Photolytic Zirconium Benzyl Bond Cleavage and Subsequent Aryl C−F Activation in Zirconium Complexes of Fluorinated Aryl Diamides
O'Connor, Paul E.; Berg, David J.; Barclay, Tosha; Organometallics 21 (2002) 3947–; doi:10.1021/om0204181

data_4077011
_publ_section_title
;
 Photolytic Zirconium Benzyl Bond Cleavage and Subsequent Aryl C&#x2212;F
 Activation in Zirconium Complexes of Fluorinated Aryl Diamides
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              3947
_journal_paper_doi               10.1021/om0204181
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C64 H54 F18 N4 O4 Zr2'
_chemical_formula_weight         1467.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                82.974(2)
_cell_angle_beta                 79.912(2)
_cell_angle_gamma                87.465(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9913(11)
_cell_length_b                   11.0332(14)
_cell_length_c                   15.2867(19)
_cell_measurement_temperature    293(2)
_cell_volume                     1481.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11259
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.462
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             740
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0344P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                3960
_reflns_number_total             5201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0204181.cif
_cod_data_source_block           zrdcmp3a
_cod_database_code               4077011