#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/17/7051752.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_7051752
loop_
_publ_author_name
'Altamura, Maria'
'Fedi, Valentina'
'Giannotti, Danilo'
'Paoli, Paola'
'Rossi, Patrizia'
_publ_section_title
;
 Privileged structures: synthesis and structural investigations on
 tricyclic sulfonamides
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2219
_journal_paper_doi               10.1039/b9nj00279k
_journal_volume                  33
_journal_year                    2009
_chemical_formula_sum            'C26 H22 Cl2 N2 O7 S3'
_chemical_formula_weight         641.54
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.706(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4934(4)
_cell_length_b                   40.567(2)
_cell_length_c                   8.9646(7)
_cell_measurement_temperature    298
_cell_volume                     2849.4(3)
_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      298
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Xcalibur3 4 circles diffractometer'
_diffrn_measurement_method       'intensity from ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54018
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11997
_diffrn_reflns_theta_full        62.27
_diffrn_reflns_theta_max         62.27
_diffrn_reflns_theta_min         5.34
_exptl_absorpt_coefficient_mu    4.523
_exptl_absorpt_correction_T_max  0.179
_exptl_absorpt_correction_T_min  0.114
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.00077(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         4254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0598
_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)+(0.0737P)²+3.4353P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.1715
_reflns_number_gt                2912
_reflns_number_total             4254
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b9nj00279k.txt
_cod_data_source_block           5b*(Me2SO4)
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               7051752
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -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
S1A S 0.85567(16) 0.82148(3) 0.27696(17) 0.0562(4) Uani 1 1 d . . .
Cl1A Cl 1.2993(3) 0.75091(4) 0.8454(3) 0.1175(8) Uani 1 1 d . . .
O1A O 0.8477(5) 0.84154(9) 0.1443(4) 0.0703(11) Uani 1 1 d . . .
O2A O 0.9117(5) 0.78819(8) 0.2862(5) 0.0695(11) Uani 1 1 d . . .
O3A O 0.8945(4) 0.87284(7) 0.6669(4) 0.0560(9) Uani 1 1 d . . .
N1A N 0.9852(5) 0.84065(10) 0.4365(5) 0.0497(11) Uani 1 1 d . . .
C1A C 0.6565(6) 0.82069(11) 0.2935(6) 0.0490(12) Uani 1 1 d . . .
C2A C 0.5696(6) 0.84971(11) 0.2950(6) 0.0475(12) Uani 1 1 d . . .
C3A C 0.4163(6) 0.84884(12) 0.3141(6) 0.0521(13) Uani 1 1 d . . .
H3A H 0.3572 0.8682 0.3131 0.062 Uiso 1 1 calc R . .
C4A C 0.3527(7) 0.81907(14) 0.3347(7) 0.0662(15) Uani 1 1 d . . .
H4A H 0.2486 0.8184 0.3464 0.079 Uiso 1 1 calc R . .
C5A C 0.4366(7) 0.79019(14) 0.3386(8) 0.0741(17) Uani 1 1 d . . .
H5A H 0.3919 0.7703 0.3559 0.089 Uiso 1 1 calc R . .
C6A C 0.5884(7) 0.79091(12) 0.3165(7) 0.0674(16) Uani 1 1 d . . .
H6A H 0.6456 0.7713 0.3170 0.081 Uiso 1 1 calc R . .
C7A C 1.0322(6) 0.82758(11) 0.5947(6) 0.0493(12) Uani 1 1 d . . .
C8A C 0.9931(6) 0.84407(12) 0.7118(7) 0.0535(13) Uani 1 1 d . . .
C9A C 1.0542(7) 0.83302(13) 0.8713(7) 0.0686(16) Uani 1 1 d . . .
H9A H 1.0329 0.8449 0.9503 0.082 Uiso 1 1 calc R . .
C10A C 1.1472(8) 0.80404(15) 0.9094(8) 0.0765(18) Uani 1 1 d . . .
H10A H 1.1874 0.7961 1.0149 0.092 Uiso 1 1 calc R . .
C11A C 1.1802(7) 0.78710(14) 0.7934(8) 0.0720(17) Uani 1 1 d . . .
C12A C 1.1280(6) 0.79852(12) 0.6379(7) 0.0584(14) Uani 1 1 d . . .
H12A H 1.1560 0.7871 0.5617 0.070 Uiso 1 1 calc R . .
S1B S 0.73636(17) 0.94045(3) 0.62494(16) 0.0558(4) Uani 1 1 d . . .
Cl1B Cl 0.2610(2) 0.99801(4) 0.0081(2) 0.0895(6) Uani 1 1 d . . .
