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_7046397
_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_formula_moiety         'C108 H167 N3 O16 Ti3'
_chemical_formula_sum            'C108 H167 N3 O16 Ti3'
_chemical_formula_weight         1907.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-07-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-07-13 deposited with the CCDC.
2018-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.799(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2420(6)
_cell_length_b                   30.8848(14)
_cell_length_c                   32.6649(13)
_cell_measurement_reflns_used    9709
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      26.87
_cell_measurement_theta_min      2.34
_cell_volume                     14350.9(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            223865
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.226
_diffrn_reflns_theta_min         0.908
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0786 before and 0.0528 after correction. The Ratio of minimum to maximum transmission is 0.9010. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.883
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4120
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.223
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1232
_refine_ls_number_reflns         31655
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0695
_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^)+(0.0740P)^2^+19.8440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.1872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22417
_reflns_number_total             31655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01229f2.cif
_cod_data_source_block           test2_sq
_cod_depositor_comments
'Adding full bibliography for 7046397--7046398.cif.'
_cod_database_code               7046397
_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
 C13A-C13E \\sim C13C-C13A \\sim C13G-C13A \\sim C13B-C13A \\sim C13F-C13A
\\sim C13D-C13A
 with sigma of 0.02
 C38C-C38A \\sim C38G-C38A \\sim C38B-C38A \\sim C38F-C38A \\sim C38D-C38A
\\sim C38E-C38A
 with sigma of 0.02
 C45F-C45A \\sim C45E-C45A \\sim C45C-C45A \\sim C45B-C45A \\sim C45G-C45A
\\sim C45D-C45A
 with sigma of 0.02
 C50A-C49A \\sim C51A-C49A
 with sigma of 0.02
 C22B-C22A \\sim C22D-C22A \\sim C22C-C22A
 with sigma of 0.02
 C51B-C49B \\sim C50B-C49B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C13C) = Uanis(C13E) = Uanis(C13G) = Uanis(C13B) = Uanis(C13F) =
Uanis(C13D)
Uanis(C38C) = Uanis(C38G) = Uanis(C38B) = Uanis(C38F) = Uanis(C38D) =
Uanis(C38E)
Uanis(C45C) = Uanis(C45D) = Uanis(C45B)
Uanis(C45G) = Uanis(C45E) = Uanis(C45F)
Uanis(C51A) = Uanis(C49A) = Uanis(C50A)
Uanis(C53) = Uanis(C52) = Uanis(C54)
Uanis(C22C) = Uanis(C22F)
Uanis(C22E) = Uanis(C22B)
Uanis(C51B) = Uanis(C49B) = Uanis(C50B)
4. Others
 Sof(C13F)=Sof(H13J)=Sof(H13K)=Sof(H13L)=Sof(C13E)=Sof(H13M)=Sof(H13N)=
 Sof(H13O)=Sof(C13G)=Sof(H13P)=Sof(H13Q)=Sof(H13R)=1-FVAR(1)
