#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/02/7000299.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_7000299
loop_
_publ_author_name
'Lee, Young Hoon'
'Harrowfield, Jack'
'Kim, Yang'
'Lim, Woo Taik'
'Park, Yu Cheol'
'Thuéry, Pierre'
_publ_section_title
;
 Functionalised azetidines as ligands: pyridyl-complemented
 coordination
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              434
_journal_page_last               442
_journal_paper_doi               10.1039/b812295d
_journal_year                    2009
_chemical_formula_sum            'C21 H21 N O6 S2'
_chemical_formula_weight         447.51
_chemical_name_systematic
;
?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.361(3)
_cell_length_b                   5.9990(12)
_cell_length_c                   22.999(5)
_cell_measurement_reflns_used    7893
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.26
_cell_measurement_theta_min      2.87
_cell_volume                     2119.4(8)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'ADSC Quantum 210'
_diffrn_measurement_method       'two φ and two ω scans with 2° steps'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Sybchrotron Radiation'
_diffrn_radiation_type           'Synchrotron Radiation'
_diffrn_radiation_wavelength     0.76999
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7385
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.26
_diffrn_reflns_theta_min         2.87
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(8)
_refine_ls_extinction_coef       0.026(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4351
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0490
_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)+(0.0921P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                3650
_reflns_number_total             4351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b812295d.txt
_cod_data_source_block           yk0633
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2119.4(7)
_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               7000299
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'
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
S1 S 0.60706(5) 0.06480(12) 0.26590(4) 0.0436(2) Uani 1 1 d . . .
S2 S 0.33142(5) 0.20754(13) 0.43511(3) 0.0458(2) Uani 1 1 d . . .
O1 O 0.66851(15) 0.2004(5) 0.29533(13) 0.0613(7) Uani 1 1 d . . .
O2 O 0.61002(17) -0.1708(4) 0.27312(13) 0.0612(7) Uani 1 1 d . . .
O3 O 0.51297(13) 0.1328(3) 0.28549(9) 0.0408(5) Uani 1 1 d . . .
O4 O 0.36652(16) 0.3419(4) 0.38171(10) 0.0489(5) Uani 1 1 d . . .
O5 O 0.37211(19) 0.3149(5) 0.48310(10) 0.0664(7) Uani 1 1 d . . .
O6 O 0.34298(17) -0.0259(4) 0.42536(12) 0.0607(7) Uani 1 1 d . . .
N1 N 0.3269(2) 0.1685(6) 0.20226(16) 0.0674(9) Uani 1 1 d . . .
C1 C 0.6482(2) 0.3282(6) 0.17277(18) 0.0553(8) Uani 1 1 d . . .
H1 H 0.6717 0.4290 0.1992 0.066 Uiso 1 1 calc R . .
C2 C 0.6505(3) 0.3696(8) 0.1133(2) 0.0740(12) Uani 1 1 d . . .
H2 H 0.6758 0.4998 0.0994 0.089 Uiso 1 1 calc R . .
C3 C 0.6155(3) 0.2195(9) 0.07538(19) 0.0801(14) Uani 1 1 d . . .
H3 H 0.6175 0.2500 0.0358 0.096 Uiso 1 1 calc R . .
C4 C 0.5777(3) 0.0255(8) 0.09374(19) 0.0771(12) Uani 1 1 d . . .
H4 H 0.5550 -0.0747 0.0669 0.092 Uiso 1 1 calc R . .
C5 C 0.5733(3) -0.0205(7) 0.15304(17) 0.0611(9) Uani 1 1 d . . .
H5 H 0.5466 -0.1499 0.1664 0.073 Uiso 1 1 calc R . .
C6 C 0.6093(2) 0.1292(5) 0.19152(15) 0.0471(7) Uani 1 1 d . . .
C7 C 0.49465(19) 0.3712(4) 0.29210(14) 0.0400(6) Uani 1 1 d . . .
H7A H 0.5289 0.4565 0.2645 0.048 Uiso 1 1 calc R . .
H7B H 0.5098 0.4198 0.3310 0.048 Uiso 1 1 calc R . .
C8 C 0.39773(18) 0.4087(4) 0.28112(12) 0.0377(7) Uani 1 1 d . . .
C9 C 0.3811(2) 0.6584(5) 0.29134(19) 0.0535(8) Uani 1 1 d . . .
H9A H 0.3943 0.6950 0.3310 0.080 Uiso 1 1 calc R . .
H9B H 0.3211 0.6916 0.2835 0.080 Uiso 1 1 calc R . .
H9C H 0.4175 0.7444 0.2659 0.080 Uiso 1 1 calc R . .
C10 C 0.3774(2) 0.3473(5) 0.21791(14) 0.0412(6) Uani 1 1 d . . .
C11 C 0.4176(2) 0.4756(5) 0.17839(14) 0.0478(7) Uani 1 1 d . . .
H11 H 0.4528 0.5940 0.1896 0.057 Uiso 1 1 calc R . .
C12 C 0.4050(3) 0.4269(8) 0.12226(18) 0.0729(12) Uani 1 1 d . . .
H12 H 0.4316 0.5175 0.0946 0.087 Uiso 1 1 calc R . .
C13 C 0.3554(3) 0.2515(8) 0.10283(18) 0.0714(11) Uani 1 1 d . . .
H13 H 0.3487 0.2238 0.0633 0.086 Uiso 1 1 calc R . .
