Cationic Alkylaluminum-Complexed Zirconocene Hydrides: NMR-Spectroscopic Identification, Crystallographic Structure Determination, and Interconversion with Other Zirconocene Cations
Steven M. Baldwin; John E. Bercaw; Lawrence M. Henling; Michael W. Day; Hans H. Brintzinger; Journal of the American Chemical Society 133 (2011) 1805–1813; doi:10.1021/ja1050428

data_4105613
_publ_section_title
;
 Cationic Alkylaluminum-Complexed Zirconocene Hydrides: NMR-Spectroscopic
 Identification, Crystallographic Structure Determination, and
 Interconversion with Other Zirconocene Cations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1805
_journal_page_last               1813
_journal_paper_doi               10.1021/ja1050428
_journal_volume                  133
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H57 Al2 Si Zr, C24 B F20, 0.5(C7 H8)'
_chemical_formula_sum            'C63.5 H61 Al2 B F20 Si Zr'
_chemical_formula_weight         1388.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   17.3916(7)
_cell_length_b                   26.6355(12)
_cell_length_c                   27.3497(12)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.95
_cell_measurement_theta_min      2.36
_cell_volume                     12669.3(9)
_computing_cell_refinement       'Bruker SAINT-Plus v7.66A'
_computing_data_collection       'Bruker APEX2 v2009.7-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.66A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 6 settings'
_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  0.0698
_diffrn_reflns_av_sigmaI/netI    0.1015
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            115139
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  0.9719
_exptl_absorpt_correction_T_min  0.9189
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       Block
_exptl_crystal_F_000             5656
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.804
_refine_ls_hydrogen_treatment    'Riding (except hydrides)'
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     1456
_refine_ls_number_reflns         23731
_refine_ls_number_restraints     8713
_refine_ls_restrained_S_all      1.608
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0779
_reflns_number_gt                13557
_reflns_number_total             23731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1050428_si_003.cif
_cod_data_source_block           smb10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_formula_sum        'C63.50 H61 Al2 B F20 Si Zr'
_cod_database_code               4105613