Unprecedented Water Effect as a Key Element in Salicyl-Glycine Schiff Base Synthesis.
Bakalorz, Karolina; Przypis, Łukasz; Tomczyk, Mateusz Michał; Książek, Maria; Grzesik, Ryszard; Kuźnik, Nikodem; Molecules (Basel, Switzerland) 25 (2020) 1257–; doi:10.3390/molecules25051257

data_1557746
_publ_section_title
;
 Unprecedented Water Effect as a Key Element in Salicyl-Glycine Schiff
 Base Synthesis.
;
_journal_issue                   5
_journal_name_full               'Molecules (Basel, Switzerland)'
_journal_page_first              1257
_journal_paper_doi               10.3390/molecules25051257
_journal_volume                  25
_journal_year                    2020
_chemical_formula_moiety         'C9 H9 K N O4'
_chemical_formula_sum            'C9 H9 K N O4'
_chemical_formula_weight         234.27
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 99.765(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.879(3)
_cell_length_b                   6.2395(6)
_cell_length_c                   8.7555(9)
_cell_measurement_reflns_used    963
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      68.9840
_cell_measurement_theta_min      4.6950
_cell_volume                     1016.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41q (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(1)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type
;
SuperNova diffractometer (Agilent Technologies) with Atlas detector
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3619
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         58.816
_diffrn_reflns_theta_min         4.753
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.567
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41q (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         1350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0615
_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^)+(0.1067P)^2^+0.3216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                972
_reflns_number_total             1350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Kuznik-1a-1b.cif
_cod_data_source_block           1b_psl19_nk1_glysal_3a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1557746
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.740
_shelx_estimated_absorpt_t_max   0.956
_shelx_res_checksum              80753
_shelx_hkl_checksum              88333