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_7713102
_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         'C20 H24 Cl2 Si Zr'
_chemical_formula_sum            'C20 H24 Cl2 Si Zr'
_chemical_formula_weight         454.60
_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     dual
_audit_update_record
;
2023-03-13 deposited with the CCDC.	2023-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                74.342(6)
_cell_angle_beta                 71.581(9)
_cell_angle_gamma                75.201(6)
_cell_formula_units_Z            2
_cell_length_a                   9.640(2)
_cell_length_b                   10.518(3)
_cell_length_c                   10.543(2)
_cell_measurement_reflns_used    219
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17.5789
_cell_measurement_theta_min      2.7604
_cell_measurement_wavelength     0.710730
_cell_volume                     959.5(4)
_computing_molecular_graphics
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2021)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CCD-LDI-APEX2
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'APEXII Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_orient_matrix_UB_11      -0.0330256
_diffrn_orient_matrix_UB_12      -0.0877758
_diffrn_orient_matrix_UB_13      0.0470247
_diffrn_orient_matrix_UB_21      0.0927638
_diffrn_orient_matrix_UB_22      -0.0482332
_diffrn_orient_matrix_UB_23      -0.0561929
_diffrn_orient_matrix_UB_31      0.0521879
_diffrn_orient_matrix_UB_32      -0.0098863
_diffrn_orient_matrix_UB_33      0.0714499
_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     0.1045
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4221
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         2.047
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.714
_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    1.573
_exptl_crystal_description       prism
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         4221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+2.7187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1394
_reflns_number_gt                2879
_reflns_number_total             4221
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt01306e2.cif
_cod_data_source_block           3a-Zr_SAR074
_cod_database_code               7713102
_shelx_res_checksum              89000
_shelx_hkl_checksum              96299