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_7040945
_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         'C64 H56 N4 O18 Ti4, 2(C2 H3 N)'
_chemical_formula_sum            'C68 H62 N6 O18 Ti4'
_chemical_formula_weight         1442.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-20
_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                85.061(2)
_cell_angle_beta                 89.175(2)
_cell_angle_gamma                86.151(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0501(4)
_cell_length_b                   12.0820(4)
_cell_length_c                   23.2457(8)
_cell_measurement_reflns_used    9611
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.59
_cell_measurement_theta_min      2.53
_cell_volume                     3364.0(2)
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_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
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            57801
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         33.668
_diffrn_reflns_theta_min         2.154
_diffrn_source                   'Advanced Light Source station 11.3.1'
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  0.8624
_exptl_absorpt_correction_T_min  0.7781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0637 before and 0.0473 after correction.
The Ratio of minimum to maximum transmission is 0.9022.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         20585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0460P)^2^+2.2600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1185
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14514
_reflns_number_total             20585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03842e2.cif
_cod_data_source_block           1ti_a1b2_c5_a_sq
_cod_depositor_comments
'Adding full bibliography for 7040945--7040948.cif.'
_cod_database_code               7040945
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.936
_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 Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C34(H34A,H34B), C50(H50A,H50B), C42(H42A,H42B), C10(H10A,H10B),
 C26(H26A,H26B), C35(H35A,H35B), C3(H3A,H3B), C18(H18A,H18B), C58(H58A,H58B),
 C51(H51A,H51B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C45(H45), C46(H46), C44(H44), C47(H47), C24(H24), C23(H23), C12(H12),
 C31(H31), C5(H5), C14(H14), C7(H7), C30(H30), C56(H56), C21(H21), C6(H6),
 C53(H53), C22(H22), C28(H28), C13(H13), C15(H15), C55(H55), C29(H29), C40(H40),
  C63(H63), C54(H54), C37(H37), C39(H39), C38(H38), C60(H60), C62(H62), C61(H61)
2.c Idealised Me refined as rotating group:
 C1AA(H1AA,H1AB,H1AC), C1BA(H1BA,H1BB,H1BC)
;
_shelx_res_checksum              8933
_shelx_fab_checksum              29098
_olex2_submission_special_instructions 'No special instructions were received'