An improved method for the synthesis of zirconium (CCC-N-heterocyclic carbene) pincer complexes and applications in hydroamination.
Cho, Joon; Hollis, T Keith; Helgert, Theodore R; Valente, Edward J; Chemical communications (Cambridge, England)  (2008) 5001–5003; doi:10.1039/b805174g

data_7103415
_publ_section_title
;
 An improved method for the synthesis of zirconium (CCC-N-heterocyclic
 carbene) pincer complexes and applications in hydroamination.
;
_journal_issue                   40
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5001
_journal_page_last               5003
_journal_paper_doi               10.1039/b805174g
_journal_year                    2008
_chemical_formula_moiety         'C22 H31 I2 N5 Zr1'
_chemical_formula_sum            'C22 H31 I2 N5 Zr'
_chemical_formula_weight         710.56
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.495(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1754(2)
_cell_length_b                   23.4958(4)
_cell_length_c                   10.8780(2)
_cell_measurement_reflns_used    12058
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.4998
_cell_measurement_theta_min      3.0812
_cell_volume                     2572.17(8)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction)'
_computing_data_collection       'CrysAlis (Oxford Diffraction)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction)'
_computing_molecular_graphics    WinGX
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 16.0309
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_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  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20493
_diffrn_reflns_theta_full        30.64
_diffrn_reflns_theta_max         30.64
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.846
_exptl_absorpt_correction_T_max  0.506
_exptl_absorpt_correction_T_min  0.318
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlis (Oxford Diffraction)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.5239
_exptl_crystal_size_mid          0.3841
_exptl_crystal_size_min          0.2732
_refine_diff_density_max         2.620
_refine_diff_density_min         -2.273
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         7719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0419P)^2^+6.6851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                6112
_reflns_number_total             7719
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b805174g.txt
_cod_data_source_block           mc074a
_cod_database_code               7103415