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_1554180
_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         'C22 H26 Cl5 N2 O3 Ti'
_chemical_formula_sum            'C22 H26 Cl5 N2 O3 Ti'
_chemical_formula_weight         591.60
_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     dual
_audit_creation_date             2019-01-09
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.9365(3)
_cell_length_b                   14.9569(2)
_cell_length_c                   21.2219(3)
_cell_measurement_reflns_used    50064
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      32.5760
_cell_measurement_theta_min      3.1550
_cell_volume                     5058.47(14)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction
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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)'
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_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 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega -103.00  -55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5248  178.0000 -180.0000 48

  2 omega  -40.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5248   38.0000 -180.0000 95

  3 omega -103.00  -55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5248  178.0000   30.0000 48

  4 omega  -54.00   61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5248   19.0000 -180.0000 115

  5 omega  -49.00   56.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5248   77.0000 -150.0000 105

  6 omega -104.00  -57.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5248 -178.0000 -150.0000 47

  7 omega  -55.00   50.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311  -77.0000   60.0000 105

  8 omega  -55.00   50.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311  -77.0000 -120.0000 105

  9 omega  -20.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311  -99.0000  -90.0000 79

 10 omega  -12.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311   77.0000    0.0000 105

 11 omega  -55.00   50.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311  -77.0000  -30.0000 105

 12 omega   -4.00   92.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311   38.0000    0.0000 96

 13 omega  -55.00   50.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311  -77.0000  120.0000 105

 14 omega  -12.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311   77.0000 -180.0000 105

 15 omega  -54.00   41.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311  -38.0000  -90.0000 95

 16 omega  -90.00    5.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5248  -38.0000    0.0000 95

 17 omega  -20.00   26.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311  -99.0000 -180.0000 46

 18 omega   -8.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311   57.0000  -60.0000 97
;
_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      -0.0248282000
_diffrn_orient_matrix_UB_12      -0.0011684000
_diffrn_orient_matrix_UB_13      0.0277358000
_diffrn_orient_matrix_UB_21      -0.0369275000
_diffrn_orient_matrix_UB_22      0.0024306000
_diffrn_orient_matrix_UB_23      -0.0185848000
_diffrn_orient_matrix_UB_31      -0.0013092000
_diffrn_orient_matrix_UB_32      -0.0473317000
_diffrn_orient_matrix_UB_33      -0.0016171000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            248707
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.959
_diffrn_reflns_theta_min         2.888
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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    1.554
_exptl_crystal_description       prism
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.3517
_exptl_crystal_size_mid          0.1178
_exptl_crystal_size_min          0.0475
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         9356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+4.0684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8471
_reflns_number_total             9356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma9b00182_si_003.cif
_cod_data_source_block           Complex3
_cod_original_cell_volume        5058.45(14)
_cod_database_code               1554180
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 H26 Cl5 N2 O3 Ti'
_chemical_oxdiff_usercomment     '@ 120 K BRML204'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H20A)=Sof(H20B)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H22A)=Sof(H22B)=1-FVAR(1)
 Sof(H20C)=Sof(H20D)=Sof(H22C)=Sof(H22D)=Sof(C21B)=Sof(H21C)=Sof(H21D)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B), C19(H19A,H19B),
 C20(H20A,H20B), C20(H20C,H20D), C21A(H21A,H21B), C22(H22A,H22B), C22(H22C,
 H22D), C21B(H21C,H21D)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C12(H12)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_olex2_submission_special_instructions 'No special instructions were received'