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_4103713
_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         'C11 H13 Cl Zr'
_chemical_formula_sum            'C11 H13 Cl Zr'
_chemical_formula_weight         271.88
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2009-05-13T04:18:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.3670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7624(6)
_cell_length_b                   11.7215(10)
_cell_length_c                   13.6347(11)
_cell_measurement_reflns_used    8199
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.29
_cell_volume                     1079.84(16)
_computing_cell_refinement       'Bruker SMART'
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11766
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    1.216
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, BRUKER 2001'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+0.7525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0536
_reflns_number_gt                2234
_reflns_number_total             2447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107749b_si_002.cif
_cod_data_source_block           sjmecls
_cod_database_code               4103713