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_1554176
_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         'C36 H36 Cl10 N4 O4 Ti2, 2(C7 H8)'
_chemical_formula_sum            'C50 H52 Cl10 N4 O4 Ti2'
_chemical_formula_weight         1223.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.694(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1807(5)
_cell_length_b                   19.7102(6)
_cell_length_c                   18.0932(7)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.4160
_cell_measurement_theta_min      3.3990
_cell_volume                     5351.5(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_details
;
  1 omega  -88.00   28.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -19.0000   30.0000 116

  2 omega  -85.00  -41.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  157.0000  -80.3391 44

  3 omega  -32.00   63.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747   38.0000 -150.0000 95

  4 omega  -20.00   31.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000  -60.0000 51

  5 omega  -20.00   31.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000  -30.0000 51

  6 omega  -20.00   31.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000  150.0000 51

  7 omega  -32.00   63.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747   38.0000  120.0000 95

  8 omega  -12.00   72.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372   38.0000  -90.0000 84

  9 omega    4.00   36.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -57.0000 -120.0000 32
;
_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      -0.0080838000
_diffrn_orient_matrix_UB_12      0.0033009000
_diffrn_orient_matrix_UB_13      -0.0394920000
_diffrn_orient_matrix_UB_21      -0.0465370000
_diffrn_orient_matrix_UB_22      -0.0016514000
_diffrn_orient_matrix_UB_23      0.0006380000
_diffrn_orient_matrix_UB_31      -0.0014039000
_diffrn_orient_matrix_UB_32      0.0358000000
_diffrn_orient_matrix_UB_33      0.0036792000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47257
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.613
_diffrn_reflns_theta_min         3.076
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       plate
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.3408
_exptl_crystal_size_mid          0.2758
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         7083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0304P)^2^+6.7281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5393
_reflns_number_total             7083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma9b00182_si_004.cif
_cod_data_source_block           Complex3dimer
_cod_database_code               1554176
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C18 H18 Cl5 N2 O2 Ti'
_chemical_oxdiff_usercomment     '@ 120 K BRML204a'
_reflns_odcompleteness_completeness 99.79
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C19B(0.35) H19A(0.35) H19B(0.35) H19C(0.35) C25B(0.35) C20B(0.35)
 H20B(0.35) C24B(0.35) H24B(0.35) C23B(0.35) H23B(0.35) C22B(0.35) H22B(0.35)
 C21B(0.35) H21B(0.35) C19A(0.65) H19D(0.65) H19E(0.65) H19F(0.65) C20A(0.65)
 C21A(0.65) H21A(0.65) C22A(0.65) H22A(0.65) C23A(0.65) H23A(0.65) C24A(0.65)
 H24A(0.65) C25A(0.65) H25A(0.65)
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C15(H15A,H15B), C16(H16A,H16B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C12(H12), C20B(H20B), C24B(H24B), C23B(H23B),
 C22B(H22B), C21B(H21B), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A),
 C25A(H25A)
3.c Fitted hexagon refined as free rotating group:
 C25B(C20B,C24B,C23B,C22B,C21B)
3.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19B(H19A,H19B,H19C), C19A(H19D,
 H19E,H19F)
;
_olex2_submission_special_instructions 'No special instructions were received'