Radically Initiated Group Transfer Polymerization of Methacrylates by Titanium Amino-Phenolate Complexes
Coward, Daniel L.; Lake, Benjamin R. M.; Poli, Rinaldo; Shaver, Michael P.; Macromolecules 52 (2019) 3252–; doi:10.1021/acs.macromol.9b00182

data_1554181
_publ_section_title
;
 Radically Initiated Group Transfer Polymerization of Methacrylates by
 Titanium Amino-Phenolate Complexes
;
_journal_issue                   9
_journal_name_full               Macromolecules
_journal_page_first              3252
_journal_paper_doi               10.1021/acs.macromol.9b00182
_journal_volume                  52
_journal_year                    2019
_chemical_formula_moiety         '2(C26 H38 Cl N2 O3 Ti), C4 H8 O'
_chemical_formula_sum            'C56 H84 Cl2 N4 O7 Ti2'
_chemical_formula_weight         1091.91
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.8755(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.61539(7)
_cell_length_b                   15.80257(11)
_cell_length_c                   20.58955(17)
_cell_measurement_reflns_used    25040
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.0510
_cell_measurement_theta_min      4.3130
_cell_volume                     2783.01(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -50.00   29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000  -60.0000 79

  2 omega -117.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000 -180.0000 105

  3 omega  -96.00   -2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  125.0000  -60.0000 94

  4 omega -113.00  -66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686 -136.0000  151.0000 47

  5 omega  -70.00   27.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   57.0000 -150.0000 97

  6 omega -113.00  -17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000   60.0000 96

  7 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  150.0000 82

  8 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 79

  9 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 82

 10 omega   40.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -180.0000 59

 11 omega   40.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -60.0000 59

 12 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -30.0000 82

 13 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -60.0000 55

 14 omega   31.00  156.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000   30.0000 125

 15 omega   31.00  156.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000 -120.0000 125

 16 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 79

 17 omega   37.00  142.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  -30.0000 105

 18 omega   41.00  139.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000 -180.0000 98

 19 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 79

 20 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 79

 21 omega   40.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   30.0000 59

 22 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   30.0000 55

 23 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 82

 24 omega   87.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000 -120.0000 91

 25 omega   30.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -60.0000 79

 26 omega   94.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  150.0000 84

 27 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -150.0000 55

 28 omega   40.00   99.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   90.0000 59

 29 omega   39.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -150.0000 82

 30 omega   80.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000 -150.0000 98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0345050000
_diffrn_orient_matrix_UB_12      -0.0013579000
_diffrn_orient_matrix_UB_13      0.0751361000
_diffrn_orient_matrix_UB_21      -0.1761751000
_diffrn_orient_matrix_UB_22      0.0079580000
_diffrn_orient_matrix_UB_23      0.0055197000
_diffrn_orient_matrix_UB_31      -0.0149191000
_diffrn_orient_matrix_UB_32      -0.0971708000
_diffrn_orient_matrix_UB_33      -0.0006001000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44749
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.187
_diffrn_reflns_theta_min         3.535
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.751
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       plate
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.2663
_exptl_crystal_size_mid          0.0972
_exptl_crystal_size_min          0.0344
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5809
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0932P)^2^+1.4057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1386
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5526
_reflns_number_total             5809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma9b00182_si_001.cif
_cod_data_source_block           Complex2
_cod_database_code               1554181
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C26 H38 Cl N2 O3 Ti'
_chemical_oxdiff_usercomment     '@ 120 K BRML205'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 C27B-H27B = C27B-H27A
 0.99 with sigma of 0.02
 H27A-H27B
 1.61 with sigma of 0.04
3. Others
 Fixed Sof: O4(0.5) C28(0.5) H28A(0.5) H28B(0.5) C29(0.5) H29A(0.5) H29B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C19(H19A,H19B), C20(H20A,H20B), C23(H23A,H23B),
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_olex2_submission_special_instructions 'No special instructions were received'