#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:03:15 +0100 (vie 25 de mar de 2016) $
#$Revision: 179738 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/34/7003469.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7003469
loop_
_publ_author_name
'Chmura, Amanda J.'
'Cousins, David M.'
'Davidson, Matthew G.'
'Jones, Matthew D.'
'Lunn, Matthew D.'
'Mahon, Mary F.'
_publ_section_title
;
 Robust chiral zirconium alkoxide initiators for the room-temperature
 stereoselective ring-opening polymerisation of rac-lactide
;
_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              1437
_journal_page_last               1443
_journal_paper_doi               10.1039/b716304e
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_sum            'C38 H46 N2 O6 Ti'
_chemical_formula_weight         674.67
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000
_cell_angle_beta                 122.9800(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   19.9450(2)
_cell_length_b                   9.4060(2)
_cell_length_c                   11.1810(2)
_cell_measurement_reflns_used    12553
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.51
_cell_volume                     1759.58(6)
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo & Scalepack (Otwinski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
(1999) J. Appl. Cryst. 32, 115-119.
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'nonius kappa ccd'
_diffrn_measurement_method       ccd
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15092
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.76
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Nonius Kappa CCD'
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       yellow
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3973
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0506P)²+0.6639P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                3658
_reflns_number_total             3973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b716304e.txt
_cod_data_source_block           (R2)2Ti(OiPr)2
_cod_original_cell_volume        1759.58(5)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7003469
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.5000 0.70257(4) 1.0000 0.02062(12) Uani 1 2 d S . .
O2 O 0.45025(8) 0.58062(15) 0.84958(14) 0.0275(3) Uani 1 1 d . . .
N1 N 0.44327(10) 0.88267(18) 0.83050(16) 0.0224(3) Uani 1 1 d . . .
C1 C 0.37466(17) 0.5083(3) 0.7811(3) 0.0452(6) Uani 1 1 d . . .
H1 H 0.3401 0.5671 0.8012 0.054 Uiso 1 1 calc R . .
H11 H 0.3493(14) 0.995(3) 0.696(2) 0.031(6) Uiso 1 1 d . . .
O1 O 0.40780(7) 0.73388(14) 1.00599(12) 0.0238(3) Uani 1 1 d . . .
C2 C 0.38364(16) 0.3696(3) 0.8506(3) 0.0547(7) Uani 1 1 d . . .
H2A H 0.4142 0.3048 0.8292 0.082 Uiso 1 1 calc R . .
H2B H 0.3307 0.3290 0.8148 0.082 Uiso 1 1 calc R . .
H2C H 0.4119 0.3830 0.9540 0.082 Uiso 1 1 calc R . .
O3 O 0.11835(9) 1.01474(17) 0.70746(18) 0.0382(4) Uani 1 1 d . . .
C3 C 0.33503(17) 0.5080(4) 0.6272(3) 0.0646(9) Uani 1 1 d . . .
H3A H 0.3233 0.6060 0.5917 0.097 Uiso 1 1 calc R . .
H3B H 0.2851 0.4540 0.5843 0.097 Uiso 1 1 calc R . .
H3C H 0.3700 0.4637 0.6015 0.097 Uiso 1 1 calc R . .
C4 C 0.33807(11) 0.8029(2) 0.93504(19) 0.0220(4) Uani 1 1 d . . .
C5 C 0.28183(11) 0.7810(2) 0.9712(2) 0.0252(4) Uani 1 1 d . . .
H5 H 0.2940 0.7173 1.0464 0.030 Uiso 1 1 calc R . .
C6 C 0.20845(12) 0.8505(2) 0.8994(2) 0.0264(4) Uani 1 1 d . . .
H6 H 0.1711 0.8340 0.9256 0.032 Uiso 1 1 calc R . .
C7 C 0.18986(11) 0.9441(2) 0.7896(2) 0.0270(4) Uani 1 1 d . . .
C8 C 0.24550(11) 0.9690(2) 0.7538(2) 0.0256(4) Uani 1 1 d . . .
H8 H 0.2332 1.0345 0.6799 0.031 Uiso 1 1 calc R . .
C9 C 0.31934(11) 0.8993(2) 0.82486(19) 0.0226(4) Uani 1 1 d . . .
C10 C 0.05620(14) 0.9797(3) 0.7273(3) 0.0490(6) Uani 1 1 d . . .
H10A H 0.0469 0.8769 0.7164 0.074 Uiso 1 1 calc R . .
H10B H 0.0072 1.0295 0.6562 0.074 Uiso 1 1 calc R . .
H10C H 0.0713 1.0085 0.8232 0.074 Uiso 1 1 calc R . .
C11 C 0.37282(12) 0.9311(2) 0.7778(2) 0.0241(4) Uani 1 1 d . . .
C12 C 0.48785(11) 0.9363(2) 0.7652(2) 0.0256(4) Uani 1 1 d . . .
H12 H 0.5274 0.8611 0.7815 0.031 Uiso 1 1 calc R . .
C13 C 0.53565(13) 1.0672(2) 0.8472(2) 0.0342(5) Uani 1 1 d . . .
H13A H 0.4990 1.1425 0.8374 0.051 Uiso 1 1 calc R . .
H13B H 0.5669 1.1004 0.8089 0.051 Uiso 1 1 calc R . .
H13C H 0.5718 1.0429 0.9482 0.051 Uiso 1 1 calc R . .