O1B O 0.9074(4) 0.94430(8) 0.7409(4) 0.0702(11) Uani 1 1 d . . .
O2B O 0.6119(5) 0.96521(8) 0.6090(5) 0.0726(11) Uani 1 1 d . . .
O3B O 0.6507(4) 0.87863(7) 0.2859(4) 0.0544(9) Uani 1 1 d . . .
N1B N 0.7505(5) 0.93729(10) 0.4512(5) 0.0486(11) Uani 1 1 d . . .
C1B C 0.6539(6) 0.90296(12) 0.6645(6) 0.0488(12) Uani 1 1 d . . .
C2B C 0.7390(6) 0.87297(12) 0.6852(6) 0.0499(12) Uani 1 1 d . . .
C3B C 0.6674(7) 0.84471(13) 0.7184(6) 0.0625(15) Uani 1 1 d . . .
H3B H 0.7241 0.8246 0.7315 0.075 Uiso 1 1 calc R . .
C4B C 0.5095(8) 0.84653(17) 0.7320(7) 0.0721(17) Uani 1 1 d . . .
H4B H 0.4625 0.8277 0.7573 0.087 Uiso 1 1 calc R . .
C5B C 0.4231(8) 0.87572(18) 0.7087(7) 0.0742(17) Uani 1 1 d . . .
H5B H 0.3163 0.8765 0.7148 0.089 Uiso 1 1 calc R . .
C6B C 0.4945(7) 0.90410(15) 0.6759(6) 0.0641(15) Uani 1 1 d . . .
H6B H 0.4361 0.9240 0.6615 0.077 Uiso 1 1 calc R . .
C7B C 0.6016(6) 0.93552(11) 0.3033(6) 0.0454(11) Uani 1 1 d . . .
C8B C 0.5509(6) 0.90631(11) 0.2199(6) 0.0477(12) Uani 1 1 d . . .
C9B C 0.4153(7) 0.90483(13) 0.0719(7) 0.0604(14) Uani 1 1 d . . .
H9B H 0.3849 0.8849 0.0167 0.072 Uiso 1 1 calc R . .
C10B C 0.3258(7) 0.93318(13) 0.0071(7) 0.0629(15) Uani 1 1 d . . .
H10B H 0.2340 0.9326 -0.0923 0.075 Uiso 1 1 calc R . .
C11B C 0.3732(7) 0.96244(12) 0.0904(7) 0.0567(14) Uani 1 1 d . . .
C12B C 0.5104(6) 0.96409(12) 0.2367(6) 0.0545(13) Uani 1 1 d . . .
H12B H 0.5419 0.9841 0.2904 0.065 Uiso 1 1 calc R . .
S1S S 1.10933(18) 0.92457(3) 0.3122(2) 0.0673(5) Uani 1 1 d . . .
O1S O 1.0416(4) 0.90867(8) 0.4268(4) 0.0593(9) Uani 1 1 d . . .
C1S C 1.1199(9) 0.96726(15) 0.3552(10) 0.101(2) Uani 1 1 d . . .
H1S1 H 1.2104 0.9714 0.4581 0.152 Uiso 1 1 calc R . .
H1S2 H 1.0135 0.9744 0.3583 0.152 Uiso 1 1 calc R . .
H1S3 H 1.1417 0.9792 0.2726 0.152 Uiso 1 1 calc R . .
C2S C 0.9370(9) 0.92524(16) 0.1226(8) 0.089(2) Uani 1 1 d . . .
H2S1 H 0.9134 0.9032 0.0807 0.134 Uiso 1 1 calc R . .
H2S2 H 0.9660 0.9388 0.0490 0.134 Uiso 1 1 calc R . .
H2S3 H 0.8379 0.9341 0.1349 0.134 Uiso 1 1 calc R . .
H1NB H 0.828(6) 0.9260(12) 0.449(6) 0.051(16) Uiso 1 1 d . . .
H1NA H 0.980(6) 0.8619(12) 0.425(6) 0.058(15) 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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
O1A S1A O2A 119.9(2) . . ?
O1A S1A N1A 105.1(2) . . ?
O2A S1A N1A 107.7(2) . . ?
O1A S1A C1A 110.2(2) . . ?
O2A S1A C1A 106.8(2) . . ?
N1A S1A C1A 106.3(2) . . ?
C2B O3A C8A 117.3(4) . . ?
C7A N1A S1A 122.3(3) . . ?
C6A C1A C2A 118.8(5) . . ?
C6A C1A S1A 119.9(4) . . ?
C2A C1A S1A 121.1(4) . . ?
