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_4088259
_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         'C35 H33 Si Zr, C19 H3 Al F15, C7 H8'
_chemical_formula_sum            'C61 H44 Al F15 Si Zr'
_chemical_formula_weight         1208.25
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_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             2013-11-21T14:41:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                70.988(3)
_cell_angle_beta                 80.287(3)
_cell_angle_gamma                78.634(3)
_cell_formula_units_Z            4
_cell_length_a                   12.5266(8)
_cell_length_b                   21.2097(14)
_cell_length_c                   21.4671(15)
_cell_measurement_reflns_used    7371
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.64
_cell_measurement_theta_min      2.41
_cell_measurement_wavelength     0.71073
_cell_volume                     5252.9(6)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0495
_diffrn_reflns_av_unetI/netI     0.09
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            51731
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.981
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1405
_refine_ls_number_reflns         23781
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.2564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                15114
_reflns_number_total             23781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00965_si_001.cif
_cod_data_source_block           3c_MeAlF15
_cod_depositor_comments
;

2026-05-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C122 H88 Al2 F30 Si2 Zr2'
_cod_original_formula_weight         2416.5
_cod_original_formula_moiety         'C122 H88 Al2 F30 Si2 Zr2'
_cod_original_formula_units_Z            2
_cod_database_code               4088259