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_7713110
_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         'C35 H46 Cl2 Si Zr, 1/3(C7 H16)'
_chemical_formula_sum            'C37.33333 H51.33333 Cl2 Si Zr'
_chemical_formula_weight         690.32
_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
_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                86.522(3)
_cell_angle_beta                 85.210(2)
_cell_angle_gamma                84.849(2)
_cell_formula_units_Z            6
_cell_length_a                   12.6320(8)
_cell_length_b                   18.1924(14)
_cell_length_c                   23.8569(17)
_cell_measurement_reflns_used    9085
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4931
_cell_measurement_theta_min      2.2509
_cell_measurement_wavelength     0.710730
_cell_volume                     5433.4(7)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2020)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CCD-LDI-APEX2
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'APEXII Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_orient_matrix_UB_11      -0.0050593
_diffrn_orient_matrix_UB_12      -0.0358960
_diffrn_orient_matrix_UB_13      0.0333632
_diffrn_orient_matrix_UB_21      -0.0488453
_diffrn_orient_matrix_UB_22      0.0370101
_diffrn_orient_matrix_UB_23      0.0210114
_diffrn_orient_matrix_UB_31      -0.0628139
_diffrn_orient_matrix_UB_32      -0.0199131
_diffrn_orient_matrix_UB_33      -0.0148273
_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_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            74930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         1.895
_diffrn_source_current           1.0
_diffrn_source_power             50.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.806
_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    1.266
_exptl_crystal_description       prism
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.097
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1153
_refine_ls_number_reflns         24534
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+1.6020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                18204
_reflns_number_total             24534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt01306e2.cif
_cod_data_source_block           3j_Zr_SAR2307
_cod_depositor_comments
;

2024-10-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C112 H154 Cl6 Si3 Zr3'
_cod_original_formula_weight         2070.97
_cod_original_formula_moiety         '3(C35 H46 Cl2 Si Zr), C7 H16'
_cod_original_formula_units_Z            2
_cod_database_code               7713110
_shelx_res_checksum              31840
_shelx_hkl_checksum              46277
_shelx_fab_checksum              33625