Solid-State 91Zr NMR Spectroscopy Studies of Zirconocene Olefin Polymerization Catalyst Precursors
Aaron J. Rossini; Ivan Hung; Samuel A. Johnson; Carla Slebodnick; Mike Mensch; Paul A. Deck; Robert W. Schurko; Journal of the American Chemical Society 132 (2010) 18301–18317; doi:10.1021/ja107749b

data_4103715
_publ_section_title
;
 Solid-State 91Zr NMR Spectroscopy Studies of Zirconocene Olefin
 Polymerization Catalyst Precursors
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18301
_journal_page_last               18317
_journal_paper_doi               10.1021/ja107749b
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C18 H30 Br2 O2 Si4 Zr'
_chemical_formula_sum            'C18 H30 Br2 O2 Si4 Zr'
_chemical_formula_weight         641.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.9355(13)
_cell_length_b                   14.682(3)
_cell_length_c                   24.174(2)
_cell_measurement_reflns_used    92
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      4.65
_cell_volume                     5300.9(13)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics
'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_publication_material
'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_structure_refinement
'SHELXL-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_structure_solution
'SHELXS-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0548
_diffrn_reflns_av_sigmaI/netI    0.1021
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            3879
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        7.82
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.622
_exptl_absorpt_correction_T_max  0.8107
_exptl_absorpt_correction_T_min  0.3614
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Siemens XSCANS psi-scans'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flat_plate
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.00061(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                1844
_reflns_number_total             3202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107749b_si_004.cif
_cod_data_source_block           strap2
_cod_original_cell_volume        5301.0(12)
_cod_database_code               4103715