O3B C2A C3A 123.1(4) . . ?
O3B C2A C1A 116.1(4) . . ?
C3A C2A C1A 120.6(4) . . ?
C4A C3A C2A 118.8(5) . . ?
C3A C4A C5A 122.3(5) . . ?
C4A C5A C6A 119.1(5) . . ?
C5A C6A C1A 120.4(5) . . ?
C8A C7A C12A 118.7(5) . . ?
C8A C7A N1A 121.2(4) . . ?
C12A C7A N1A 120.0(5) . . ?
C7A C8A C9A 121.2(5) . . ?
C7A C8A O3A 118.4(5) . . ?
C9A C8A O3A 120.4(5) . . ?
C10A C9A C8A 118.5(6) . . ?
C11A C10A C9A 120.4(6) . . ?
C10A C11A C12A 121.7(5) . . ?
C10A C11A Cl1A 119.4(5) . . ?
C12A C11A Cl1A 118.9(5) . . ?
C11A C12A C7A 119.4(5) . . ?
O2B S1B O1B 120.1(2) . . ?
O2B S1B N1B 106.7(2) . . ?
O1B S1B N1B 106.1(2) . . ?
O2B S1B C1B 106.9(2) . . ?
O1B S1B C1B 108.5(2) . . ?
N1B S1B C1B 108.0(2) . . ?
C2A O3B C8B 118.4(3) . . ?
C7B N1B S1B 121.8(3) . . ?
C2B C1B C6B 119.2(5) . . ?
C2B C1B S1B 123.6(4) . . ?
C6B C1B S1B 117.2(4) . . ?
C3B C2B C1B 120.3(5) . . ?
C3B C2B O3A 122.5(5) . . ?
C1B C2B O3A 117.1(4) . . ?
C2B C3B C4B 119.5(5) . . ?
C5B C4B C3B 120.7(5) . . ?
C4B C5B C6B 120.0(5) . . ?
C5B C6B C1B 120.3(5) . . ?
C8B C7B C12B 118.5(5) . . ?
C8B C7B N1B 121.5(4) . . ?
C12B C7B N1B 119.9(4) . . ?
C7B C8B C9B 121.9(4) . . ?
C7B C8B O3B 116.8(4) . . ?
C9B C8B O3B 121.1(4) . . ?
C10B C9B C8B 119.2(5) . . ?
C9B C10B C11B 119.5(5) . . ?
C10B C11B C12B 121.4(5) . . ?
C10B C11B Cl1B 119.3(4) . . ?
C12B C11B Cl1B 119.3(4) . . ?
C11B C12B C7B 119.5(5) . . ?
O1S S1S C2S 105.7(3) . . ?
O1S S1S C1S 105.8(3) . . ?
C2S S1S C1S 98.5(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
S1A O1A 1.421(4) . ?
S1A O2A 1.424(3) . ?
S1A N1A 1.627(4) . ?
S1A C1A 1.754(5) . ?
Cl1A C11A 1.741(6) . ?
O3A C2B 1.392(5) . ?
O3A C8A 1.402(6) . ?
N1A C7A 1.419(6) . ?
C1A C6A 1.389(7) . ?
C1A C2A 1.392(6) . ?
C2A O3B 1.378(5) . ?
C2A C3A 1.379(6) . ?
C3A C4A 1.364(7) . ?
C4A C5A 1.365(8) . ?
C5A C6A 1.379(8) . ?
C7A C8A 1.389(7) . ?
C7A C12A 1.400(6) . ?
C8A C9A 1.393(7) . ?
C9A C10A 1.384(8) . ?
C10A C11A 1.363(8) . ?
C11A C12A 1.370(8) . ?
S1B O2B 1.425(3) . ?
S1B O1B 1.432(4) . ?
S1B N1B 1.613(5) . ?
S1B C1B 1.767(5) . ?
Cl1B C11B 1.730(5) . ?
O3B C8B 1.394(5) . ?
N1B C7B 1.438(6) . ?
C1B C2B 1.390(7) . ?
C1B C6B 1.397(7) . ?
C2B C3B 1.383(7) . ?
C3B C4B 1.395(8) . ?
C4B C5B 1.366(8) . ?
C5B C6B 1.384(8) . ?
C7B C8B 1.378(6) . ?
C7B C12B 1.394(6) . ?
C8B C9B 1.382(7) . ?
C9B C10B 1.377(7) . ?
C10B C11B 1.377(7) . ?
C11B C12B 1.379(7) . ?
S1S O1S 1.503(3) . ?
S1S C2S 1.764(7) . ?
S1S C1S 1.769(6) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652906
