Regioselective Synthesis of 1,2- and 1,3-Di(silylamido)cyclopentadienyl Zirconium Complexes
Sudupe, María; Cano, Jesús; Royo, Pascual; Mosquera, Marta E. G.; Frutos, Luis M.; Castaño, Obis; Organometallics 29 (2010) 263–; doi:10.1021/om9009087

data_4067385
_publ_section_title
;
 Regioselective Synthesis of 1,2- and 1,3-Di(silylamido)cyclopentadienyl
 Zirconium Complexes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              263
_journal_paper_doi               10.1021/om9009087
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C18 H36 N2 Si2 Zr1'
_chemical_formula_sum            'C18 H36 N2 Si2 Zr'
_chemical_formula_weight         427.89
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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
_cell_angle_beta                 108.379(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9417(11)
_cell_length_b                   13.1856(15)
_cell_length_c                   16.3703(6)
_cell_measurement_reflns_used    133
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.171
_cell_measurement_theta_min      3.134
_cell_volume                     2241.3(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17955
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.525
_exptl_crystal_size_mid          0.495
_exptl_crystal_size_min          0.393
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         5144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+1.7204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0791
_reflns_number_gt                4004
_reflns_number_total             5144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9009087_si_001.cif
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4067385