Octa- and Nonamethylfluorenyl Complexes of Zirconium(IV): Reactive Hydride Derivatives and Reversible Hydrogen Migration between the Metal and the Fluorenyl Ligand
Bazinet, Patrick; Tilley, T. Don; Organometallics 28 (2009) 2285–; doi:10.1021/om900047x

data_4069136
_publ_section_title
;
 Octa- and Nonamethylfluorenyl Complexes of Zirconium(IV): Reactive
 Hydride Derivatives and Reversible Hydrogen Migration between the Metal
 and the Fluorenyl Ligand
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2285
_journal_paper_doi               10.1021/om900047x
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C33 H50 Si2 Zr'
_chemical_formula_sum            'C33 H50 Si2 Zr'
_chemical_formula_weight         594.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.454(3)
_cell_angle_beta                 92.927(3)
_cell_angle_gamma                104.927(3)
_cell_formula_units_Z            2
_cell_length_a                   9.926(2)
_cell_length_b                   9.966(2)
_cell_length_c                   16.895(4)
_cell_measurement_reflns_used    2584
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      24.296
_cell_measurement_theta_min      3.393
_cell_volume                     1599.1(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  POV-Ray
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8121
_diffrn_reflns_theta_full        24.70
_diffrn_reflns_theta_max         24.70
_diffrn_reflns_theta_min         3.39
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sababs, 2004'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0678P)^2^+0.4265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                4130
_reflns_number_total             5239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900047x_si_002.cif
_cod_data_source_block           pat2
_cod_database_code               4069136