Aggregated initiators: defining their role in the ROP of rac-lactide.
Cols, Jean-Marie E P; Hill, Victoria G.; Williams, Stella K.; McIntosh, Ruaraidh D.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10626–10635; doi:10.1039/c8dt01229f

data_7046398
_publ_section_title
;
 Aggregated initiators: defining their role in the ROP of rac-lactide.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10626
_journal_page_last               10635
_journal_paper_doi               10.1039/c8dt01229f
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration S
_chemical_formula_moiety         'C33 H51 N O4, 2(C H4 O)'
_chemical_formula_sum            'C35 H59 N O6'
_chemical_formula_weight         589.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-02-17
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.02.06 svn.r3384 for OlexSys, GUI svn.r5312)
;
_audit_update_record
;
2017-07-13 deposited with the CCDC.
2018-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.02228(2)
_cell_length_b                   11.92120(2)
_cell_length_c                   33.55582(6)
_cell_measurement_reflns_used    256451
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.1030
_cell_measurement_theta_min      3.9220
_cell_volume                     3609.143(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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      3.00  29.40   0.80    2.00    --   38.00  91.00  36.17   33
  2  \w      2.00  28.40   0.80    2.00    --   38.00  92.00-144.40   33
  3  \w   -112.00 -16.00   0.80    2.00    --  -43.17 -57.00-150.00  120
  4  \w   -115.00 -20.60   0.80    2.00    --  -43.17 -38.00  60.00  118
  5  \w   -115.00 -20.60   0.80    2.00    --  -43.17 -38.00 -60.00  118
  6  \w    -70.00  26.80   0.80    2.00    --  -43.17  57.00   0.00  121
  7  \w   -115.00 -20.60   0.80    2.00    --  -43.17 -38.00-120.00  118
  8  \w    -70.00  26.80   0.80    2.00    --  -43.17  57.00-120.00  121
  9  \w     23.00  98.20   0.80    2.00    --   43.17-125.00-180.00   94
 10  \w     14.00  46.00   0.80    2.00    --   46.00  80.00 178.36   40
 11  \w     13.00  39.40   0.80    2.00    --   46.00  83.00 -39.13   33
 12  \w     18.00  46.00   0.80    2.00    --   50.00  81.00-115.28   35
 13  \w     96.00 124.00   0.80    2.00    --   50.00  82.00  93.79   35
 14  \w     22.00  50.00   0.80    2.00    --   54.00  78.00-135.93   35
 15  \w     22.00  50.00   0.80    2.00    --   54.00  78.00 -35.99   35
 16  \w     22.00  50.00   0.80    2.00    --   54.00  78.00  15.34   35
 17  \w     28.00 132.00   0.80    2.00    --   58.00  76.00 123.95  130
 18  \w     36.00 140.00   0.80    2.00    --   66.00  76.00  33.82  130
 19  \w     36.00 140.00   0.80    2.00    --   66.00  76.00 171.69  130
 20  \w     38.00 136.40   0.80    2.00    --   66.00  69.00 152.59  123
 21  \w     36.00 138.40   0.80    2.00    --   66.00  75.00 -96.57  128
 22  \w     36.00 140.00   0.80    2.00    --   66.00  77.00 -62.79  130
 23  \w     40.00 144.00   0.80    2.00    --   70.00  77.00-130.23  130
 24  \w     40.00 144.00   0.80    2.00    --   70.00  76.00  42.33  130
 25  \w     40.00 142.40   0.80    2.00    --   70.00  75.00 -19.21  128
 26  \w     45.00 145.80   0.80    2.00    --   74.00  70.00-155.83  126
 27  \w     44.00 148.00   0.80    2.00    --   74.00  77.00 -11.89  130
 28  \w     44.00 148.00   0.80    2.00    --   74.00  77.00  57.07  130
