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_4088257
_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
'C40 H49 Zr, C19 H3 B F15, 0.5(C5 H12), 0.5(C7 H8)'
_chemical_formula_sum            'C65 H62 B F15 Zr'
_chemical_formula_weight         1230.17
_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
_cell_angle_alpha                102.555(5)
_cell_angle_beta                 90.026(5)
_cell_angle_gamma                98.579(5)
_cell_formula_units_Z            4
_cell_length_a                   11.3858(16)
_cell_length_b                   20.846(3)
_cell_length_c                   26.352(4)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.75
_cell_measurement_wavelength     0.71073
_cell_volume                     6033.2(15)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2014)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'CRYSCALc (T. Roisnel, local program, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.943
_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_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.3303
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            26223
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.543
_diffrn_reflns_theta_min         0.792
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       stick
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.570
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.376
_refine_diff_density_min         -3.024
_refine_diff_density_rms         0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     997
_refine_ls_number_reflns         26223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.2418
_refine_ls_R_factor_gt           0.1367
_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^)+(0.1419P)^2^+56.4371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3243
_refine_ls_wR_factor_ref         0.3715
_reflns_number_gt                12394
_reflns_number_total             26223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00965_si_001.cif
_cod_data_source_block           3b_MeBF15
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_space_group_crystal_system' value 'Triclinic' was changed
to 'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 

2026-05-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C130 H124 B2 F30 Zr2'
_cod_original_formula_weight         2460.34
_cod_original_formula_moiety
'2(C40 H49 Zr), 2(C19 H3 B F15), C5 H12, C7 H8'
_cod_original_formula_units_Z            2
_cod_database_code               4088257