#------------------------------------------------------------------------------
#$Date: 2021-09-06 15:39:59 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268962 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/35/1563536.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_1563536
loop_
_publ_author_name
'Roymuhury, Sagnik K.'
'Mandal, Mrinmay'
'Chakraborty, Debashis'
'Ramkumar, Venkatachalam'
_publ_section_title
;
 Homoleptic titanium and zirconium complexes exhibiting unusual
 Oiminol--metal coordination: application in stereoselective ring-opening
 polymerization of lactide
;
_journal_issue                   27
_journal_name_full               'Polymer Chemistry'
_journal_page_first              3953
_journal_page_last               3967
_journal_paper_doi               10.1039/D1PY00237F
_journal_volume                  12
_journal_year                    2021
_chemical_formula_sum            'C19 H26 N2 O3 S2'
_chemical_formula_weight         394.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-18 deposited with the CCDC.	2021-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                98.4485(11)
_cell_angle_beta                 94.8760(11)
_cell_angle_gamma                94.1161(12)
_cell_formula_units_Z            2
_cell_length_a                   9.8710(3)
_cell_length_b                   9.8841(3)
_cell_length_c                   10.9592(3)
_cell_measurement_reflns_used    8999
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.08
_cell_measurement_theta_min      2.59
_cell_volume                     1049.96(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15632
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.887
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       BLock
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.130
_refine_diff_density_max         2.190
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0743
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1191P)²+1.3564P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2076
_refine_ls_wR_factor_ref         0.2207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3160
_reflns_number_total             3699
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1py00237f2.cif
_cod_data_source_block           Ligand_2
_cod_depositor_comments
'Adding full bibliography for 1563535--1563538.cif.'
_cod_original_cell_volume        1049.95(5)
_cod_database_code               1563536
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.910
_shelx_estimated_absorpt_t_max   0.965
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.3350(3) 0.4601(4) 0.5850(3) 0.0457(7) Uani 1 1 d . . . . .
H1 H -0.3060 0.3779 0.5476 0.055 Uiso 1 1 calc R U . . .
C2 C -0.4325(4) 0.4702(5) 0.6720(4) 0.0636(10) Uani 1 1 d . . . . .
H2 H -0.4750 0.3943 0.6988 0.076 Uiso 1 1 calc R U . . .
C3 C -0.4577(5) 0.5970(6) 0.7117(4) 0.0806(13) Uani 1 1 d . . . . .
H3 H -0.5205 0.6197 0.7683 0.097 Uiso 1 1 calc R U . . .
C4 C -0.2884(3) 0.5886(3) 0.5626(3) 0.0405(7) Uani 1 1 d . . . . .
C5 C -0.1903(3) 0.6332(3) 0.4795(3) 0.0429(7) Uani 1 1 d . . . . .
C6 C -0.0025(3) 0.4760(3) 0.2511(3) 0.0407(7) Uani 1 1 d . . . . .
H6 H -0.0310 0.3843 0.2515 0.049 Uiso 1 1 calc R U . . .
C7 C 0.0922(3) 0.5113(3) 0.1644(3) 0.0367(6) Uani 1 1 d . . . . .
C8 C 0.1369(3) 0.6490(3) 0.1584(3) 0.0364(6) Uani 1 1 d . . . . .
C9 C 0.2247(3) 0.6806(3) 0.0710(3) 0.0360(6) Uani 1 1 d . . . . .
C10 C 0.2671(3) 0.5711(3) -0.0074(3) 0.0405(7) Uani 1 1 d . . . . .
H10 H 0.3253 0.5907 -0.0661 0.049 Uiso 1 1 calc R U . . .
C11 C 0.2275(3) 0.4343(3) -0.0029(3) 0.0417(7) Uani 1 1 d . . . . .
C12 C 0.1392(3) 0.4068(3) 0.0826(3) 0.0399(7) Uani 1 1 d . . . . .
H12 H 0.1100 0.3160 0.0861 0.048 Uiso 1 1 calc R U . . .
C13 C 0.2713(3) 0.8306(3) 0.0621(3) 0.0441(7) Uani 1 1 d . . . . .
C14 C 0.1477(4) 0.9113(4) 0.0367(4) 0.0633(10) Uani 1 1 d . . . . .
H14A H 0.1778 1.0062 0.0386 0.095 Uiso 1 1 calc R U . . .
H14B H 0.0861 0.9033 0.0990 0.095 Uiso 1 1 calc R U . . .
H14C H 0.1018 0.8748 -0.0434 0.095 Uiso 1 1 calc R U . . .
C15 C 0.3562(5) 0.8974(4) 0.1828(4) 0.0681(11) Uani 1 1 d . . . . .