 29  \w     49.00 149.80   0.80    5.00    --   78.00  72.00 157.49  126
 30  \w     51.00 155.00   0.80    5.00    --   82.00  74.00  43.74  130
 31  \w     53.00 154.60   0.80    5.00    --   82.00  73.00  82.86  127
 32  \w     53.00 153.80   0.80    5.00    --   82.00  70.00 -68.31  126
 33  \w     58.00 156.40   0.80    5.00    --   86.00  67.00 113.29  123
 34  \w     58.00 156.40   0.80    5.00    --   86.00  69.00-157.69  123
 35  \w     55.00 159.00   0.80    5.00    --   86.00  74.00 -72.82  130
 36  \w     60.00 161.60   0.80    5.00    --   90.00  71.00 122.58  127
 37  \w     61.00 161.80   0.80    5.00    --   90.00  70.00 111.91  126
 38  \w     61.00 161.80   0.80    5.00    --   90.00  72.00  20.45  126
 39  \w     63.00 167.00   0.80    5.00    --   94.00  74.00-140.20  130
 40  \w     65.00 166.60   0.80    5.00    --   94.00  73.00 135.49  127
 41  \w     65.00 165.80   0.80    5.00    --   94.00  70.00-116.10  126
 42  \w     64.00 165.60   0.80    5.00    --   94.00  71.00 -55.12  127
 43  \w     72.00 173.60   0.80    5.00    --  102.00  71.00 -43.93  127
 44  \w     74.00 172.40   0.80    5.00    --  102.00  66.00 167.26  123
 45  \w     76.00 178.40   0.80    5.00    --  106.00  77.00  55.47  128
 46  \w     80.00 178.40   0.80    5.00    --  111.00  77.00 150.00  123
 47  \w     80.00 178.40   0.80    5.00    --  111.00  77.00-180.00  123
 48  \w     41.00 135.40   0.80    5.00    --  111.00 -45.00-180.00  118
 49  \w     40.00 121.60   0.80    5.00    --  111.00-125.00  90.00  102
 50  \w     40.00 121.60   0.80    5.00    --  111.00-125.00 -60.00  102
 51  \w     31.00 108.60   0.80    5.00    --  111.00 -94.00 -30.00   97
 52  \w     80.00 178.40   0.80    5.00    --  111.00  77.00 -90.00  123
 53  \w     84.00 178.40   0.80    5.00    --  111.00  61.00 -60.00  118
 54  \w     80.00 178.40   0.80    5.00    --  111.00  77.00  90.00  123
 55  \w     94.00 178.80   0.80    5.00    --  111.00 125.00 -30.00  106
 56  \w     40.00 121.60   0.80    5.00    --  111.00-125.00-120.00  102
 57  \w     80.00 178.40   0.80    5.00    --  111.00  77.00-120.00  123
 58  \w     84.00 178.40   0.80    5.00    --  111.00  61.00-150.00  118
 59  \w     80.00 178.40   0.80    5.00    --  111.00  77.00   0.00  123
 60  \w     37.00 134.60   0.80    5.00    --  111.00 -30.00-120.00  122
 61  \w     94.00 178.80   0.80    5.00    --  111.00 125.00 -90.00  106
 62  \w     84.00 178.40   0.80    5.00    --  111.00  61.00 150.00  118
 63  \w     80.00 178.40   0.80    5.00    --  111.00  77.00 120.00  123
 64  \w     81.00 178.60   0.80    5.00    --  111.00  70.00 -28.37  122
 65  \w     40.00 121.60   0.80    5.00    --  111.00-125.00 -30.00  102
 66  \w     80.00 178.40   0.80    5.00    --  111.00  77.00 -30.00  123
 67  \w     31.00 108.60   0.80    5.00    --  111.00 -94.00-180.00   97
 68  \w     80.00 178.40   0.80    5.00    --  111.00  77.00  60.00  123
 69  \w     84.00 178.40   0.80    5.00    --  111.00  61.00 120.00  118
 70  \w     84.00 178.40   0.80    5.00    --  111.00  61.00-180.00  118
 71  \w     31.00 108.60   0.80    5.00    --  111.00 -94.00 120.00   97
 72  \w     94.00 178.80   0.80    5.00    --  111.00 125.00 150.00  106
 73  \w     94.00 178.80   0.80    5.00    --  111.00 125.00-180.00  106
 74  \w     40.00 121.60   0.80    5.00    --  111.00-125.00  60.00  102
