Crystal structures of <i>Z</i>–Gly–Aib–O^{-^}·0.5Ca^2+^·H~2~O and <i>Z</i>–Gly–Aib–OH
Gessmann, Renate; Brückner, Hans; Petratos, Kyriacos; Acta Crystallographica Section E 74 (2018) 1173–1177; doi:10.1107/S2056989018010745

data_2242575
_publ_section_title
;
 Crystal structures of
 <i>Z</i>--Gly--Aib--O^{-^}&#x00B7;0.5Ca^2+^&#x00B7;H~2~O and
 <i>Z</i>--Gly--Aib--OH
;
_journal_coeditor_code           EX2009
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1173
_journal_page_last               1177
_journal_paper_doi               10.1107/S2056989018010745
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'Ca 2+, 2(C14 H17 N2 O5 -), H2 O'
_chemical_formula_moiety         'Ca 2+, 2C14 H17 N2 O5 -, H2 O'
_chemical_formula_sum            'C28 H38 Ca N4 O12'
_chemical_formula_weight         662.70
_chemical_name_systematic
;
Calcium(II) bis[2-(2-{[(benzyloxy)carbonyl]amino}acetamido)-2-methylpropanoate]
monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2015
_cell_angle_alpha                90
_cell_angle_beta                 112.55(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.996(3)
_cell_length_b                   5.5740(11)
_cell_length_c                   20.607(4)
_cell_measurement_reflns_used    4716
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.
_cell_measurement_theta_min      0.666
_cell_volume                     1590.8(6)
_computing_cell_refinement
;
<i>XDS</i> (Kabsch, 2010)
;
_computing_data_reduction
;
<i>XDS</i> (Kabsch, 2010)
;
_computing_molecular_graphics
;
<i>COOT</i> (Emsley <i>et al.</i>,  2010), <i>SwissPDBViewer</i>
(Guex & Peitsch, 1997)
;
_computing_publication_material
;
CHEMDRAW (Mills, 2006),  ORTEPIII (Burnett & Johnson, (1996),
ORTEP-3 for Windows (Farrugia, 2012), <i>POVRAY</i>
 (Persistence of Vision, 2004), PyMOL (DeLano, 2002)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS86 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type
'Pilatus3 6M detector on beamline I24 of Diamond Light Source'
_diffrn_measurement_method       \f-scans
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.59038
_diffrn_reflns_av_R_equivalents  0.1277
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28071
_diffrn_reflns_theta_full        20.746
_diffrn_reflns_theta_max         26.291
_diffrn_reflns_theta_min         1.221
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       brick
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.270
_refine_diff_density_min         -0.563
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0776
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+1.1073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2000
_refine_ls_wR_factor_ref         0.2140
_reflns_number_gt                3941
_reflns_number_total             4716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ex2009sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-11-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '0.5(Ca 2+), C14 H17 N2 O5 -, 0.5(H2 O)'
_cod_original_formula_iupac      '0.5Ca 2+, C14 H17 N2 O5 -, 0.5H2 O'
_cod_original_formula_sum        'C14 H19 Ca0.50 N2 O6'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     331.35
_cod_database_code               2242575
_cod_database_fobs_code          2242575
_shelx_hkl_checksum              97387
_shelx_res_checksum              10922
_shelxl_version_number           2.014