Synthesis of a Zirconium Sandwich Complex and Crystallographic Characterization of Its Adduct with Tetrahydrofuran
Christopher A. Bradley; Emil Lobkovsky; Paul J. Chirik; Journal of the American Chemical Society 125 (2003) 8110–8111; doi:10.1021/ja035594v

data_4113884
_publ_section_title
;
 Synthesis of a Zirconium Sandwich Complex and Crystallographic
 Characterization of Its Adduct with Tetrahydrofuran
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8110
_journal_page_last               8111
_journal_paper_doi               10.1021/ja035594v
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C37 H58 O2 Si4 Zr'
_chemical_formula_weight         732.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.191(3)
_cell_angle_beta                 97.918(3)
_cell_angle_gamma                104.530(3)
_cell_formula_units_Z            2
_cell_length_a                   10.3208(15)
_cell_length_b                   11.4540(17)
_cell_length_c                   18.018(3)
_cell_measurement_temperature    173(2)
_cell_volume                     2013.7(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.808
_diffrn_measured_fraction_theta_max 0.808
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26841
_diffrn_reflns_theta_full        32.46
_diffrn_reflns_theta_max         32.46
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  0.9206
_exptl_absorpt_correction_T_min  0.8498
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         11761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.423
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.4881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                9849
_reflns_number_total             11761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja035594vsi20030411_101214.cif
_cod_data_source_block           cb27
_cod_original_formula_sum        'C32 H46 O2 Si4 Zr * (C5 H12) '
_cod_database_code               4113884