 75  \w     40.00 121.60   0.80    5.00    --  111.00-125.00 -90.00  102
 76  \w     84.00 178.40   0.80    5.00    --  111.00  61.00 -90.00  118
 77  \w     84.00 178.40   0.80    5.00    --  111.00  61.00  30.00  118
 78  \w     84.00 178.40   0.80    5.00    --  111.00  61.00-120.00  118
 79  \w     42.00 138.00   0.80    5.00    --  111.00 -59.00-155.99  120
 80  \w     84.00 178.40   0.80    5.00    --  111.00  61.00  60.00  118
 81  \w     84.00 178.40   0.80    5.00    --  111.00  61.00   0.00  118
 82  \w     96.00 178.40   0.80    5.00    --  111.00  79.00-104.95  103
 83  \w     84.00 178.40   0.80    5.00    --  111.00  61.00  90.00  118
 84  \w     94.00 178.80   0.80    5.00    --  111.00 125.00   0.00  106
 85  \w     42.00 138.80   0.80    5.00    --  111.00 -61.00  60.00  121
 86  \w     80.00 178.40   0.80    5.00    --  111.00  74.00-155.24  123
 87  \w     80.00 178.40   0.80    5.00    --  111.00  77.00  30.00  123
 88  \w     40.00 121.60   0.80    5.00    --  111.00-125.00 120.00  102
 89  \w     41.00 135.40   0.80    5.00    --  111.00 -45.00 -90.00  118
 90  \w     38.00 142.80   0.80    5.00    --  111.00 -77.00-120.00  131
 91  \w     80.00 178.40   0.80    5.00    --  111.00  77.00 -60.00  123
 92  \w     88.00 178.40   0.80    5.00    --  111.00  45.00 -30.00  113
 93  \w      6.00 122.00   0.80    2.00    --   43.17  19.00-180.00  145
 94  \w    -42.00 130.00   0.80    2.00    --   43.17   0.00-120.00  215
 95  \w     18.00 113.20   0.80    2.00    --   43.17  57.00  30.00  119
 96  \w    -42.00 130.00   0.80    2.00    --   43.17   0.00-180.00  215
 97  \w    -42.00 130.00   0.80    2.00    --   43.17   0.00-150.00  215
 98  \w     95.00 123.00   0.80    2.00    --   50.00  79.00  81.78   35
 99  \w     22.00  50.00   0.80    2.00    --   54.00  78.00  67.74   35
100  \w     28.00 132.00   0.80    2.00    --   58.00  77.00-166.11  130
101  \w     28.00 132.00   0.80    2.00    --   58.00  76.00  62.14  130
102  \w     36.00 140.00   0.80    2.00    --   66.00  77.00-161.33  130
103  \w     36.00 140.00   0.80    2.00    --   66.00  77.00 -77.61  130
104  \w     36.00 138.40   0.80    2.00    --   66.00  75.00  57.33  128
105  \w     36.00 138.40   0.80    2.00    --   66.00  75.00 -40.99  128
106  \w     36.00 138.40   0.80    2.00    --   66.00  75.00 -83.60  128
107  \w     40.00 142.40   0.80    2.00    --   70.00  75.00 -33.37  128
108  \w     40.00 144.00   0.80    2.00    --   70.00  76.00 156.11  130
109  \w     43.00 140.60   0.80    2.00    --   70.00  63.00 142.00  122
110  \w     40.00 144.00   0.80    2.00    --   70.00  76.00 -43.25  130
111  \w     40.00 144.00   0.80    2.00    --   70.00  76.00  78.96  130
112  \w     40.00 144.00   0.80    2.00    --   70.00  76.00 151.36  130
113  \w     44.00 148.00   0.80    2.00    --   74.00  77.00-152.19  130
114  \w     43.00 147.00   0.80    2.00    --   74.00  74.00  92.75  130
115  \w     47.00 144.60   0.80    2.00    --   74.00  63.00 -66.73  122
116  \w     51.00 148.60   0.80    5.00    --   78.00  62.00 127.18  122
117  \w     49.00 150.60   0.80    5.00    --   78.00  73.00-163.62  127
118  \w     53.00 153.00   0.80    5.00    --   82.00  68.00-158.34  125
119  \w     57.00 157.00   0.80    5.00    --   86.00  65.00-120.08  125
120  \w     67.00 164.60   0.80    5.00    --   94.00  61.00-175.28  122
