#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/19/7051960.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_7051960
loop_
_publ_author_name
'Altamura, Maria'
'Dapporto, Paolo'
'Guidi, Antonio'
'Harmat, Nicholas J. S.'
'Jierry, Loïc'
'Libralesso, Elisa'
'Paoli, Paola'
'Rossi, Patrizia'
_publ_section_title
;
 Investigation on the flexibility of chiral tricyclic derivatives
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1617
_journal_paper_doi               10.1039/b801569d
_journal_volume                  32
_journal_year                    2008
_chemical_formula_sum            'C15 H13 N O6 S'
_chemical_formula_weight         335.32
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.32(1)
_cell_angle_beta                 90.98(1)
_cell_angle_gamma                99.13(1)
_cell_formula_units_Z            2
_cell_length_a                   8.117(1)
_cell_length_b                   8.432(1)
_cell_length_c                   11.705(2)
_cell_measurement_temperature    150
_cell_volume                     748.96(19)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_molecular_graphics    'ORTEP-3 (Farruggia, 1997)'
_computing_publication_material  'PARST97 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'Xcalibur3 4 circles diffractometer'
_diffrn_measurement_method       'intensity from ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9073
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         4.32
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0415
_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)+(0.0791P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                2612
_reflns_number_total             3290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801569d.txt
_cod_data_source_block           3
_cod_original_cell_volume        748.96(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7051960
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S -0.68340(5) 1.53454(5) 0.83256(4) 0.02377(16) Uani 1 1 d . . .
O1 O -0.53178(15) 1.08586(14) 0.66069(11) 0.0297(3) Uani 1 1 d . . .
O2 O -0.08308(16) 1.05748(16) 0.75533(12) 0.0314(3) Uani 1 1 d . . .
O3 O -0.12921(17) 1.21940(16) 0.64172(12) 0.0339(3) Uani 1 1 d . . .
O4 O -0.72400(15) 1.39265(16) 0.87628(11) 0.0328(3) Uani 1 1 d . . .
O5 O -0.77569(14) 1.67209(15) 0.87104(11) 0.0327(3) Uani 1 1 d . . .
O1W O -0.13038(17) 1.07716(17) 0.38932(13) 0.0334(3) Uani 1 1 d . . .
N1 N -0.38583(17) 1.33561(17) 0.77830(13) 0.0229(3) Uani 1 1 d . . .
C1 C -0.60589(19) 1.32545(19) 0.62241(15) 0.0215(4) Uani 1 1 d . . .
C2 C -0.69135(19) 1.4593(2) 0.67442(15) 0.0211(3) Uani 1 1 d . . .
C3 C -0.7771(2) 1.5312(2) 0.60577(17) 0.0258(4) Uani 1 1 d . . .
C4 C -0.7803(2) 1.4664(2) 0.48039(17) 0.0286(4) Uani 1 1 d . . .
C5 C -0.7009(2) 1.3300(2) 0.42720(16) 0.0282(4) Uani 1 1 d . . .
C6 C -0.6150(2) 1.2590(2) 0.49640(16) 0.0255(4) Uani 1 1 d . . .
C7 C -0.5094(2) 1.2420(2) 0.69053(15) 0.0232(4) Uani 1 1 d . . .
C8 C -0.3473(2) 1.51573(19) 0.82885(14) 0.0205(3) Uani 1 1 d . . .
C9 C -0.46903(19) 1.6191(2) 0.86362(14) 0.0206(3) Uani 1 1 d . . .
C10 C -0.4249(2) 1.7935(2) 0.91828(16) 0.0272(4) Uani 1 1 d . . .
C11 C -0.2586(2) 1.8676(2) 0.94272(17) 0.0307(4) Uani 1 1 d . . .
C12 C -0.1364(2) 1.7675(2) 0.90812(17) 0.0303(4) Uani 1 1 d . . .
C13 C -0.1794(2) 1.5935(2) 0.85125(15) 0.0253(4) Uani 1 1 d . . .
C14 C -0.2798(2) 1.2356(2) 0.81963(16) 0.0245(4) Uani 1 1 d . . .
C15 C -0.1555(2) 1.1701(2) 0.72749(15) 0.0232(4) Uani 1 1 d . . .
