Di-tert-butylbiphenylphosphinimide Titanium and Zirconium Complexes: Pendant Arene−Metal Interactions
Ghesner, Ioan; Fenwick, Andrew; Stephan, Douglas W.; Organometallics 25 (2006) 4985–; doi:10.1021/om060569u

data_4074351
_publ_section_title
;
 Di-tert-butylbiphenylphosphinimide Titanium and Zirconium
 Complexes:&#x00A0; Pendant Arene&#x2212;Metal Interactions
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4985
_journal_paper_doi               10.1021/om060569u
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C32 H54 N4 P Zr'
_chemical_formula_weight         616.98
_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                89.866(10)
_cell_angle_beta                 89.743(9)
_cell_angle_gamma                84.667(10)
_cell_formula_units_Z            4
_cell_length_a                   11.705(11)
_cell_length_b                   16.532(15)
_cell_length_c                   18.632(17)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3590(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34371
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.835831
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         12543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0865P)^2^+1.5409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1502
_reflns_number_gt                9055
_reflns_number_total             12543
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060569usi20060818_090738.cif
_cod_data_source_block           t-Bu2(2-C6H4Ph)PNZr(NEt2)3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074351