1,3-Double Siloxo-Bridged Zirconium Metallocene for Propene and 1-Hexene Regioselective Oligomerization
Londaitsbehere, Addis; Cuenca, Tomás; Mosquera, Marta E.G.; Cano, Jesús; Milione, Stefano; Grassi, Alfonso; Organometallics 31 (2012) 2108–; doi:10.1021/om2011535

data_4076390
_publ_section_title
;
 1,3-Double Siloxo-Bridged Zirconium Metallocene for Propene and 1-Hexene
 Regioselective Oligomerization
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              2108
_journal_paper_doi               10.1021/om2011535
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C18 H30 Cl2 O2 Si4 Zr.C1.5 H3 O0.5'
_chemical_formula_sum            'C19.5 H33 Cl2 O2.5 Si4 Zr'
_chemical_formula_weight         581.94
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.416(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.400(3)
_cell_length_b                   15.493(2)
_cell_length_c                   14.738(2)
_cell_measurement_reflns_used    78
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      19.827
_cell_measurement_theta_min      3.044
_cell_volume                     2867.5(9)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1179
_diffrn_reflns_av_sigmaI/netI    0.1175
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23936
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.54
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  1.369
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.272
_exptl_crystal_size_min          0.154
_platon_squeeze_details
;
 A molecule of acetone crystallize with every two molecules of this compound but 
 presented severe disorder and it was not possible to get a chemical sensible
 model for it, so Squeeze procedure was used to remove their contribution
 to the structure factors.
;
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         6570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1293
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0759P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1613
_reflns_number_gt                3659
_reflns_number_total             6570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2011535_si_002.cif
_cod_data_source_block           2.0.5C3H6O
_cod_original_cell_volume        2867.5(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C19.50 H33 Cl2 O2.50 Si4 Zr'
_cod_database_code               4076390