H15A H 0.4331 0.8458 0.1973 0.102 Uiso 1 1 calc R U . . .
H15B H 0.3008 0.8985 0.2507 0.102 Uiso 1 1 calc R U . . .
H15C H 0.3878 0.9898 0.1756 0.102 Uiso 1 1 calc R U . . .
C16 C 0.3611(4) 0.8412(4) -0.0439(4) 0.0582(9) Uani 1 1 d . . . . .
H16A H 0.4430 0.7970 -0.0288 0.087 Uiso 1 1 calc R U . . .
H16B H 0.3842 0.9362 -0.0488 0.087 Uiso 1 1 calc R U . . .
H16C H 0.3123 0.7972 -0.1206 0.087 Uiso 1 1 calc R U . . .
C17 C 0.2768(4) 0.3204(4) -0.0922(4) 0.0629(10) Uani 1 1 d . . . . .
H17A H 0.2767 0.2379 -0.0555 0.094 Uiso 1 1 calc R U . . .
H17B H 0.3678 0.3467 -0.1099 0.094 Uiso 1 1 calc R U . . .
H17C H 0.2172 0.3043 -0.1677 0.094 Uiso 1 1 calc R U . . .
C18 C 0.3237(6) 0.9763(6) 0.5929(8) 0.121(3) Uani 1 1 d . . . . .
H18A H 0.3544 0.9945 0.6797 0.181 Uiso 1 1 calc R U . . .
H18B H 0.3113 1.0614 0.5627 0.181 Uiso 1 1 calc R U . . .
H18C H 0.3905 0.9289 0.5487 0.181 Uiso 1 1 calc R U . . .
C19 C 0.0724(5) 0.9771(4) 0.6682(4) 0.0743(12) Uani 1 1 d . . . . .
H19A H -0.0194 0.9358 0.6623 0.111 Uiso 1 1 calc R U . . .
H19B H 0.0716 1.0664 0.6437 0.111 Uiso 1 1 calc R U . . .
H19C H 0.1126 0.9856 0.7522 0.111 Uiso 1 1 calc R U . . .
N1 N -0.1386(3) 0.5324(3) 0.4059(3) 0.0428(6) Uani 1 1 d . . . . .
N2 N -0.0474(3) 0.5690(3) 0.3268(2) 0.0421(6) Uani 1 1 d . . . . .
O1 O -0.1605(3) 0.7549(2) 0.4771(3) 0.0682(8) Uani 1 1 d . . . . .
O2 O 0.0958(3) 0.7529(3) 0.2377(2) 0.0540(7) Uani 1 1 d . . . . .
O3 O 0.1975(4) 0.7523(3) 0.6355(3) 0.0766(9) Uani 1 1 d . . . . .
S1 S -0.36471(14) 0.71435(12) 0.64961(12) 0.0804(4) Uani 1 1 d . . . . .
S2 S 0.16814(11) 0.87402(9) 0.57041(9) 0.0596(3) Uani 1 1 d . . . . .
H1N H -0.156(4) 0.463(4) 0.405(3) 0.036(10) Uiso 1 1 d . . . . .
H2O H 0.053(4) 0.725(4) 0.270(4) 0.046(12) Uiso 1 1 d . . . . .
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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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
C4 C1 C2 111.0(3) . . ?
C4 C1 H1 124.5 . . ?
C2 C1 H1 124.5 . . ?
C3 C2 C1 113.6(4) . . ?
C3 C2 H2 123.2 . . ?
C1 C2 H2 123.2 . . ?
C2 C3 S1 113.2(3) . . ?
C2 C3 H3 123.4 . . ?
S1 C3 H3 123.4 . . ?
C1 C4 C5 132.2(3) . . ?
C1 C4 S1 110.8(2) . . ?
C5 C4 S1 117.0(2) . . ?
O1 C5 N1 122.8(3) . . ?
O1 C5 C4 121.2(3) . . ?
N1 C5 C4 116.0(3) . . ?
N2 C6 C7 120.9(3) . . ?
N2 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C12 C7 C8 118.8(3) . . ?
C12 C7 C6 119.4(3) . . ?
C8 C7 C6 121.9(3) . . ?
O2 C8 C9 118.7(3) . . ?
O2 C8 C7 120.5(3) . . ?
C9 C8 C7 120.8(3) . . ?
C10 C9 C8 117.2(3) . . ?
C10 C9 C13 121.8(3) . . ?
C8 C9 C13 121.0(3) . . ?
C11 C10 C9 123.8(3) . . ?
C11 C10 H10 118.1 . . ?
C9 C10 H10 118.1 . . ?
C12 C11 C10 117.6(3) . . ?
C12 C11 C17 121.5(3) . . ?
C10 C11 C17 120.8(3) . . ?
