Mechanistic Insights on the Controlled Switch from Oligomerization to Polymerization of 1-Hexene Catalyzed by an NHC-Zirconium Complex
Despagnet-Ayoub, Emmanuelle; Takase, Michael K.; Henling, Lawrence M.; Labinger, Jay A.; Bercaw, John E.; Organometallics 34 (2015) 4707–; doi:10.1021/acs.organomet.5b00472

data_4087667
_publ_section_title
;
 Mechanistic Insights on the Controlled Switch from Oligomerization to
 Polymerization of 1-Hexene Catalyzed by an NHC-Zirconium Complex
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4707
_journal_paper_doi               10.1021/acs.organomet.5b00472
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C88.34 H106 B F20 N2 O5.5 Zr'
_chemical_formula_weight         1765.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                110.410(2)
_cell_angle_beta                 103.088(3)
_cell_angle_gamma                103.450(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4145(9)
_cell_length_b                   18.8131(12)
_cell_length_c                   21.1906(15)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.96
_cell_measurement_theta_min      2.31
_cell_volume                     4246.7(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 v2014.7-1 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (She ldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            166089
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.391
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/3 (Sheldrick, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1838
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.892
_refine_diff_density_min         -1.486
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1188
_refine_ls_number_reflns         25914
_refine_ls_number_restraints     417
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+5.2871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21530
_reflns_number_total             25914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00472_si_001.cif
_cod_data_source_block           P14042
_cod_original_formula_sum        'C88.34 H106 B F20 N2 O5.50 Zr'
_cod_database_code               4087667
_shelx_estimated_absorpt_t_min   0.895
_shelx_estimated_absorpt_t_max   0.967
_shelxl_version_number           2014/6
_shelx_res_checksum              91928
_shelx_hkl_checksum              92491