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_4103714
_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         'C14 H20 Br2 O Si2 Zr'
_chemical_formula_sum            'C14 H20 Br2 O Si2 Zr'
_chemical_formula_weight         511.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.587(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5792(5)
_cell_length_b                   8.5955(3)
_cell_length_c                   15.3894(5)
_cell_measurement_reflns_used    6585
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.9669
_cell_measurement_theta_min      4.1012
_cell_volume                     1784.39(11)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction, 2009)'
_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      100(2)
_diffrn_detector                 CCD
_diffrn_detector_type            'Oxford Diffraction Sapphire 3 CCD'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_UB_11      0.0522357000
_diffrn_orient_matrix_UB_12      -0.0089338000
_diffrn_orient_matrix_UB_13      0.0050358000
_diffrn_orient_matrix_UB_21      -0.0027462000
_diffrn_orient_matrix_UB_22      -0.0433414000
_diffrn_orient_matrix_UB_23      0.0388511000
_diffrn_orient_matrix_UB_31      -0.0049888000
_diffrn_orient_matrix_UB_32      -0.0697390000
_diffrn_orient_matrix_UB_33      -0.0248407000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0641
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16281
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         4.18
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    5.222
_exptl_absorpt_correction_T_max  0.583
_exptl_absorpt_correction_T_min  0.293
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro, Oxford Diffraction Ltd., v171.33.66 (release 28-04-2010
 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Numerical absorption
 correction based on Gaussian integration over a multifaceted crystal model.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.165
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         5194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.867
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0221P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0554
_reflns_number_gt                3541
_reflns_number_total             5194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107749b_si_003.cif
_cod_data_source_block           cs905
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1784.40(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4103714