NH⋯O and OH⋯O interactions of glycine derivatives with squaric acid
Anioła, Michalina; Dega-Szafran, Zofia; Katrusiak, Andrzej; Szafran, Mirosław; New Journal of Chemistry 38 (2014) 3556–; doi:10.1039/C4NJ00212A

data_7054324
_publ_section_title
;
 NH&#x22EF;O and OH&#x22EF;O interactions of glycine derivatives with
 squaric acid
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3556
_journal_paper_doi               10.1039/C4NJ00212A
_journal_volume                  38
_journal_year                    2014
_chemical_formula_moiety         'C4 H O4, C3 H8 N O2, 0.5(H2 O)'
_chemical_formula_sum            'C7 H10 N O6.5'
_chemical_formula_weight         212.16
_chemical_name_common            'Sarcosinium hydrogen squarate semihydrate'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.0249(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.6068(2)
_cell_length_b                   7.21436(8)
_cell_length_c                   15.44410(17)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      75.31
_cell_measurement_theta_min      5.37
_cell_volume                     1836.43(4)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction, 2002)'
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'Mercury (2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.981
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0098
_diffrn_reflns_av_sigmaI/netI    0.0075
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6657
_diffrn_reflns_theta_full        75.31
_diffrn_reflns_theta_max         75.31
_diffrn_reflns_theta_min         5.37
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; 
Correction for absorption was made using XEMP (SHELXTL, 
Sheldrick (1990)).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.141
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.807
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         1862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.807
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0842P)^2^+1.1792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                1823
_reflns_number_total             1862
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7054216
_cod_data_source_file            c4nj00212a5.cif
_cod_data_source_block           m
_cod_depositor_comments
;
The following automatic conversions were performed:
'__exptl_crystal_description' tag replaced with
'_exptl_crystal_description'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

2018-03-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C14 H20 N2 O13'
_cod_original_formula_weight         424.32
_cod_original_formula_moiety         '2(C4 H O4), 2(C3 H8 N O2), H2 O'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7054324