Ionic co-crystals of enantiopure and racemic histidine with calcium halides
Shemchuk, Oleksii; Degli Esposti, Lorenzo; Grepioni, Fabrizia; Braga, Dario; CrystEngComm  (2017) –; doi:10.1039/C7CE01326D

data_7229218
_publ_section_title
;
 Ionic co-crystals of enantiopure and racemic histidine with calcium
 halides
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01326D
_journal_year                    2017
_chemical_formula_sum            'C6 H13 Br Ca0.5 N3 O4'
_chemical_formula_weight         291.14
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-07-19 deposited with the CCDC.
2017-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                95.772(9)
_cell_angle_beta                 96.250(9)
_cell_angle_gamma                103.656(10)
_cell_formula_units_Z            2
_cell_length_a                   4.8911(6)
_cell_length_b                   10.0848(12)
_cell_length_c                   11.8785(13)
_cell_measurement_reflns_used    1255
_cell_measurement_temperature    295
_cell_measurement_theta_max      27.6100
_cell_measurement_theta_min      4.1950
_cell_volume                     561.11(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1340
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.845
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -43.00  49.00   1.00  291.57    --  -16.36  77.00-180.00   92
  2  \w     -7.00  84.00   1.00  291.57    --   17.61  77.00 -60.00   91
  3  \w     32.00  83.00   1.00  291.57    --   17.61  77.00  90.00   51
  4  \w     -5.00  70.00   1.00  291.57    --   17.61  77.00  60.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1159
_diffrn_reflns_av_sigmaI/netI    0.1544
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3874
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.97
_diffrn_reflns_theta_min         3.48
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.889
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             294
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.540
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2517
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1304
_refine_ls_R_factor_gt           0.0938
_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^)+(0.1117P)^2^+0.3498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2379
_refine_ls_wR_factor_ref         0.2683
_reflns_number_gt                1596
_reflns_number_total             2517
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c7ce01326d2.cif
_cod_data_source_block           DL_Histidine_CalciumBromide
_cod_original_cell_volume        561.11(11)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C6 H13 Br Ca0.50 N3 O4'
_cod_database_code               7229218