Formation of a Dynamic η2(O,N)-Hydroxylaminato Zirconocene Complex by Nitrosoarene Insertion into a Zr−C σ-Bond
Cummings, Sarah A.; Radford, Robert; Erker, Gerhard; Kehr, Gerald; Fröhlich, Roland; Organometallics 25 (2006) 839–; doi:10.1021/om050946n

data_4074865
_publ_section_title
;
 Formation of a Dynamic \h2(O,N)-Hydroxylaminato Zirconocene Complex by
 Nitrosoarene Insertion into a Zr&#x2212;C \s-Bond
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              839
_journal_paper_doi               10.1021/om050946n
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C18 H21 N O Zr'
_chemical_formula_weight         358.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 97.76(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.558(1)
_cell_length_b                   7.936(1)
_cell_length_c                   23.267(1)
_cell_measurement_reflns_used    6716
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      0.41
_cell_volume                     3212.3(5)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20783
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  0.9348
_exptl_absorpt_correction_T_min  0.7960
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995 & 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0022(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         7642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0284P)^2^+1.3189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                6251
_reflns_number_total             7642
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050946nsi20051103_082529.cif
_cod_data_source_block           erk3446
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4074865