Well-defined Ti4 pre-catalysts for the ring-opening polymerisation of lactide.
Cols, Jean-Marie E P; Taylor, Cameron E.; Gagnon, Kevin J.; Teat, Simon J.; McIntosh, Ruaraidh D.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 17729–17738; doi:10.1039/c6dt03842e

data_7040947
_publ_section_title
;
 Well-defined Ti4 pre-catalysts for the ring-opening polymerisation of
 lactide.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17729
_journal_page_last               17738
_journal_paper_doi               10.1039/c6dt03842e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C96 H120 N4 O18 Ti4, 12(C7 H8)'
_chemical_formula_sum            'C180 H216 N4 O18 Ti4'
_chemical_formula_weight         2915.16
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-06 deposited with the CCDC.
2016-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.5294(8)
_cell_length_b                   19.5294(8)
_cell_length_c                   20.7148(9)
_cell_measurement_reflns_used    9816
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.87
_cell_measurement_theta_min      2.46
_cell_volume                     7900.6(6)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2 v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57486
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.142
_diffrn_reflns_theta_min         2.458
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0707 before and 0.0563 after correction.
The Ratio of minimum to maximum transmission is 0.8645.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 3339 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         8746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0550P)^2^+4.4970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1036
_reflns_Friedel_coverage         0.940
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                7467
_reflns_number_total             8746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03842e2.cif
_cod_data_source_block           final
_cod_depositor_comments
'Adding full bibliography for 7040945--7040948.cif.'
_cod_original_cell_volume        7900.6(7)
_cod_database_code               7040947
_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. Uiso/Uaniso restraints and constraints
Uanis(C4CB) = Uanis(C3CB) = Uanis(C1CB) = Uanis(C2CB) = Uanis(C7CB) =
Uanis(C6CB) = Uanis(C5CB)
3. Others
 Sof(C1BA)=Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C2BA)=Sof(C7BA)=Sof(H7BA)=
 Sof(C6BA)=Sof(H6BE)=Sof(C5BA)=Sof(H5BA)=Sof(C4BA)=Sof(H4BA)=Sof(C3BA)=
 Sof(H3BA)=1-FVAR(1)
 Sof(C1BB)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C2BB)=Sof(C7BB)=Sof(H7BB)=
 Sof(C6BB)=Sof(H6BD)=Sof(C5BB)=Sof(H5BB)=Sof(C4BB)=Sof(H4BB)=Sof(C3BB)=
 Sof(H3BB)=FVAR(1)
 Sof(C1CB)=Sof(H1CD)=Sof(H1CE)=Sof(H1CF)=Sof(C2CB)=Sof(C7CB)=Sof(H7CB)=
 Sof(C6CB)=Sof(H6CE)=Sof(C5CB)=Sof(H5CB)=Sof(C4CB)=Sof(H4CB)=Sof(C3CB)=
 Sof(H3CB)=1-FVAR(2)
 Sof(C1CA)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=Sof(C4CA)=Sof(H4CA)=Sof(C3CA)=
 Sof(H3CA)=Sof(C8CA)=Sof(C7CA)=Sof(H7CA)=Sof(C6CA)=Sof(H6CD)=Sof(C5CA)=
 Sof(H5CA)=FVAR(2)
4.a Free rotating group:
 C1BB(C2BB,C7BB,C6BB,C5BB,C4BB,C3BB), C1BA(C2BA,C7BA,C6BA,C5BA,C4BA,C3BA,C5,C6,
 C6A,C6D,C6C,C6B), C1CA(C4CA,C3CA,C8CA,C7CA,C6CA,C5CA), C1CB(C2CB,C7CB,C6CB,
 C5CB,C4CB,C3CB)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C10(H10A,H10B)
4.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C8(H8), C7(H7), C15(H15), C14(H14), C7AA(H7AA), C3AA(H3AA),
 C4AA(H4AA), C5AA(H5AA), C6AA(H6AA), C7BB(H7BB), C6BB(H6BD), C5BB(H5BB),
 C4BB(H4BB), C3BB(H3BB), C7BA(H7BA), C6BA(H6BE), C5BA(H5BA), C4BA(H4BA),
 C3BA(H3BA), C5(H5), C4CA(H4CA), C3CA(H3CA), C7CA(H7CA), C6CA(H6CD), C5CA(H5CA),
  C7CB(H7CB), C6CB(H6CE), C5CB(H5CB), C4CB(H4CB), C3CB(H3CB)
4.d Idealised Me refined as rotating group:
 C13C(H13A,H13B,H13C), C13D(H13D,H13E,H13F), C13B(H13G,H13H,H13I), C1AA(H1AA,
 H1AB,H1AC), C1BB(H1BA,H1BB,H1BC), C1BA(H1BD,H1BE,H1BF), C6D(H6DA,H6DB,H6DC),
 C6C(H6CA,H6CB,H6CC), C6B(H6BA,H6BB,H6BC), C1CA(H1CA,H1CB,H1CC), C1CB(H1CD,H1CE,
 H1CF)
;
_shelx_res_checksum              52877
_olex2_submission_special_instructions 'No special instructions were received'