Oxamate-based potassium–organic assembly with the uncommon binodal (6,12)-coordinated alb topology
Simosono, Cintia A.; Flores, Leonã S.; Simões, Tatiana R. G.; do Pim, Walace D.; Julve, Miguel; Marinho, Maria Vanda; CrystEngComm 27 (2025) 176–183; doi:10.1039/D4CE01066C

data_7249650
_publ_section_title
;
 Oxamate-based potassium--organic assembly with the uncommon binodal
 (6,12)-coordinated alb topology
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              176
_journal_page_last               183
_journal_paper_doi               10.1039/D4CE01066C
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C5 H3 K N O3'
_chemical_formula_sum            'C5 H3 K N O3'
_chemical_formula_weight         164.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc25mwmb
_audit_creation_date             2020-07-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-07-08 deposited with the CCDC.	2024-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.2425(2)
_cell_length_b                   26.0431(9)
_cell_length_c                   6.4409(2)
_cell_measurement_reflns_used    8304
_cell_measurement_temperature    292.92(10)
_cell_measurement_theta_max      28.5290
_cell_measurement_theta_min      4.2100
_cell_volume                     1214.86(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.92(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2923
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -61.00  40.00   1.00    7.88    --   11.79 -57.00   0.00  101
  2  \w    -20.00  53.00   1.00    7.88    --   11.79 -99.00-120.00   73
  3  \w    -16.00  85.00   1.00    7.88    --   11.79  57.00 -60.00  101
  4  \w    -16.00  85.00   1.00    7.88    --   11.79  57.00 150.00  101
  5  \w    -13.00  86.00   1.00    7.88    --   11.79  38.00  60.00   99
  6  \w    -20.00  53.00   1.00    7.88    --   11.79 -99.00 150.00   73
  7  \w    -20.00  53.00   1.00    7.88    --   11.79 -99.00 120.00   73
  8  \w    -15.00  56.00   1.00    7.88    --   11.79-105.00 -43.00   71
  9  \w     34.00  99.00   1.00    7.88    --   11.79-178.00  30.00   65
 10  \w    -20.00  29.00   1.00    7.88    --  -12.03 -99.00 150.00   49
 11  \w    -20.00  23.00   1.00    7.88    --   11.79 -99.00  60.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0244805000
_diffrn_orient_matrix_UB_12      -0.0261066000
_diffrn_orient_matrix_UB_13      0.0151731000
_diffrn_orient_matrix_UB_21      0.0129398000
_diffrn_orient_matrix_UB_22      -0.0029224000
_diffrn_orient_matrix_UB_23      -0.1084820000
_diffrn_orient_matrix_UB_31      0.0939519000
_diffrn_orient_matrix_UB_32      0.0072157000
_diffrn_orient_matrix_UB_33      0.0109892000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            25240
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.775
_diffrn_reflns_theta_min         3.258
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0293P)^2^+0.9832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1492
_reflns_number_total             1697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01066c2.cif
_cod_data_source_block           cis042_a
_cod_depositor_comments          'Adding full bibliography for 7249650.cif.'
_cod_database_code               7249650
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.815
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C4(H4), C6(H6), C5(H5)
;
_shelx_res_checksum              72586
_olex2_date_sample_data_collection 2016-08-24
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.206
_oxdiff_exptl_absorpt_empirical_full_min 0.822