C11 C12 C7 121.9(3) . . ?
C11 C12 H12 119.1 . . ?
C7 C12 H12 119.1 . . ?
C16 C13 C14 106.7(3) . . ?
C16 C13 C15 107.2(3) . . ?
C14 C13 C15 110.5(3) . . ?
C16 C13 C9 112.1(3) . . ?
C14 C13 C9 110.5(3) . . ?
C15 C13 C9 109.8(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C11 C17 H17A 109.5 . . ?
C11 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C11 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
S2 C18 H18A 109.5 . . ?
S2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
S2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
S2 C19 H19A 109.5 . . ?
S2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
S2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C5 N1 N2 118.1(3) . . ?
C5 N1 H1N 124(3) . . ?
N2 N1 H1N 118(3) . . ?
C6 N2 N1 119.4(3) . . ?
C8 O2 H2O 106(4) . . ?
C3 S1 C4 91.5(2) . . ?
O3 S2 C19 105.79(19) . . ?
O3 S2 C18 104.0(2) . . ?
C19 S2 C18 99.7(3) . . ?
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
C1 C4 1.383(5) . ?
C1 C2 1.410(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.313(7) . ?
C2 H2 0.9300 . ?
C3 S1 1.684(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.472(4) . ?
C4 S1 1.712(3) . ?
C5 O1 1.223(4) . ?
C5 N1 1.345(4) . ?
C6 N2 1.275(4) . ?
C6 C7 1.449(4) . ?
C6 H6 0.9300 . ?
C7 C12 1.398(4) . ?
C7 C8 1.413(4) . ?
C8 O2 1.354(4) . ?
C8 C9 1.399(4) . ?
C9 C10 1.391(4) . ?
C9 C13 1.540(4) . ?
C10 C11 1.389(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.375(4) . ?
C11 C17 1.516(5) . ?
C12 H12 0.9300 . ?
C13 C16 1.531(4) . ?
C13 C14 1.532(5) . ?
C13 C15 1.537(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 S2 1.755(5) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 S2 1.752(4) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
N1 N2 1.368(4) . ?
N1 H1N 0.69(4) . ?
O2 H2O 0.65(4) . ?
O3 S2 1.519(3) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 C1 C2 C3 0.3(5) . . . . ?
C1 C2 C3 S1 -0.9(5) . . . . ?
C2 C1 C4 C5 -178.6(3) . . . . ?
C2 C1 C4 S1 0.5(4) . . . . ?
C1 C4 C5 O1 -177.8(3) . . . . ?
S1 C4 C5 O1 3.1(4) . . . . ?
C1 C4 C5 N1 3.5(5) . . . . ?
S1 C4 C5 N1 -175.6(2) . . . . ?
N2 C6 C7 C12 -180.0(3) . . . . ?
N2 C6 C7 C8 -1.0(5) . . . . ?
C12 C7 C8 O2 -178.6(3) . . . . ?
C6 C7 C8 O2 2.4(4) . . . . ?
C12 C7 C8 C9 1.2(4) . . . . ?
C6 C7 C8 C9 -177.8(3) . . . . ?
O2 C8 C9 C10 178.7(3) . . . . ?
C7 C8 C9 C10 -1.1(4) . . . . ?
O2 C8 C9 C13 -1.6(4) . . . . ?
C7 C8 C9 C13 178.6(3) . . . . ?
C8 C9 C10 C11 -0.2(4) . . . . ?
C13 C9 C10 C11 -179.8(3) . . . . ?
C9 C10 C11 C12 1.3(5) . . . . ?
C9 C10 C11 C17 179.5(3) . . . . ?
C10 C11 C12 C7 -1.2(5) . . . . ?
C17 C11 C12 C7 -179.3(3) . . . . ?
C8 C7 C12 C11 0.0(4) . . . . ?
C6 C7 C12 C11 179.0(3) . . . . ?
C10 C9 C13 C16 2.5(4) . . . . ?
C8 C9 C13 C16 -177.2(3) . . . . ?
C10 C9 C13 C14 121.3(3) . . . . ?
C8 C9 C13 C14 -58.3(4) . . . . ?
C10 C9 C13 C15 -116.6(3) . . . . ?
C8 C9 C13 C15 63.8(4) . . . . ?
O1 C5 N1 N2 1.1(5) . . . . ?
C4 C5 N1 N2 179.8(3) . . . . ?
C7 C6 N2 N1 178.8(3) . . . . ?
C5 N1 N2 C6 -176.1(3) . . . . ?
C2 C3 S1 C4 1.0(4) . . . . ?
C1 C4 S1 C3 -0.8(3) . . . . ?
C5 C4 S1 C3 178.4(3) . . . . ?
