Catalytically Active N-Acylamidine‒Zirconium Complexes: Synthesis, Structures, and Application in Ethylene Polymerization
Holtrichter-Rößmann, Thorsten; Häger, Ina; Daniliuc, Constantin-Gabriel; Fröhlich, Roland; Bergander, Klaus; Troll, Carsten; Rieger, Bernhard; Rojas, René S.; Würthwein, Ernst-Ulrich; Organometallics 35 (2016) 1906–; doi:10.1021/acs.organomet.6b00240

data_4088617
_publ_section_title
;
 Catalytically Active N-Acylamidine--Zirconium Complexes: Synthesis,
 Structures, and Application in Ethylene Polymerization
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1906
_journal_paper_doi               10.1021/acs.organomet.6b00240
_journal_volume                  35
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_sum            'C56 H52 Cl8 N4 O2 Zr2'
_chemical_formula_weight         1279.06
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.63920(10)
_cell_length_b                   16.9432(2)
_cell_length_c                   30.9376(5)
_cell_measurement_reflns_used    10719
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     5576.88(12)
_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      223(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            36287
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.08
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_T_max  0.9029
_exptl_absorpt_correction_T_min  0.7949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         9672
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0722P)^2^+9.3491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1234
_reflns_number_gt                9391
_reflns_number_total             9672
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00240_si_007.cif
_cod_data_source_block           erk6500
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4088617