Crystal structure of bis(L-asparaginium hydrogensquarate) monohydrate
Yadav, Harsh; Sinha, Nidhi; Goel, Sahil; Singh, Budhendra; Bdikin, Igor; Saini, Anupama; Gopalaiah, Kovuru; Kumar, Binay; Acta Crystallographica, Section B 73 (2017) 347–359; doi:10.1107/S2052520617002906

data_2108049
_publ_contact_author_address
;
Department of Physics & Electronics, SGTB Khalsa College, University of Delhi,
Delhi 110007,
India
;
_publ_contact_author_email       nidhisinha5@yahoo.co.in
_publ_contact_author_name        'Nidhi Sinha'
_publ_contact_author_phone       +91-9818662161
_publ_section_title
;
 Crystal structure of bis(L-asparaginium hydrogensquarate) monohydrate
;
_journal_coeditor_code           BP5095
_journal_date_accepted           2017-02-21
_journal_date_recd_electronic    2016-12-03
_journal_issue                   3
_journal_name_full               'Acta Crystallographica, Section B'
_journal_page_first              347
_journal_page_last               359
_journal_paper_category          FA
_journal_paper_doi               10.1107/S2052520617002906
_journal_volume                  73
_journal_year                    2017
_chemical_formula_moiety         'C4 H9 N2 O3, C4 H O4, 0.5(H2 O)'
_chemical_formula_sum            'C8 H11 N2 O7.5'
_chemical_formula_weight         255.19
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7808(13)
_cell_length_b                   8.9659(6)
_cell_length_c                   6.0713(4)
_cell_measurement_reflns_used    2347
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1602
_cell_measurement_theta_min      3.3556
_cell_volume                     1076.76(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5216
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.160
_diffrn_reflns_theta_min         3.356
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       Block
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.157
_refine_ls_abs_structure_details
;
 Flack x determined using 882 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_coef       0.018(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0410P)^2^+0.1760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                2394
_reflns_number_total             2531
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bp5095sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-09-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C16 H22 N4 O15'
_cod_original_formula_weight         510.38
_cod_original_formula_moiety         '2(C4 H9 N2 O3), 2(C4 H O4), H2 O'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        1076.75(12)
_cod_database_code               2108049
_shelx_hkl_checksum              5692
_shelx_res_checksum              59566
_cod_database_fobs_code 2108049