#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:18:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180071 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/17/7051742.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_7051742
loop_
_publ_author_name
'Dolenc, Darko'
'Modec, Barbara'
_publ_section_title
;
 EDA Complexes of N-halosaccharins with N- and O-donor ligands
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2344
_journal_paper_doi               10.1039/b9nj00263d
_journal_volume                  33
_journal_year                    2009
_chemical_formula_sum            'C7 H6 I N O4 S'
_chemical_formula_weight         327.09
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.2461(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4574(2)
_cell_length_b                   9.0194(2)
_cell_length_c                   12.9095(3)
_cell_measurement_temperature    150(2)
_cell_volume                     984.74(4)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0138
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4319
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    3.451
_exptl_absorpt_correction_T_max  0.8197
_exptl_absorpt_correction_T_min  0.7241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
HKL SCALEPACK (Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0203P)²+0.9634P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0466
_reflns_number_gt                2025
_reflns_number_total             2239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b9nj00263d.txt
_cod_data_source_block           NISac.H2O
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7051742
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
I1 I 0.495878(16) 0.666711(16) 0.793880(11) 0.01551(6) Uani 1 1 d . . .
S1 S 0.23798(6) 0.48423(6) 0.93483(4) 0.01439(12) Uani 1 1 d . . .
O1S O 0.2891(2) 0.57112(19) 1.02149(13) 0.0213(4) Uani 1 1 d . . .
O1 O 0.6370(3) 0.8897(2) 0.73956(15) 0.0223(4) Uani 1 1 d . . .
H1O H 0.714(4) 0.882(4) 0.731(3) 0.035(11) Uiso 1 1 d . . .
H2O H 0.592(5) 0.926(5) 0.678(3) 0.061(12) Uiso 1 1 d . . .
O2S O 0.09204(19) 0.52847(19) 0.88682(13) 0.0216(4) Uani 1 1 d . . .
O7 O 0.5480(2) 0.3073(2) 0.77141(14) 0.0223(4) Uani 1 1 d . . .
N1 N 0.3799(2) 0.4756(2) 0.84616(15) 0.0169(4) Uani 1 1 d . . .
C1 C 0.2418(3) 0.2926(3) 0.95866(17) 0.0152(4) Uani 1 1 d . . .
C2 C 0.1518(3) 0.2129(3) 1.02878(18) 0.0191(5) Uani 1 1 d . . .
H2 H 0.0783 0.2588 1.0714 0.023 Uiso 1 1 calc R . .
C3 C 0.1774(3) 0.0605(3) 1.03205(19) 0.0207(5) Uani 1 1 d . . .
H3 H 0.1204 0.0031 1.0787 0.025 Uiso 1 1 calc R . .
C4 C 0.2861(3) -0.0080(3) 0.96712(19) 0.0218(5) Uani 1 1 d . . .
H4 H 0.2992 -0.1103 0.9703 0.026 Uiso 1 1 calc R . .
C5 C 0.3755(3) 0.0741(3) 0.89762(19) 0.0198(5) Uani 1 1 d . . .
H5 H 0.4484 0.0283 0.8544 0.024 Uiso 1 1 calc R . .
C6 C 0.3529(3) 0.2265(3) 0.89457(18) 0.0156(5) Uani 1 1 d . . .
C7 C 0.4396(3) 0.3346(2) 0.82976(19) 0.0162(5) Uani 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'
I I -0.4742 1.8119 '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
N1 I1 O1 177.68(7) . . ?
O1S S1 O2S 116.20(10) . . ?
O1S S1 N1 110.31(10) . . ?
O2S S1 N1 109.71(10) . . ?
O1S S1 C1 113.38(11) . . ?
O2S S1 C1 111.36(11) . . ?
N1 S1 C1 93.56(10) . . ?
I1 O1 H1O 116(3) . . ?
I1 O1 H2O 109(3) . . ?
H1O O1 H2O 107(4) . . ?
C7 N1 S1 114.35(16) . . ?
C7 N1 I1 122.30(15) . . ?
S1 N1 I1 121.55(11) . . ?
C2 C1 C6 122.7(2) . . ?
C2 C1 S1 127.99(19) . . ?
C6 C1 S1 109.26(17) . . ?
C1 C2 C3 116.5(2) . . ?
C1 C2 H2 121.7 . . ?
C3 C2 H2 121.7 . . ?
C4 C3 C2 121.5(2) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C5 C4 C3 121.0(2) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C6 C5 C4 118.1(2) . . ?
C6 C5 H5 121.0 . . ?
C4 C5 H5 121.0 . . ?
C5 C6 C1 120.1(2) . . ?
C5 C6 C7 126.8(2) . . ?
C1 C6 C7 113.1(2) . . ?
O7 C7 N1 123.9(2) . . ?
O7 C7 C6 126.5(2) . . ?
N1 C7 C6 109.65(19) . . ?
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
I1 N1 2.0961(19) . ?
I1 O1 2.4431(19) . ?
S1 O1S 1.4312(17) . ?
S1 O2S 1.4353(17) . ?
S1 N1 1.664(2) . ?
S1 C1 1.756(2) . ?
O1 H1O 0.67(4) . ?
O1 H2O 0.94(4) . ?
O7 C7 1.215(3) . ?
N1 C7 1.386(3) . ?
C1 C2 1.386(3) . ?
C1 C6 1.389(3) . ?
C2 C3 1.392(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.392(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.388(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.481(3) . ?
