Mechanism of Catalytic Cyclohydroamination by Zirconium Salicyloxazoline Complexes
Laura E. N. Allan; Guy J. Clarkson; David J. Fox; Andrew L. Gott; Peter Scott; Journal of the American Chemical Society 132 (2010) 15308–15320; doi:10.1021/ja106588m

data_4103402
_publ_section_title
;
 Mechanism of Catalytic Cyclohydroamination by Zirconium Salicyloxazoline
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15308
_journal_page_last               15320
_journal_paper_doi               10.1021/ja106588m
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C33 H55 N3 O2 Zr'
_chemical_formula_weight         617.02
_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                 115.4160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.1703(2)
_cell_length_b                   9.71680(10)
_cell_length_c                   39.0199(6)
_cell_measurement_reflns_used    27429
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.23
_cell_measurement_theta_min      2.96
_cell_volume                     6564.92(15)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            63814
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         2.96
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK(CrysAlis, Oxford Diffraction)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.770
_refine_diff_density_min         -1.773
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         16115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0392P)^2^+4.6523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                12293
_reflns_number_total             16115
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja106588m_si_002.cif
_cod_data_source_block           la5
_cod_original_cell_volume        6564.92(14)
_cod_database_code               4103402