Complex transitions between dihydrate and anhydrate forms of ectoine – unexpected behavior of a highly hygroscopic compatible solute in the solid state
Hützler, Wilhelm Maximilian; Mossou, Estelle; Vollrath, Ronnald; Kohagen, Miriam; El Ghrissi, Imadine; Grininger, Martin; Zaccai, Giuseppe; Smiatek, Jens; Oesterhelt, Dieter; CrystEngComm 22 (2020) 169–172; doi:10.1039/C9CE01599J

data_7238044
_publ_section_title
;
 Complex transitions between dihydrate and anhydrate forms of ectoine --
 unexpected behavior of a highly hygroscopic compatible solute in the
 solid state
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              169
_journal_page_last               172
_journal_paper_doi               10.1039/C9CE01599J
_journal_volume                  22
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C6 H10 N2 O2, 2(H2 O)'
_chemical_formula_sum            'C6 H14 N2 O4'
_chemical_formula_weight         178.19
_chemical_name_common
'(S)-2-methyl-3,4,5,6-tetrahydropyrimidine-4-carboxylic acid'
_chemical_name_systematic        'Ectoine dihydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-01-15 deposited with the CCDC.	2019-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5940(3)
_cell_length_b                   8.6265(5)
_cell_length_c                   13.3619(6)
_cell_measurement_reflns_used    2290
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      49.82
_cell_measurement_theta_min      5.13
_cell_volume                     875.33(7)
_computing_cell_refinement       'APEX3 (Bruker, 2012)'
_computing_data_collection       'APEX3 (Bruker, 2012)'
_computing_data_reduction        'APEX3 (Bruker, 2012)'
_computing_molecular_graphics
;
Mercury (Version 3.3, Macrae et al., 2008) and XP in SHELXTL-Plus (Sheldrick,
2008)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Siemens CCD three-circle diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12908
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         69.553
_diffrn_reflns_theta_min         6.626
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: deionized water'
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.137
_refine_diff_density_min         -0.133
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
; 
 Flack x determined using 623 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1575
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.2764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0751
_reflns_Friedel_coverage         0.658
_reflns_Friedel_fraction_full    0.960
_reflns_Friedel_fraction_max     0.934
_reflns_number_gt                1575
_reflns_number_total             1575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01599j2.cif
_cod_data_source_block           mhmg1
_cod_depositor_comments
;Adding full bibliography for 7238043--7238045.cif.

 Adding full bibliography for 7238043--7238045.cif.
;
_cod_database_code               7238044
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.723
_shelx_estimated_absorpt_t_max   0.861
_shelx_res_checksum              74158