Bis[(amidomethyl)pyridine] Zirconium(IV) Complexes: Synthesis, Characterization, and Activity as Olefin Polymerization Catalysts†
Annunziata, Liana; Pappalardo, Daniela; Tedesco, Consiglia; Pellecchia, Claudio; Organometallics 28 (2009) 688–; doi:10.1021/om800736w

data_4068346
_publ_section_title
;
 Bis[(amidomethyl)pyridine] Zirconium(IV) Complexes: Synthesis,
 Characterization, and Activity as Olefin Polymerization Catalysts&#x2020;
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              688
_journal_paper_doi               10.1021/om800736w
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C30 H28 F10 N6 Zr'
_chemical_formula_sum            'C30 H28 F10 N6 Zr'
_chemical_formula_weight         753.80
_chemical_name_systematic
; 
 ? 
;
_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                90.499(6)
_cell_angle_beta                 93.571(7)
_cell_angle_gamma                96.789(6)
_cell_formula_units_Z            2
_cell_length_a                   9.463(2)
_cell_length_b                   12.446(3)
_cell_length_c                   12.821(3)
_cell_measurement_temperature    100(1)
_cell_volume                     1496.3(6)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1994)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.857
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: 0.0000 - 180.0000
         Image width: 1.0000
            Exp time: 5.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 41.4125
              2theta: -10.1675
scan:
    Number of images: 40
               Slice: -15.0000 - 25.0000
         Image width: 1.0000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: -90.0000
                 Phi: 0.0000
                 XTD: 41.4125
              2theta: -10.1675
scan:
    Number of images: 40
               Slice: -15.0000 - 25.0000
         Image width: 1.0000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: -90.0000
                 Phi: 90.0000
                 XTD: 41.4125
              2theta: -10.1675

;
_diffrn_measurement_device
;
Mercury2 (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC7: Eulerian 3 circle
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0560
_diffrn_orient_matrix_UB_12      -0.0197
_diffrn_orient_matrix_UB_13      0.0886
_diffrn_orient_matrix_UB_21      -0.0151
_diffrn_orient_matrix_UB_22      0.0705
_diffrn_orient_matrix_UB_23      0.0368
_diffrn_orient_matrix_UB_31      -0.0610
_diffrn_orient_matrix_UB_32      -0.0313
_diffrn_orient_matrix_UB_33      0.0376
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8298
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.65
_diffrn_source_current           40.0000
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.410
_refine_diff_density_min         -1.512
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         5033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0695
_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^)+(0.1398P)^2^+1.9866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2113
_refine_ls_wR_factor_ref         0.2182
_reflns_number_gt                4628
_reflns_number_total             5033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800736w_si_002.cif
_cod_data_source_block           crio5
_cod_database_code               4068346