Tetra-<i>n</i>-butylammonium orotate monohydrate: knowledge-based comparison of the results of accurate and lower-resolution analyses and a non-routine disorder refinement
Ara, Irene; Basdouri, Zeineb; Falvello, Larry R.; Graia, Mohsen; Guerra, Pablo; Tomás, Milagros; Acta Crystallographica Section E 75 (2019) 1632–1637; doi:10.1107/S2056989019013380

data_2243125
_publ_section_title
;
 Tetra-<i>n</i>-butylammonium orotate monohydrate: knowledge-based
 comparison of the results of accurate and lower-resolution analyses and a
 non-routine disorder refinement
;
_journal_coeditor_code           HB7858
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1632
_journal_page_last               1637
_journal_paper_doi               10.1107/S2056989019013380
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C16 H36 N +, C5 H3 N2 O4 -, H2 O'
_chemical_formula_moiety         'C16 H36 N +, C5 H3 N2 O4 -, H2 O'
_chemical_formula_sum            'C21 H41 N3 O5'
_chemical_formula_weight         415.57
_chemical_name_common
;
Tetra-<i>n</i>-butylammonium orotate monohydrate
;
_chemical_name_systematic
;
Tetra-<i>n</i>-butylammonium
2,6-dioxo-1,2,3,6-tetrahydropyrimidine-4-carboxylate 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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 97.347(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0905(5)
_cell_length_b                   14.8664(8)
_cell_length_c                   16.1261(9)
_cell_measurement_reflns_used    17418
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.1520
_cell_measurement_theta_min      1.9880
_cell_volume                     2399.2(2)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2018)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2007) and
Mercury (Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
<i>SHELXL2018/1</i> (Sheldrick, 2015b), WinGX (Farrugia, 2012),
<i>CrystalExplorer</i> (Spackman & Jayatilaka, 2009)
;
_computing_structure_refinement
;
<i>SHELXL2018/1</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26211
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.143
_diffrn_reflns_theta_min         1.870
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2018)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       irregular
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         6560
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0533P)^2^+0.9257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                5274
_reflns_number_total             6560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7858sup1.cif
_cod_data_source_block           100K
_cod_database_code               2243125
_cod_database_fobs_code          2243125
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.987
_shelx_hkl_checksum              96670
_shelx_res_checksum              28439