2-Propyl 3,3-dibromo-2-hydroxypyrrolidine-1-carboxylate
Nichol, Gary S.; Gunawan, Steven; Xu, Zhigang; Dietrich, Justin; Hulme, Christopher; Acta Crystallographica Section E 66 (2010) o597–; doi:10.1107/S1600536810005106

data_2225233
_publ_section_title
;
 2-Propyl 3,3-dibromo-2-hydroxypyrrolidine-1-carboxylate
;
_journal_coeditor_code           FJ2278
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o597
_journal_paper_doi               10.1107/S1600536810005106
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C8 H13 Br2 N O3'
_chemical_formula_moiety         'C8 H13 Br2 N O3'
_chemical_formula_sum            'C8 H13 Br2 N O3'
_chemical_formula_weight         331.01
_chemical_name_systematic
;
2-Propyl 3,3-dibromo-2-hydroxypyrrolidine-1-carboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.880(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1061(5)
_cell_length_b                   5.9914(3)
_cell_length_c                   18.5496(9)
_cell_measurement_reflns_used    4995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.30
_cell_measurement_theta_min      2.21
_cell_volume                     1117.26(10)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction
'SAINT (Bruker, 2007) and CELL_NOW (Sheldrick, 2004)'
_computing_molecular_graphics
;
ORTEP3 for Windows (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEXII DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube with Miracol optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            34994
_diffrn_reflns_theta_full        36.38
_diffrn_reflns_theta_max         36.38
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    7.238
_exptl_absorpt_correction_T_max  0.5142
_exptl_absorpt_correction_T_min  0.1437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(TWINABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.414
_refine_diff_density_min         -0.770
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         9572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0410P)^2^+0.6397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                7956
_reflns_number_total             9572
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fj2278.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2225233
_cod_database_fobs_code          2225233