Crystal structure of (2RS)-2-bromomethyl-4,4-dimethyl-3,4-dihydro- 2H-pyrrole 1-oxide hemi(hydrobromide), C~7~H~12~BrNO · ½HBr
Frey, W.; Gulla, M.; Jäger, V.; Zeitschrift für Kristallographie - New Crystal Structures 221 (2006) 215–216; doi:

data_8101970
_publ_section_title
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Crystal structure of (2RS)-2-bromomethyl-4,4-dimethyl-3,4-dihydro-
2H-pyrrole 1-oxide hemi(hydrobromide), C~7~H~12~BrNO &#x00B7; &#x00BD;HBr
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              215
_journal_page_last               216
_journal_volume                  221
_journal_year                    2006
_chemical_formula_sum            'C7 H12.5 Br1.5 N O'
_chemical_formula_weight         246.55
_chemical_melting_point          326.5(5)
_chemical_name_systematic
; 
(2RS)-2-bromomethyl-4,4-dimethyl-3,4-dihydro-2H-pyrrole 
1-oxide hemi-hydrobromide 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.037(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.249(2)
_cell_length_b                   8.5709(10)
_cell_length_c                   11.0831(10)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      24
_cell_volume                     1882.5(4)
_computing_cell_refinement       'Bruker Xscans, Release 2.31'
_computing_data_collection       'Bruker Xscans, Release 2.31'
_computing_data_reduction        'Bruker Xscans, Release 2.31'
_computing_molecular_graphics    'SHELXTL-Plus, XP (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2026
_diffrn_reflns_theta_full        67.48
_diffrn_reflns_theta_max         67.48
_diffrn_reflns_theta_min         4.46
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.995
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.460
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.00337(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0592P)^2^+8.3856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1159
_reflns_number_gt                1549
_reflns_number_total             1636
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1775.cff
_cod_data_source_block           wf1009mg
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '326-327 K' was changed to '326.5(5)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
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_cod_original_cell_volume        1882.5(3)
_cod_original_sg_symbol_H-M      C12/c1
_cod_original_formula_sum        'C7 H12.50 Br1.50 N O'
_cod_database_code               8101970