(<i>R</i>)- and (<i>S</i>)-2-(4-Bromophenyl)-2-oxoethyl 2-Methoxymethylpyrrolidine-1-dithiocarboxylate
Biedermann, Matthias; Hartung, Helmut; Dölling, Wolfgang; Verjus, Pierre; Acta Crystallographica Section C 54 (1998) 507–509; doi:10.1107/S0108270197016570

data_2007177
_publ_section_title
;
 (<i>R</i>)- and (<i>S</i>)-2-(4-Bromophenyl)-2-oxoethyl
 2-Methoxymethylpyrrolidine-1-dithiocarboxylate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              507
_journal_page_last               509
_journal_paper_doi               10.1107/S0108270197016570
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C15 H18 Br N O2 S2'
_chemical_formula_sum            'C15 H18 Br N O2 S2'
_chemical_formula_weight         388.33
_chemical_melting_point          363(4)
_chemical_name_systematic
; (R)-2-(4-bromophenyl)-2-oxoethyl 2-methoxymethylpyrrolidine-1-
dithiocarboxylate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7824(7)
_cell_length_b                   10.5830(10)
_cell_length_c                   16.3440(10)
_cell_measurement_reflns_used    80
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.3
_cell_measurement_theta_min      10.2
_cell_volume                     1692.0(2)
_computing_cell_refinement       'STADI4 (Stoe, 1996a)'
_computing_data_collection       'STADI4 (Stoe, 1996a)'
_computing_data_reduction        'X-RED (STOE, 1996b)'
_computing_molecular_graphics    'XP/PC (Siemens, 1990)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Stoe Stadi4 diffractometer'
_diffrn_measurement_method       \q/2\q
_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3432
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        6.8
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.68
_exptl_absorpt_correction_T_max  0.466
_exptl_absorpt_correction_T_min  0.396
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            brown--yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         .330
_refine_diff_density_min         -.303
_refine_ls_abs_structure_details
'Flack (1983) parameter = 0.00(2); 1716 Friedel pairs'
_refine_ls_extinction_coef       0.0019(4)
_refine_ls_extinction_method     SHELXL93_(Sheldrick,_1993)
_refine_ls_goodness_of_fit_all   1.242
_refine_ls_goodness_of_fit_obs   1.170
_refine_ls_hydrogen_treatment    H_atoms:_see_below
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.294
_refine_ls_restrained_S_obs      1.170
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_obs          .0623
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0237P)^2^+1.8808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1326
_refine_ls_wR_factor_obs         .0941
_reflns_number_observed          1891
_reflns_number_total             2969
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            jz1254.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '86--93_C' was changed to '363(4)' -
it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '86--93_C' was changed to '363(4)' -
it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0237P)^2^+1.8808P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0237P)^2^+1.8808P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1692.1(2)
_cod_database_code               2007177