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_4067383
_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         'C25 H50 Li2 N2 O2 Si2'
_chemical_formula_sum            'C25 H50 Li2 N2 O2 Si2'
_chemical_formula_weight         480.73
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.394(2)
_cell_length_b                   14.923(4)
_cell_length_c                   19.5851(9)
_cell_measurement_reflns_used    90
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      19.514
_cell_measurement_theta_min      3.192
_cell_volume                     3037.8(10)
_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  0.0813
_diffrn_reflns_av_sigmaI/netI    0.0641
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26264
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.957
_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    1.051
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.27(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         6972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0527P)^2^+0.6474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1484
_reflns_number_gt                5177
_reflns_number_total             6972
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9009087_si_001.cif
_cod_data_source_block           3
_cod_original_cell_volume        3037.9(10)
_cod_database_code               4067383