Potassium [1-(<i>tert</i>-butoxycarbonyl)-1<i>H</i>-indol-3-yl]trifluoroborate hemihydrate
Berionni, Guillaume; Mayer, Peter; Mayr, Herbert; Acta Crystallographica Section E 68 (2012) m551–m552; doi:10.1107/S1600536812014225

data_2234671
_publ_section_title
;
 Potassium
 [1-(<i>tert</i>-butoxycarbonyl)-1<i>H</i>-indol-3-yl]trifluoroborate
 hemihydrate
;
_journal_coeditor_code           HP2034
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m551
_journal_page_last               m552
_journal_paper_doi               10.1107/S1600536812014225
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'K +, C13 H14 B1 F3 N1 O2, 0.5H2 O1'
_chemical_formula_moiety         'K +, C13 H14 B1 F3 N1 O2, 0.5(H2 O1)'
_chemical_formula_sum            'C13 H15 B F3 K N O2.5'
_chemical_formula_weight         332.17
_chemical_name_systematic
;
Potassium [1-(<i>tert</i>-butoxycarbonyl)-1<i>H</i>-indol-3-yl]trifluoroborate
hemihydrate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   5.84280(10)
_cell_length_b                   16.3177(2)
_cell_length_c                   32.1286(5)
_cell_measurement_reflns_used    12366
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     3063.17(8)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 2004)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD; rotation images'
_diffrn_radiation_monochromator  'MONTEL, graded multilayered X-ray optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            24771
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    0.384
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.44056(4)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.236
_refine_ls_abs_structure_details
;
Flack (1983),
2995 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         7001
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+1.0137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0745
_reflns_number_gt                6369
_reflns_number_total             7001
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            hp2034.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C13 H15 B F3 K N O2.50'
_cod_database_code               2234671
_cod_database_fobs_code          2234671