Union carbide polymerization catalysts: from uncovering active site structures to designing molecularly-defined analogs
Trummer, David; Nobile, Anna Giorgia; Payard, Pierre-Adrien; Ashuiev, Anton; Kakiuchi, Yuya; Klose, Daniel; Jeschke, Gunnar; Copéret, Christophe; Chemical Science 13 (2022) 11091–11098; doi:10.1039/D2SC04235E

data_1567649
_publ_section_title
;
 Union carbide polymerization catalysts: from uncovering active site
 structures to designing molecularly-defined analogs
;
_journal_issue                   37
_journal_name_full               'Chemical Science'
_journal_page_first              11091
_journal_page_last               11098
_journal_paper_doi               10.1039/D2SC04235E
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C24 H48 Cl2 Cr2 Si4'
_chemical_formula_sum            'C24 H48 Cl2 Cr2 Si4'
_chemical_formula_weight         623.88
_chemical_name_common            '[Cr(Cp)(CH(SiMe3)2)Cl]2'
_chemical_name_systematic
di[(bistrimethylsilyl)methyl)(cyclopentadienyl)chromium(chlorido)]
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Pyrophoric
_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
_audit_creation_date             2022-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-01 deposited with the CCDC.	2022-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.402(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2426(5)
_cell_length_b                   7.9314(3)
_cell_length_c                   15.6465(5)
_cell_measurement_reflns_used    3730
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      2.66
_cell_volume                     1610.96(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      99.98
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11809
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.399
_diffrn_reflns_theta_min         2.656
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0576 before and 0.0438 after correction. The Ratio of minimum to maximum transmission is 0.8501. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic brownish violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       plate
_exptl_crystal_F_000             660
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         3288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0616P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2646
_reflns_number_total             3288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04235e3.cif
_cod_data_source_block           prelim_p21_c_sx
_cod_depositor_comments
'Adding full bibliography for 1567649--1567650.cif.'
_cod_database_code               1567649
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.753
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C005(H005)
2.b Aromatic/amide H refined with riding coordinates:
 C006(H006), C008(H008), C009(H009), C00A(H00D), C00C(H00H)
2.c Idealised Me refined as rotating group:
 C007(H00A,H00B,H00C), C00B(H00E,H00F,H00G), C00D(H00I,H00J,H00K), C00E(H00L,
 H00M,H00N), C00F(H00O,H00P,H00Q), C00G(H00R,H00S,H00T)
;
_shelx_res_checksum              9851
_shelx_hkl_checksum              91855
_olex2_exptl_crystal_mounting_method 'paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'