Discrete Ionic Complexes of Highly Isoselective Zirconocenes. Solution Dynamics, Trimethylaluminum Adducts, and Implications in Propylene Polymerization
Theurkauff, Gabriel; Bader, Manuela; Marquet, Nicolas; Bondon, Arnaud; Roisnel, Thierry; Guegan, Jean-Paul; Amar, Anissa; Boucekkine, Abdou; Carpentier, Jean-François; Kirillov, Evgueni; Organometallics 35 (2016) 258–; doi:10.1021/acs.organomet.5b00965

data_4088255
_publ_section_title
;
 Discrete Ionic Complexes of Highly Isoselective Zirconocenes. Solution
 Dynamics, Trimethylaluminum Adducts, and Implications in Propylene
 Polymerization
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              258
_journal_paper_doi               10.1021/acs.organomet.5b00965
_journal_volume                  35
_journal_year                    2016
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C41 H52 Zr1'
_chemical_formula_sum            'C41 H52 Zr'
_chemical_formula_weight         636.05
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2009-04-29T09:33:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.699(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8379(5)
_cell_length_b                   16.3525(7)
_cell_length_c                   17.4766(8)
_cell_measurement_reflns_used    7172
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      2.39
_cell_measurement_wavelength     0.71073
_cell_volume                     3379.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28752
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.25
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         7661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+2.8913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.097
_reflns_number_gt                6108
_reflns_number_total             7661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00965_si_001.cif
_cod_data_source_block           2b
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088255