Multipolar model and Hirshfeld atom refinement of tetraaquabis(hydrogenmaleato)iron(II).
Ferreira Guimarães, Hellen; Lages Rodrigues, Bernardo; Acta crystallographica Section B, Structural science, crystal engineering and materials 81 (2025) –; doi:10.1107/S2052520625003403

data_2312836
_publ_section_title
;
 Multipolar model and Hirshfeld atom refinement of
 tetraaquabis(hydrogenmaleato)iron(II).
;
_journal_issue                   3
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_paper_doi               10.1107/S2052520625003403
_journal_volume                  81
_journal_year                    2025
_chemical_formula_moiety         'C4 H7 Fe0.5 O6'
_chemical_formula_sum            'C4 H7 Fe0.5 O6'
_chemical_formula_weight         179.019
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2025-02-05
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2025.01.22 svn.rc7346086 for OlexSys, GUI svn.r7128)
;
_cell_angle_alpha                108.907(1)
_cell_angle_beta                 105.498(1)
_cell_angle_gamma                92.310(1)
_cell_formula_units_Z            2
_cell_length_a                   5.2066(1)
_cell_length_b                   7.3264(1)
_cell_length_c                   9.2475(1)
_cell_measurement_reflns_used    13896
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      79.0550
_cell_measurement_theta_min      2.4250
_cell_volume                     318.455(9)
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9818
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9818
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13896
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9818
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         79.60
_diffrn_reflns_theta_min         2.44
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.250
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             184.538
_refine_diff_density_max         0.5035
_refine_diff_density_min         -0.7267
_refine_diff_density_rms         0.0612
_refine_ls_d_res_high            0.3613
_refine_ls_d_res_low             8.3552
_refine_ls_extinction_coef       0.030(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.1446
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     161
_refine_ls_number_reflns         13896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1446
_refine_ls_R_factor_all          0.0176
_refine_ls_R_factor_gt           0.0174
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0067P)^2^+0.0088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0478
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              18
_reflns_limit_k_min              -20
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                13721
_reflns_number_total             13896
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            woz5002.cif
_cod_data_source_block           HAR
_cod_database_code               2312836
_olex2_refinement_description
;
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
- for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         PBE0
   BASIS SET:      cc-pVTZ
   CHARGE:         0
   MULTIPLICITY:   5
   DATE:           2025-02-05_15-17-27
;
_olex2_submission_special_instructions 'No special instructions were received'