Differentiation of diastereotopic bromine atoms in SN2 reactions of gem-dibromides
Niels Muenster; Klaus Harms; Ulrich Koert; Chem.Commun. 48 (2012) 1866–; doi:10.1039/c2cc17599a

data_7107326
_publ_section_title
;
 Differentiation of diastereotopic bromine atoms in SN2 reactions of
 gem-dibromides
;
_journal_name_full               Chem.Commun.
_journal_page_first              1866
_journal_paper_doi               10.1039/c2cc17599a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C28 H31 Br N2 O9 S'
_chemical_formula_sum            'C28 H31 Br N2 O9 S'
_chemical_formula_weight         651.52
_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                87.467(4)
_cell_angle_beta                 89.464(5)
_cell_angle_gamma                87.999(4)
_cell_formula_units_Z            4
_cell_length_a                   10.4715(6)
_cell_length_b                   14.8297(7)
_cell_length_c                   19.0746(11)
_cell_measurement_reflns_used    9238
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.8
_cell_volume                     2957.3(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-AREA'
_computing_molecular_graphics    'DIAMOND 3.2g'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2008 (Giacovazzo et al, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.0708
_diffrn_reflns_av_sigmaI/netI    0.1643
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29197
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    1.516
_exptl_absorpt_correction_T_max  0.8526
_exptl_absorpt_correction_T_min  0.7406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.610
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         10519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.610
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0110P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0613
_reflns_number_gt                4455
_reflns_number_total             10519
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2cc17599a.txt
_cod_data_source_block           nm147
_cod_database_code               7107326