H2O H -0.007(3) 1.025(3) 0.710(2) 0.050(7) Uiso 1 1 d . . .
H1W H -0.236(4) 1.021(3) 0.379(3) 0.067(8) Uiso 1 1 d . . .
H2W H -0.119(4) 1.124(3) 0.475(3) 0.076(9) Uiso 1 1 d . . .
H3 H -0.826(3) 1.625(3) 0.6476(19) 0.041(6) Uiso 1 1 d . . .
H4 H -0.843(3) 1.520(3) 0.437(2) 0.039(6) Uiso 1 1 d . . .
H5 H -0.709(3) 1.289(2) 0.340(2) 0.041(6) Uiso 1 1 d . . .
H6 H -0.557(2) 1.170(2) 0.4562(16) 0.022(4) Uiso 1 1 d . . .
H10 H -0.516(2) 1.859(2) 0.9420(17) 0.027(5) Uiso 1 1 d . . .
H11 H -0.229(3) 1.991(3) 0.978(2) 0.041(6) Uiso 1 1 d . . .
H12 H -0.018(3) 1.818(2) 0.9246(18) 0.032(5) Uiso 1 1 d . . .
H13 H -0.093(2) 1.522(2) 0.8272(16) 0.024(5) Uiso 1 1 d . . .
H14A H -0.348(2) 1.138(3) 0.8341(18) 0.032(5) Uiso 1 1 d . . .
H14B H -0.221(2) 1.300(2) 0.8922(18) 0.025(5) 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
O4 S1 O5 118.92(8) . . ?
O4 S1 C2 108.88(8) . . ?
O5 S1 C2 109.53(8) . . ?
O4 S1 C9 109.99(8) . . ?
O5 S1 C9 108.22(7) . . ?
C2 S1 C9 99.56(8) . . ?
C7 N1 C8 127.30(14) . . ?
C7 N1 C14 114.88(14) . . ?
C8 N1 C14 117.77(14) . . ?
C2 C1 C6 117.83(15) . . ?
C2 C1 C7 125.44(15) . . ?
C6 C1 C7 116.69(14) . . ?
C3 C2 C1 122.33(15) . . ?
C3 C2 S1 121.05(13) . . ?
C1 C2 S1 116.62(13) . . ?
C2 C3 C4 118.86(16) . . ?
C5 C4 C3 119.59(16) . . ?
C6 C5 C4 121.24(17) . . ?
C5 C6 C1 120.08(16) . . ?
O1 C7 N1 119.23(15) . . ?
O1 C7 C1 119.41(15) . . ?
N1 C7 C1 121.09(14) . . ?
C13 C8 C9 117.83(14) . . ?
C13 C8 N1 118.64(14) . . ?
C9 C8 N1 123.43(14) . . ?
C10 C9 C8 121.35(14) . . ?
C10 C9 S1 117.40(12) . . ?
C8 C9 S1 121.17(12) . . ?
C11 C10 C9 120.04(15) . . ?
C10 C11 C12 119.37(17) . . ?
C11 C12 C13 120.96(16) . . ?
C12 C13 C8 120.40(16) . . ?
N1 C14 C15 111.69(14) . . ?
O3 C15 O2 126.10(15) . . ?
O3 C15 C14 123.11(15) . . ?
O2 C15 C14 110.79(14) . . ?
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 O4 1.4379(13) . ?
S1 O5 1.4381(12) . ?
S1 C2 1.7544(17) . ?
S1 C9 1.7578(16) . ?
O1 C7 1.2331(19) . ?
O2 C15 1.311(2) . ?
O3 C15 1.211(2) . ?
N1 C7 1.374(2) . ?
N1 C8 1.426(2) . ?
N1 C14 1.469(2) . ?
C1 C2 1.399(2) . ?
C1 C6 1.399(2) . ?
C1 C7 1.501(2) . ?
C2 C3 1.385(2) . ?
C3 C4 1.394(3) . ?
C4 C5 1.387(2) . ?
C5 C6 1.385(3) . ?
C8 C13 1.397(2) . ?
C8 C9 1.402(2) . ?
C9 C10 1.390(2) . ?
C10 C11 1.379(2) . ?
C11 C12 1.387(2) . ?
C12 C13 1.390(2) . ?
C14 C15 1.525(2) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652914
