Very large cooperative effects in heterobimetallic titanium-chromium catalysts for ethylene polymerization/copolymerization.
Liu, Shaofeng; Motta, Alessandro; Mouat, Aidan R.; Delferro, Massimiliano; Marks, Tobin J.; Journal of the American Chemical Society 136 (2014) 10460–10469; doi:10.1021/ja5046742

data_4122221
_publ_section_title
;
 Very large cooperative effects in heterobimetallic titanium-chromium
 catalysts for ethylene polymerization/copolymerization.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10460
_journal_page_last               10469
_journal_paper_doi               10.1021/ja5046742
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C23 H38 Cl2 N2 S2 Si Ti'
_chemical_formula_sum            'C23 H38 Cl2 N2 S2 Si Ti'
_chemical_formula_weight         553.56
_chemical_name_systematic        CGCTiCl2-C0-SNS
_chemical_properties_physical
'air-sensitive, moisture-sensitive, oxygen-sensitive'
_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'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2013-07-11
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_audit_update_record
;
2014-05-08 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 107.348(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3021(3)
_cell_length_b                   29.2371(11)
_cell_length_c                   11.9237(4)
_cell_measurement_reflns_used    3084
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.48
_cell_measurement_theta_min      3.02
_cell_volume                     2762.58(18)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_computing_structure_solution
;
Sheldrick, G. M., Shelxtl Pc: An Integrated System for Solving, Refining, and
Displaying Crystal Structures from Diffraction Data. Version 6.014 ed.; Bruker
AXS: Madison, WI, 2000.
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.9740
_diffrn_measured_fraction_theta_max 0.9740
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1012
_diffrn_reflns_av_unetI/netI     0.0821
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22560
_diffrn_reflns_theta_full        67.0495
_diffrn_reflns_theta_max         67.05
_diffrn_reflns_theta_min         3.02
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.330
_exptl_absorpt_correction_T_max  0.7376
_exptl_absorpt_correction_T_min  0.2727
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Face-indexed via XPREP (Bruker)'
_exptl_crystal_colour            'metallic reddish violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.3309
_exptl_crystal_description       block
_exptl_crystal_F_000             1177.6718
_exptl_crystal_recrystallization_method 'hexane solution at -40C'
_exptl_crystal_size_max          0.755
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.086
_refine_diff_density_max         2.6271
_refine_diff_density_min         -0.6412
_refine_diff_density_rms         0.1656
_refine_ls_d_res_high            0.8372
_refine_ls_d_res_low             14.6186
_refine_ls_goodness_of_fit_ref   1.0286
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    56
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0286
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1237P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1994
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              34
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                3331
_reflns_number_total             4794
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja5046742_si_002.cif
_cod_data_source_block           LSF_mono_a
_cod_depositor_comments          'Adding full bibliography for 4122221.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4122221
_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C20(H20a,H20b), C21(H21a,H21b), C16(H16a,H16b), C22(H22a,H22b), C18(H18a,
 H18b), C17(H17a,H17b)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C1(H1), C6(H6), C7(H7), C5(H5)
3.c Idealised Me refined as rotating group:
 C15(H15a,H15b,H15c), C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C10(H10a,H10b,
 H10c), C11(H11a,H11b,H11c), C19(H19a,H19b,H19c), C23(H23a,H23b,H23c)
;