C1-Symmetric {Cyclopentadienyl/Indenyl}-Metallocene Catalysts: Synthesis, Structure, Isospecific Polymerization of Propylene and Stereocontrol Mechanism
Theodosopoulou, Dimitra; De La Pena, Miguel Alonso; Abou-Derhamine, Sary; Douair, Iskander; Roisnel, Thierry; Cordier, Marie; Piola, Lorenzo; Fernandez, Alvaro; Welle, Alexandre; Maron, Laurent; Carpentier, Jean-Francois; Kirillov, Evgueni; Dalton Transactions  (2023) –; doi:10.1039/D3DT01306E

data_7713107
_publ_section_title
;
 C1-Symmetric {Cyclopentadienyl/Indenyl}-Metallocene Catalysts: Synthesis,
 Structure, Isospecific Polymerization of Propylene and Stereocontrol
 Mechanism
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01306E
_journal_year                    2023
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H40 Cl2 O Si Zr'
_chemical_formula_sum            'C32 H40 Cl2 O Si Zr'
_chemical_formula_weight         630.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2023-03-13 deposited with the CCDC.	2023-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.912(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5939(16)
_cell_length_b                   13.3843(13)
_cell_length_c                   17.1306(19)
_cell_measurement_reflns_used    8923
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.6134
_cell_measurement_theta_min      2.1896
_cell_measurement_wavelength     0.71073
_cell_volume                     2965.8(6)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2019)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (G. Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      -0.0085714
_diffrn_orient_matrix_UB_12      0.0203788
_diffrn_orient_matrix_UB_13      -0.0578795
_diffrn_orient_matrix_UB_21      0.0540791
_diffrn_orient_matrix_UB_22      0.0526350
_diffrn_orient_matrix_UB_23      0.0201982
_diffrn_orient_matrix_UB_31      0.0545776
_diffrn_orient_matrix_UB_32      -0.0489539
_diffrn_orient_matrix_UB_33      -0.0023774
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.0824
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21525
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.519
_diffrn_reflns_theta_min         2.190
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       prism
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0886P)^2^+0.5835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5391
_reflns_number_total             6750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt01306e2.cif
_cod_data_source_block           3d-Zr_DT120
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7713107
_shelx_res_checksum              17067
_shelx_hkl_checksum              54543