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_7238045
_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 syn
_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            ectoine
_chemical_name_systematic
'1,4,5,6-tetrahydro-2-methyl-4-pyrimidine carboxylic acid'
_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   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-09-24 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    6083
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      62.60
_cell_measurement_theta_min      4.417
_cell_volume                     875.33(7)
_computing_cell_refinement       'ILL program RAFD19'
_computing_data_collection
'ILL program Multi Detector Acquisition software'
_computing_data_reduction        'ILL program RETREAT'
_computing_molecular_graphics
;
Mercury (Version 4.1.3, Macrae et al., 2008) and XP in SHELXTL-Plus (Sheldrick,
2008)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'from X-ray structure'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  '4 circle diffractometer D19'
_diffrn_measurement_method       'omega scan (step width in omega 0.07deg)'
_diffrn_radiation_type           neutrons
_diffrn_radiation_wavelength     1.1698
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7579
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        62.500
_diffrn_reflns_theta_max         62.552
_diffrn_reflns_theta_min         4.629
_diffrn_source                   'neutron reactor, ILL Grenoble'
_exptl_absorpt_coefficient_mu    0.044
_exptl_absorpt_correction_T_max  0.7301
_exptl_absorpt_correction_T_min  0.4339
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'ILL program D19abs'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_exptl_crystal_size_max          1.000
_exptl_crystal_size_mid          1.000
_exptl_crystal_size_min          1.000
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
;
 All f" are zero, so absolute structure could not be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         2971
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+1.2382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0806
_reflns_Friedel_coverage         0.676
_reflns_Friedel_fraction_full    0.885
_reflns_Friedel_fraction_max     0.883
_reflns_number_gt                2909
_reflns_number_total             2971
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {c650af6c-a010-4b50-a28a-ad7cd092c81e}
_cod_data_source_file            c9ce01599j2.cif
_cod_data_source_block           d_h_ect173_can
_cod_depositor_comments
;Adding full bibliography for 7238043--7238045.cif.

 Adding full bibliography for 7238043--7238045.cif.
;
_cod_database_code               7238045
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.957
_shelx_estimated_absorpt_t_max   0.957
_shelx_res_checksum              34940
_publcif_funding_html
;
;