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_7229220
_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_absolute_configuration syn
_chemical_formula_moiety         'C12 H22 Ca N6 O6, 2(I), H2 O'
_chemical_formula_sum            'C12 H24 Ca I2 N6 O7'
_chemical_formula_weight         658.25
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-09-18 deposited with the CCDC.
2017-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.9123(6)
_cell_length_b                   20.333(2)
_cell_length_c                   23.505(3)
_cell_measurement_reflns_used    732
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4496
_cell_measurement_theta_min      3.2815
_cell_volume                     2347.7(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_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 0.832
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_sigmaI/netI    0.1522
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3715
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.45
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    2.939
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1619
_refine_ls_R_factor_gt           0.0698
_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^)+(0.0097P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                1296
_reflns_number_total             2389
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c7ce01326d2.cif
_cod_data_source_block           cai2-lhi
_cod_original_cell_volume        2347.8(5)
_cod_original_sg_symbol_H-M      C2221
_cod_database_code               7229220