Chiral thiouronium salts: synthesis, characterisation and application in NMR enantio-discrimination of chiral oxoanions
Foreiter, Magdalena B.; Gunaratne, H. Q. Nimal; Nockemann, Peter; Seddon, Kenneth R.; Stevenson, Paul J.; Wassell, David F.; New Journal of Chemistry 37 (2013) 515–; doi:10.1039/c2nj40632b

data_7053234
_publ_section_title
;
 Chiral thiouronium salts: synthesis, characterisation and application in
 NMR enantio-discrimination of chiral oxoanions
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              515
_journal_paper_doi               10.1039/c2nj40632b
_journal_volume                  37
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Br, C45 H69 N2 S'
_chemical_formula_sum            'C45 H69 Br N2 S'
_chemical_formula_weight         749.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-10-29
_audit_creation_method
;
Olex2 1.1
(compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.072(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.543(2)
_cell_length_b                   11.5238(17)
_cell_length_c                   15.689(3)
_cell_measurement_reflns_used    11151
_cell_measurement_temperature    100
_cell_measurement_theta_max      34.7
_cell_measurement_theta_min      2.5
_cell_volume                     2054.8(6)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_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)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_details
;
scan:
Number of images: 180
Slice: -110.0000 - 70.0000
Image width: 1.0000
Exp time: 5.0000
Rotation axis: Omega
Omega: 0.0000
Kappa: 0.0000
Phi: 270.0000
XTD: 34.8614
2theta: -19.6361
;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.000886
_diffrn_orient_matrix_UB_12      -0.075344
_diffrn_orient_matrix_UB_13      0.045431
_diffrn_orient_matrix_UB_21      0.078244
_diffrn_orient_matrix_UB_22      0.018698
_diffrn_orient_matrix_UB_23      0.032535
_diffrn_orient_matrix_UB_31      -0.027670
_diffrn_orient_matrix_UB_32      0.020221
_diffrn_orient_matrix_UB_33      0.054922
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           Molybdenum
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.1392
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14473
_diffrn_reflns_theta_full        34.73
_diffrn_reflns_theta_max         34.73
_diffrn_reflns_theta_min         2.52
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.583
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.882
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.018(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.870
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         12111
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.870
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                8179
_reflns_number_total             12111
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2nj40632b.txt
_cod_data_source_block           p21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
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_cod_database_code               7053234