 Sof(C13C)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C13D)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C13B)=Sof(H13G)=Sof(H13H)=Sof(H13I)=FVAR(1)
 Sof(C38F)=Sof(H38J)=Sof(H38K)=Sof(H38L)=Sof(C38E)=Sof(H38M)=Sof(H38N)=
 Sof(H38O)=Sof(C38G)=Sof(H38P)=Sof(H38Q)=Sof(H38R)=1-FVAR(2)
 Sof(C38C)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C38B)=Sof(H38D)=Sof(H38E)=
 Sof(H38F)=Sof(C38D)=Sof(H38G)=Sof(H38H)=Sof(H38I)=FVAR(2)
 Sof(C45F)=Sof(H45J)=Sof(H45K)=Sof(H45L)=Sof(C45E)=Sof(H45M)=Sof(H45N)=
 Sof(H45O)=Sof(C45G)=Sof(H45P)=Sof(H45Q)=Sof(H45R)=1-FVAR(3)
 Sof(C45B)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C45C)=Sof(H45D)=Sof(H45E)=
 Sof(H45F)=Sof(C45D)=Sof(H45G)=Sof(H45H)=Sof(H45I)=FVAR(3)
 Sof(C51B)=Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(C49B)=Sof(H49B)=Sof(C50B)=
 Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(4)
 Sof(C49A)=Sof(H49A)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C50A)=
 Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(4)
 Sof(C22C)=Sof(H22J)=Sof(H22K)=Sof(H22L)=1-FVAR(5)
 Sof(C22F)=Sof(H22G)=Sof(H22H)=Sof(H22I)=FVAR(5)
 Sof(C22E)=Sof(H22M)=Sof(H22N)=Sof(H22O)=1-FVAR(6)
 Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=FVAR(6)
5.a Ternary CH refined with riding coordinates:
 C58(H58), C55(H55), C52(H52), C49A(H49A), C49B(H49B)
5.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C42(H42A,H42B), C26(H26A,H26B), C10(H10A,H10B), C35(H35A,
 H35B), C18(H18A,H18B), C19(H19A,H19B), C3(H3A,H3B), C2(H2A,H2B)
5.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C39(H39), C46(H46), C37(H37), C5(H5), C44(H44), C28(H28), C7(H7),
 C30(H30), C14(H14), C21(H21), C23(H23)
5.d Idealised Me refined as rotating group:
 C15D(H15A,H15B,H15C), C40C(H40A,H40B,H40C), C40D(H40D,H40E,H40F), C29D(H29A,
 H29B,H29C), C8C(H8CA,H8CB,H8CC), C47B(H47A,H47B,H47C), C59(H59A,H59B,H59C),
 C15B(H15D,H15E,H15F), C40B(H40G,H40H,H40I), C15C(H15G,H15H,H15I), C47D(H47D,
 H47E,H47F), C29C(H29D,H29E,H29F), C47C(H47G,H47H,H47I), C31B(H31A,H31B,H31C),
 C60(H60A,H60B,H60C), C29B(H29G,H29H,H29I), C8D(H8DA,H8DB,H8DC), C31C(H31D,H31E,
 H31F), C8B(H8BA,H8BB,H8BC), C24D(H24A,H24B,H24C), C31D(H31G,H31H,H31I),
 C24C(H24D,H24E,H24F), C56(H56A,H56B,H56C), C6B(H6BA,H6BB,H6BC), C6C(H6CA,H6CB,
 H6CC), C57(H57A,H57B,H57C), C24B(H24G,H24H,H24I), C6D(H6DA,H6DB,H6DC),
 C13C(H13A,H13B,H13C), C54(H54A,H54B,H54C), C53(H53A,H53B,H53C), C13D(H13D,H13E,
 H13F), C38C(H38A,H38B,H38C), C38B(H38D,H38E,H38F), C13B(H13G,H13H,H13I),
 C38D(H38G,H38H,H38I), C38F(H38J,H38K,H38L), C38E(H38M,H38N,H38O), C38G(H38P,
 H38Q,H38R), C51A(H51A,H51B,H51C), C50A(H50A,H50B,H50C), C13F(H13J,H13K,H13L),
 C13E(H13M,H13N,H13O), C13G(H13P,H13Q,H13R), C45B(H45A,H45B,H45C), C45C(H45D,
 H45E,H45F), C45D(H45G,H45H,H45I), C45F(H45J,H45K,H45L), C45E(H45M,H45N,H45O),
 C45G(H45P,H45Q,H45R), C51B(H51D,H51E,H51F), C50B(H50D,H50E,H50F), C22D(H22A,
 H22B,H22C), C22B(H22D,H22E,H22F), C22F(H22G,H22H,H22I), C22C(H22J,H22K,H22L),
 C22E(H22M,H22N,H22O)
;
_shelx_res_checksum              5460
_shelx_fab_checksum              2290
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'