Stereoselectivity Inversion: Isospecific Propylene Polymerization Catalyzed by Rigid Cyclic Bis(phenoxyaldimine) Titanium Complexes
Zhao, Xiangxiang; Chen, Zhongtao; Li, Hao; Ma, Yuguo; Macromolecules 53 (2020) 3806–3813; doi:10.1021/acs.macromol.0c00468

data_1558040
_publ_section_title
;
 Stereoselectivity Inversion: Isospecific Propylene Polymerization
 Catalyzed by Rigid Cyclic Bis(phenoxyaldimine) Titanium Complexes
;
_journal_issue                   10
_journal_name_full               Macromolecules
_journal_page_first              3806
_journal_page_last               3813
_journal_paper_doi               10.1021/acs.macromol.0c00468
_journal_volume                  53
_journal_year                    2020
_chemical_formula_moiety         'C64 H50 F8 N2 O4, C H Cl3'
_chemical_formula_sum            'C65 H51 Cl3 F8 N2 O4'
_chemical_formula_weight         1182.43
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.8430(5)
_cell_length_b                   23.5705(9)
_cell_length_c                   33.4177(11)
_cell_measurement_reflns_used    14238
_cell_measurement_temperature    99.94(15)
_cell_measurement_theta_max      30.0880
_cell_measurement_theta_min      3.7580
_cell_volume                     10903.7(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.94(15)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.955
_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    -49.00  11.00   0.50    8.25    --   -1.70 -57.00-120.00  120
  2  \w    -82.00 -28.00   0.50    8.25    --   -1.70 -57.00-180.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0112285000
_diffrn_orient_matrix_UB_12      -0.0235719000
_diffrn_orient_matrix_UB_13      -0.0123516000
_diffrn_orient_matrix_UB_21      -0.0042342000
_diffrn_orient_matrix_UB_22      -0.0183574000
_diffrn_orient_matrix_UB_23      0.0167306000
_diffrn_orient_matrix_UB_31      -0.0498083000
_diffrn_orient_matrix_UB_32      -0.0037651000
_diffrn_orient_matrix_UB_33      -0.0041854000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0787
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            39862
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.468
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.249
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             4880
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.491
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         10254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0874
_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^)+(0.0887P)^2^+31.5380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1948
_refine_ls_wR_factor_ref         0.2125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7607
_reflns_number_total             10254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma0c00468_si_004.cif
_cod_data_source_block           exp_566
_cod_depositor_comments
;Adding full bibliography for 1558039--1558041.cif.

 Adding full bibliography for 1558039--1558041.cif.
;
_cod_database_code               1558040
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C64 N2 O4 F8'
_chemical_oxdiff_usercomment     'LS170303-4, Mn C4H10N1'
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.964
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C65(H65)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C13(H13), C17(H17), C19(H19), C21(H21), C22(H22),
 C23(H23), C28(H28), C29(H29), C30(H30), C39(H39), C43(H43), C45(H45), C47(H47),
  C48(H48), C49(H49)
2.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,
 H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3A), O4(H4A)
;
_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 2.031
_oxdiff_exptl_absorpt_empirical_full_min 0.281