length_c                   21.482(3)
_cell_measurement_reflns_used    4889
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      25.0000
_cell_measurement_theta_min      3.0854
_cell_volume                     5269.7(11)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_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      140(2)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2074
_diffrn_reflns_av_sigmaI/netI    0.2357
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51667
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         3.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.9973
_exptl_absorpt_correction_T_min  0.7960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2006)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         9335
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.1970
_refine_ls_R_factor_gt           0.0724
_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^)+(0.0279P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                4144
_reflns_number_total             9335
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800783h_si_001.cif
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4072342