Overcoming the solvation shell during the crystallisation of diatrizoic acid from dimethylsulfoxide
Fucke, Katharina; Howard, Judith; Steed, Jonathan; Chemical Communications (Cambridge, United Kingdom) 48 (2012) 12065–12067; doi:10.1039/c2cc35995b

data_7108661
_publ_section_title
;
 Overcoming the solvation shell during the crystallisation of diatrizoic
 acid from dimethylsulfoxide
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   99
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              12065
_journal_page_last               12067
_journal_paper_doi               10.1039/c2cc35995b
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C11 H9 I3 N2 O4, 4(C2 H6 O S)'
_chemical_formula_sum            'C19 H33 I3 N2 O8 S4'
_chemical_formula_weight         926.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.7640(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.5386(5)
_cell_length_b                   9.6418(2)
_cell_length_c                   16.3885(4)
_cell_measurement_temperature    120
_cell_volume                     3222.81(13)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
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_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
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_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0487
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_diffrn_reflns_limit_k_min       -11
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_diffrn_reflns_limit_l_min       -20
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_diffrn_source                   'sealed X-ray tube'
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_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
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_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.402
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0336
_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/[\s^2^(Fo^2^)+(0.0518P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                5307
_reflns_number_total             6584
_reflns_threshold_expression     >2sigma(I)
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_cod_database_code               7108661