2-Bromo-1,3-dipyrrolidin-1-ylpropane-1,3-dionate bromide
Jonathan D. Crane; Richard P. Bunce; Acta Crystallographica Section E 60 (2004) o414–o415; doi:10.1107/S1600536804003563

data_2203311
_publ_section_title
;
 2-Bromo-1,3-dipyrrolidin-1-ylpropane-1,3-dionate bromide
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o414
_journal_page_last               o415
_journal_paper_doi               10.1107/S1600536804003563
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C11 H18 Br N2 O2 1+, Br 1-'
_chemical_formula_moiety         'C11 H18 Br N2 O2 1+, Br 1-'
_chemical_formula_sum            'C11 H18 Br2 N2 O2'
_chemical_formula_weight         370.09
_chemical_name_systematic
;
2-Bromo-1,3-dipyrrolidin-1-ylpropane-1,3-dionate bromide
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4235(13)
_cell_length_b                   12.9358(10)
_cell_length_c                   8.2935(6)
_cell_measurement_reflns_used    7940
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.77
_cell_measurement_theta_min      3.04
_cell_volume                     1440.1(2)
_computing_cell_refinement       'X-RED (Stoe & Cie,  2001)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        X-RED
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution
'X-STEP32 (Stoe & Cie, 2001) and WinGX (Farrugia, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS-II area-detector'
_diffrn_measurement_method       \w
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10894
_diffrn_reflns_theta_full        34.77
_diffrn_reflns_theta_max         34.77
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.622
_exptl_absorpt_correction_T_max  0.5016
_exptl_absorpt_correction_T_min  0.2629
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 2001)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.248
_refine_diff_density_min         -0.961
_refine_ls_abs_structure_details 'Flack (1983), 1313 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_coef       0.0136(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         3007
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0533P)^2^+7.6558P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1312
_reflns_number_gt                2578
_reflns_number_total             3007
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6168.cif
_cod_data_source_block           I
_cod_database_code               2203311
_cod_database_fobs_code          2203311