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_7054322
_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 H2 O4, C4 H O4, C4 H9 N O2, C4 H10 N O2'
_chemical_formula_sum            'C16 H22 N2 O12'
_chemical_formula_weight         434.36
_chemical_name_common            'Dimethylglycinium hydrogen squarate'
_chemical_name_systematic        'Dimethylglycine-squaric acid'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.249(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5110(5)
_cell_length_b                   6.5385(2)
_cell_length_c                   17.3475(4)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      2.47
_cell_volume                     1886.32(10)
_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 0.893
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11666
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.956
_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    1.529
_exptl_crystal_density_meas      1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                3180
_reflns_number_total             4520
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7054214
_cod_data_source_file            c4nj00212a6.cif
_cod_data_source_block           m
_cod_original_cell_volume        1886.32(9)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7054322