Crystal structure of (4<i>R</i>,5<i>S</i>,6<i>R</i>)-6-azido-5-benzyloxy-3,3,4-trifluoroazepan-1-ium 2,2,2-trifluoroacetate from synchrotron data
Patel, Alpesh Ramanlal; Bhadbhade, Mohan M.; Liu, Fei; Acta Crystallographica Section E 71 (2015) 1361–1365; doi:10.1107/S2056989015019416

data_2241216
_publ_section_title
;
 Crystal structure of
 (4<i>R</i>,5<i>S</i>,6<i>R</i>)-6-azido-5-benzyloxy-3,3,4-trifluoroazepan-1-ium
 2,2,2-trifluoroacetate from synchrotron data
;
_journal_coeditor_code           SJ5470
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1361
_journal_page_last               1365
_journal_paper_doi               10.1107/S2056989015019416
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C13 H16 F3 N4 O +, C2 F3 O2 -'
_chemical_formula_moiety         'C13 H16 F3 N4 O +, C2 F3 O2 -'
_chemical_formula_sum            'C15 H16 F6 N4 O3'
_chemical_formula_weight         414.32
_chemical_name_systematic
'(4<i>R</i>,5<i>S</i>,6<i>R</i>)-6-Azido-5-benzyloxy-3,3,4-trifluoroazepan-1-ium 2,2,2-trifluoroacetate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.42(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.8780(12)
_cell_length_b                   34.503(7)
_cell_length_c                   8.8120(18)
_cell_measurement_temperature    100
_cell_volume                     1785.6(6)
_computing_cell_refinement
;
<i>XDS</i> (Kabsch, 2010)
;
_computing_data_collection
;
<i>XDS</i> (Kabsch, 2010)
;
_computing_data_reduction
;
<i>XDS</i> (Kabsch, 2010)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009) and
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7293
_diffrn_reflns_av_R_equivalents  0.3862
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            13709
_diffrn_reflns_theta_full        21.468
_diffrn_reflns_theta_max         21.468
_diffrn_reflns_theta_min         2.374
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.414
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 390 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   2.2(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         3642
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1545
_refine_ls_R_factor_gt           0.1163
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2349
_refine_ls_wR_factor_ref         0.2613
_reflns_number_gt                2175
_reflns_number_total             3642
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5470sup1.cif
_cod_data_source_block           I
_cod_database_code               2241216
_cod_database_fobs_code          2241216
_shelx_estimated_absorpt_t_min   0.998
_shelx_estimated_absorpt_t_max   0.998
_shelx_hkl_checksum              69531
_shelx_res_checksum              38834