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_4113883
_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            'C34 H54 O Si4 Zr'
_chemical_formula_weight         682.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 94.983(6)
_cell_angle_gamma                90.000(6)
_cell_formula_units_Z            4
_cell_length_a                   12.773(3)
_cell_length_b                   16.911(4)
_cell_length_c                   17.389(4)
_cell_measurement_temperature    173(2)
_cell_volume                     3741.9(15)
_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 0.920
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Bruker 1K CCD area detector'
_diffrn_measurement_method       '0.3 deg. 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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43038
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  0.8780
_exptl_absorpt_correction_T_min  0.8080
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_meas      0
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         5.074
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         13136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.690
_refine_ls_shift/su_mean         0.061
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+1.6097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1618
_reflns_number_gt                9155
_reflns_number_total             13136
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja035594vsi20030411_101151.cif
_cod_data_source_block           cb24
_cod_original_cell_volume        3742.1(14)
_cod_database_code               4113883