The influences of electronic effect and isomerization of salalen titanium(iv) complexes on ethylene polymerization in the presence of methylaluminoxane
Li, Sihan; Zhu, Yuqiong; Liang, Huaqing; Xie, Xiuli; Zhan, Yipeng; Liang, Guodong; Zhu, Fangming; RSC Advances 9 (2019) 41824–; doi:10.1039/C9RA08899G

data_7239642
_publ_section_title
;
 The influences of electronic effect and isomerization of salalen
 titanium(iv) complexes on ethylene polymerization in the presence of
 methylaluminoxane
;
_journal_issue                   71
_journal_name_full               'RSC Advances'
_journal_page_first              41824
_journal_paper_doi               10.1039/C9RA08899G
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C25 H34 Cl2 N2 O2 Ti, C7 H8'
_chemical_formula_sum            'C32 H42 Cl2 N2 O2 Ti'
_chemical_formula_weight         605.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-06 deposited with the CCDC.	2019-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.381(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2955(4)
_cell_length_b                   30.4590(9)
_cell_length_c                   10.5847(3)
_cell_measurement_reflns_used    3382
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.9910
_cell_measurement_theta_min      4.8350
_cell_volume                     3090.82(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5826
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -124.00 -79.00   1.00   24.93    --  -36.00 -99.00  60.00   45
  2  \w   -124.00 -79.00   1.00   24.93    --  -36.00 -99.00-150.00   45
  3  \w   -114.00 -79.00   1.00   24.93    --  -36.00 -99.00 150.00   35
  4  \w     62.00 129.00   1.00   24.93    --   36.00 178.00   0.00   67
  5  \w     57.00 131.00   1.00   24.93    --   36.00 178.00-180.00   74
  6  \w     86.00 175.00   1.00   72.50    --  109.02  61.00 -30.00   89
  7  \w     44.00 139.00   1.00   72.50    --  109.02 -61.00-180.00   95
  8  \w     27.00 105.00   1.00   72.50    --  109.02-111.00  60.00   78
  9  \w     37.00 112.00   1.00   72.50    --  109.02-111.00 150.00   75
 10  \w     89.00 166.00   1.00   72.50    --  109.02  61.00-120.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1096449000
_diffrn_orient_matrix_UB_12      0.0214454000
_diffrn_orient_matrix_UB_13      -0.0478350000
_diffrn_orient_matrix_UB_21      -0.1137853000
_diffrn_orient_matrix_UB_22      0.0296834000
_diffrn_orient_matrix_UB_23      -0.0973804000
_diffrn_orient_matrix_UB_31      0.0296227000
_diffrn_orient_matrix_UB_32      0.0348847000
_diffrn_orient_matrix_UB_33      0.1124521000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0929
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9580
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.015
_diffrn_reflns_theta_min         4.716
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.172
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.163
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0828
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+9.9145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2140
_refine_ls_wR_factor_ref         0.2393
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4173
_reflns_number_total             5871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra08899g2.cif
_cod_data_source_block           HONNO-Ti
_cod_database_code               7239642
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H O Ti  N Cl'
_chemical_oxdiff_usercomment     HONNO
_reflns_odcompleteness_completeness 99.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_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.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C13(H13), C14(H14), C15(H15), C16(H16), C28(H28),
 C29(H29), C30(H30), C31(H31), C32(H32)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C)
;
_shelx_res_checksum              60212
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.404
_oxdiff_exptl_absorpt_empirical_full_min 0.574