121  \w     68.00 164.00   0.80    5.00    --   94.00  59.00 162.57  120
122  \w     69.00 169.80   0.80    5.00    --   98.00  70.00  77.30  126
123  \w     76.00 172.00   0.80    5.00    --  102.00  57.00 -56.44  120
124  \w     77.00 171.40   0.80    5.00    --  102.00  54.00  59.00  118
125  \w     37.00 134.60   0.80    5.00    --  111.00 -30.00  90.00  122
126  \w     37.00 134.60   0.80    5.00    --  111.00 -30.00  30.00  122
127  \w     37.00 134.60   0.80    5.00    --  111.00 -30.00 -60.00  122
128  \w     88.00 178.40   0.80    5.00    --  111.00  45.00  60.00  113
129  \w     39.00 133.40   0.80    5.00    --  111.00 -37.00 163.94  118
130  \w     88.00 178.40   0.80    5.00    --  111.00  30.00 150.00  113
131  \w     40.00 121.60   0.80    5.00    --  111.00-125.00 150.00  102
132  \w     88.00 178.40   0.80    5.00    --  111.00  45.00-120.00  113
133  \w     31.00 108.60   0.80    5.00    --  111.00 -94.00 150.00   97
134  \w     37.00 134.60   0.80    5.00    --  111.00 -30.00 -30.00  122
135  \w     26.00 178.80   0.80    5.00    --  111.00  -4.00-176.69  191
136  \w     30.00 178.80   0.80    5.00    --  111.00 -12.00-164.45  186
137  \w     84.00 178.40   0.80    5.00    --  111.00  61.00 -30.00  118
138  \w     32.00 156.80   0.80    5.00    --  111.00 -15.00-150.00  156
139  \w     24.00 136.80   0.80    5.00    --  111.00   0.00 120.00  141
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0054633000
_diffrn_orient_matrix_UB_12      0.0028483000
_diffrn_orient_matrix_UB_13      0.0458728000
_diffrn_orient_matrix_UB_21      0.0524255000
_diffrn_orient_matrix_UB_22      0.1229236000
_diffrn_orient_matrix_UB_23      -0.0014180000
_diffrn_orient_matrix_UB_31      -0.1624170000
_diffrn_orient_matrix_UB_32      0.0397860000
_diffrn_orient_matrix_UB_33      0.0010813000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            307438
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.367
_diffrn_reflns_theta_min         3.935
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 3264 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         7534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0520P)^2^+0.7920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.0950
_reflns_Friedel_coverage         0.772
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                7499
_reflns_number_total             7534
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01229f2.cif
_cod_data_source_block           ex16068
_cod_depositor_comments
'Adding full bibliography for 7046397--7046398.cif.'
_cod_database_code               7046398
_shelxl_version_number           2014/6
_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 Ternary CH refined with riding coordinates:
 C2(H2A)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C7(H7), C14(H14), C5(H5)
2.d Idealised Me refined as rotating group:
 C15D(H15A,H15B,H15C), C13B(H13A,H13B,H13C), C13C(H13D,H13E,H13F), C2A(H2AA,
 H2AB,H2AC), C13D(H13G,H13H,H13I), C15B(H15D,H15E,H15F), C8C(H8CA,H8CB,H8CC),
 C6B(H6BA,H6BB,H6BC), C8B(H8BA,H8BB,H8BC), C6D(H6DA,H6DB,H6DC), C8D(H8DA,H8DB,
 H8DC), C15C(H15G,H15H,H15I), C6C(H6CA,H6CB,H6CC), C2AA(H2AE,H2AF,H2AG),
 C1AA(H1AB,H1AC,H1AD)
;
_shelx_res_checksum              7847
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.414
_oxdiff_exptl_absorpt_empirical_full_min 0.710