C14 C 0.3160(3) 0.1182(8) 0.14371(18) 0.0678(10) Uani 1 1 d . . .
H14 H 0.2826 -0.0035 0.1324 0.081 Uiso 1 1 calc R . .
C15 C 0.3425(2) 0.2709(5) 0.32218(14) 0.0428(6) Uani 1 1 d . . .
H15A H 0.2811 0.2975 0.3151 0.051 Uiso 1 1 calc R . .
H15B H 0.3542 0.1133 0.3169 0.051 Uiso 1 1 calc R . .
C16 C 0.2195(2) 0.2664(5) 0.43634(15) 0.0449(6) Uani 1 1 d . . .
C17 C 0.1922(3) 0.4726(6) 0.45527(18) 0.0644(10) Uani 1 1 d . . .
H17 H 0.2322 0.5816 0.4660 0.077 Uiso 1 1 calc R . .
C18 C 0.1031(3) 0.5134(9) 0.4580(2) 0.0815(14) Uani 1 1 d . . .
H18 H 0.0829 0.6519 0.4701 0.098 Uiso 1 1 calc R . .
C19 C 0.0448(3) 0.3493(8) 0.44259(19) 0.0748(12) Uani 1 1 d . . .
H19 H -0.0146 0.3778 0.4447 0.090 Uiso 1 1 calc R . .
C20 C 0.0731(3) 0.1454(8) 0.4243(2) 0.0769(12) Uani 1 1 d . . .
H20 H 0.0331 0.0360 0.4139 0.092 Uiso 1 1 calc R . .
C21 C 0.1617(2) 0.1018(7) 0.42123(17) 0.0589(9) Uani 1 1 d . . .
H21 H 0.1816 -0.0370 0.4091 0.071 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'
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'
H H 0.0000 0.0000 '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
O1 S1 O2 119.51(16) . . ?
O1 S1 O3 109.10(14) . . ?
O2 S1 O3 104.73(13) . . ?
O1 S1 C6 109.02(17) . . ?
O2 S1 C6 109.37(16) . . ?
O3 S1 C6 103.95(13) . . ?
O5 S2 O6 120.72(18) . . ?
O5 S2 O4 102.96(14) . . ?
O6 S2 O4 109.79(14) . . ?
O5 S2 C16 109.07(17) . . ?
O6 S2 C16 108.75(15) . . ?
O4 S2 C16 104.27(14) . . ?
C7 O3 S1 117.44(17) . . ?
C15 O4 S2 119.46(18) . . ?
C10 N1 C14 119.5(3) . . ?
C2 C1 C6 117.7(4) . . ?
C3 C2 C1 120.1(4) . . ?
C2 C3 C4 122.1(4) . . ?
C3 C4 C5 119.4(4) . . ?
C6 C5 C4 118.7(4) . . ?
C5 C6 C1 121.9(4) . . ?
C5 C6 S1 118.4(3) . . ?
C1 C6 S1 119.7(3) . . ?
O3 C7 C8 108.3(2) . . ?
C15 C8 C7 111.3(2) . . ?
C15 C8 C10 110.2(2) . . ?
C7 C8 C10 108.7(2) . . ?
C15 C8 C9 110.1(3) . . ?
C7 C8 C9 106.3(2) . . ?
C10 C8 C9 110.2(2) . . ?
C11 C10 N1 122.1(3) . . ?
C11 C10 C8 114.3(3) . . ?
N1 C10 C8 123.5(3) . . ?
C12 C11 C10 117.6(3) . . ?
C11 C12 C13 124.1(4) . . ?
C12 C13 C14 117.9(4) . . ?
C13 C14 N1 118.9(4) . . ?
O4 C15 C8 106.3(2) . . ?
C21 C16 C17 121.9(3) . . ?
C21 C16 S2 119.0(2) . . ?
C17 C16 S2 119.0(3) . . ?
C16 C17 C18 118.2(4) . . ?
C19 C18 C17 120.1(4) . . ?
C20 C19 C18 120.9(4) . . ?
C19 C20 C21 119.8(4) . . ?
C16 C21 C20 119.1(4) . . ?
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
S1 O1 1.418(3) . ?
S1 O2 1.424(2) . ?
S1 O3 1.568(2) . ?
S1 C6 1.754(4) . ?
S2 O5 1.423(3) . ?
S2 O6 1.430(3) . ?
S2 O4 1.565(2) . ?
S2 C16 1.755(3) . ?
O3 C7 1.466(3) . ?
O4 C15 1.481(4) . ?
N1 C10 1.371(5) . ?
N1 C14 1.390(6) . ?
C1 C2 1.390(6) . ?
C1 C6 1.403(5) . ?
C2 C3 1.364(7) . ?
C3 C4 1.368(7) . ?
C4 C5 1.393(6) . ?
C5 C6 1.377(5) . ?
C7 C8 1.527(4) . ?
C8 C15 1.515(4) . ?
C8 C10 1.532(4) . ?
C8 C9 1.537(4) . ?
C10 C11 1.341(4) . ?
C11 C12 1.337(6) . ?
C12 C13 1.374(6) . ?
C13 C14 1.374(6) . ?
C16 C21 1.373(5) . ?
C16 C17 1.377(5) . ?
C17 C18 1.392(7) . ?
C18 C19 1.376(7) . ?
C19 C20 1.365(7) . ?
C20 C21 1.387(6) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652568