C14 C 0.43404(11) 0.9581(2) 0.6045(2) 0.0239(4) Uani 1 1 d . . .
C15 C 0.40599(14) 1.0910(2) 0.5423(2) 0.0356(5) Uani 1 1 d . . .
H15 H 0.4201 1.1729 0.6010 0.043 Uiso 1 1 calc R . .
C16 C 0.35734(15) 1.1048(3) 0.3947(2) 0.0421(6) Uani 1 1 d . . .
H16 H 0.3377 1.1959 0.3535 0.051 Uiso 1 1 calc R . .
C17 C 0.33762(14) 0.9880(3) 0.3084(2) 0.0368(5) Uani 1 1 d . . .
H17 H 0.3049 0.9982 0.2077 0.044 Uiso 1 1 calc R . .
C18 C 0.36522(14) 0.8565(2) 0.3678(2) 0.0377(5) Uani 1 1 d . . .
H18 H 0.3516 0.7752 0.3085 0.045 Uiso 1 1 calc R . .
C19 C 0.41318(13) 0.8422(2) 0.5151(2) 0.0331(5) Uani 1 1 d . . .
H19 H 0.4321 0.7506 0.5553 0.040 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ti1 O2 101.86(9) . 2_657 ?
O2 Ti1 O1 94.53(6) . . ?
O2 Ti1 O1 96.69(6) 2_657 . ?
O2 Ti1 O1 96.69(6) . 2_657 ?
O2 Ti1 O1 94.53(6) 2_657 2_657 ?
O1 Ti1 O1 162.16(8) . 2_657 ?
O2 Ti1 N1 172.30(6) . 2_657 ?
O2 Ti1 N1 85.83(6) 2_657 2_657 ?
O1 Ti1 N1 84.79(5) . 2_657 ?
O1 Ti1 N1 82.23(5) 2_657 2_657 ?
O2 Ti1 N1 85.83(6) . . ?
O2 Ti1 N1 172.30(6) 2_657 . ?
O1 Ti1 N1 82.23(5) . . ?
O1 Ti1 N1 84.79(5) 2_657 . ?
N1 Ti1 N1 86.48(8) 2_657 . ?
C1 O2 Ti1 132.60(15) . . ?
C11 N1 C12 116.58(16) . . ?
C11 N1 Ti1 124.15(13) . . ?
C12 N1 Ti1 118.93(11) . . ?
O2 C1 C3 111.7(2) . . ?
O2 C1 C2 110.2(2) . . ?
C3 C1 C2 117.0(3) . . ?
O2 C1 H1 105.7 . . ?
C3 C1 H1 105.7 . . ?
C2 C1 H1 105.7 . . ?
C4 O1 Ti1 140.32(11) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C7 O3 C10 117.53(17) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O1 C4 C5 119.76(16) . . ?
O1 C4 C9 121.84(16) . . ?
C5 C4 C9 118.39(17) . . ?
C6 C5 C4 121.43(18) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C7 C6 C5 119.93(17) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
O3 C7 C6 125.27(17) . . ?
O3 C7 C8 115.28(18) . . ?
C6 C7 C8 119.44(18) . . ?
C7 C8 C9 121.12(18) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C8 C9 C4 119.67(16) . . ?
C8 C9 C11 116.81(17) . . ?
C4 C9 C11 123.51(17) . . ?
O3 C10 H10A 109.5 . . ?
O3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C9 126.87(18) . . ?
N1 C11 H11 119.9(13) . . ?
C9 C11 H11 113.2(13) . . ?
N1 C12 C13 108.61(15) . . ?
N1 C12 C14 113.11(15) . . ?
C13 C12 C14 114.22(16) . . ?
N1 C12 H12 106.8 . . ?
C13 C12 H12 106.8 . . ?
C14 C12 H12 106.8 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C19 C14 C15 117.85(18) . . ?
C19 C14 C12 119.25(17) . . ?
C15 C14 C12 122.89(18) . . ?
C14 C15 C16 120.5(2) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C17 C16 C15 120.5(2) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C18 C17 C16 119.8(2) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C17 C18 C19 119.9(2) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C14 C19 C18 121.6(2) . . ?
C14 C19 H19 119.2 . . ?
C18 C19 H19 119.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O2 1.8200(14) . ?
Ti1 O2 1.8200(14) 2_657 ?
Ti1 O1 1.8991(12) . ?
Ti1 O1 1.8991(12) 2_657 ?
Ti1 N1 2.3253(17) 2_657 ?
Ti1 N1 2.3253(16) . ?
O2 C1 1.437(3) . ?
N1 C11 1.276(3) . ?
N1 C12 1.512(2) . ?
C1 C3 1.451(3) . ?
C1 C2 1.479(4) . ?
C1 H1 1.0000 . ?
O1 C4 1.336(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
O3 C7 1.376(2) . ?
O3 C10 1.412(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.399(2) . ?
C4 C9 1.407(3) . ?
C5 C6 1.391(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.388(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.389(3) . ?
C8 C9 1.399(3) . ?
C8 H8 0.9500 . ?
C9 C11 1.454(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11 0.98(2) . ?
C12 C13 1.521(3) . ?
C12 C14 1.524(2) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C19 1.381(3) . ?
C14 C15 1.391(3) . ?
C15 C16 1.393(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.372(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.370(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.389(3) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
