A cost-effective and innovative detector for iron ions.
Guo, Yanhui; Zhu, Jiayi; Dai, Yumei; Chen, Long; Li, Weibing; Yuan, Zihang; Zhou, Jie; Tang, En; RSC advances 15 (2025) 2645–2650; doi:10.1039/d4ra08065c

data_7249859
_publ_section_title
;
 A cost-effective and innovative detector for iron ions.
;
_journal_issue                   4
_journal_name_full               'RSC advances'
_journal_page_first              2645
_journal_page_last               2650
_journal_paper_doi               10.1039/d4ra08065c
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C30 H24 N4 O11 Zn2, 1.1[H2O]'
_chemical_formula_sum            'C30 H26.2 N4 O12.1 Zn2'
_chemical_formula_weight         747.27
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-01-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-01-18 deposited with the CCDC.	2025-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.963(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.1729(9)
_cell_length_b                   8.4424(4)
_cell_length_c                   17.3538(6)
_cell_measurement_reflns_used    15950
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.1330
_cell_measurement_theta_min      3.9250
_cell_volume                     2991.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0606
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -47.00  30.00   1.00    2.00    --   15.65 -57.00 -60.00   77
  2  \w    -10.00  16.00   1.00    2.00    --  -16.59 -99.00 -60.00   26
  3  \w    -22.00   4.00   1.00    2.00    --  -16.59 -99.00-120.00   26
  4  \w    -22.00  21.00   1.00    2.00    --  -16.59 -99.00-180.00   43
  5  \w    -49.00  32.00   1.00    2.00    --   15.65 -57.00 -90.00   81
  6  \w    -32.00  41.00   1.00    2.00    --   15.65 -92.00  61.00   73
  7  \w    -20.00  17.00   1.00    2.00    --  -16.59 -92.00  61.00   37
  8  \w    -47.00  31.00   1.00    2.00    --   15.65 -57.00-180.00   78
  9  \w     56.00  88.00   1.00    2.00    --   15.65 178.00-120.00   32
 10  \w    -13.00  12.00   1.00    2.00    --  -16.59  92.00 173.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0073737000
_diffrn_orient_matrix_UB_12      -0.0757041000
_diffrn_orient_matrix_UB_13      0.0037379000
_diffrn_orient_matrix_UB_21      -0.0142455000
_diffrn_orient_matrix_UB_22      -0.0357560000
_diffrn_orient_matrix_UB_23      -0.0157199000
_diffrn_orient_matrix_UB_31      0.0066879000
_diffrn_orient_matrix_UB_32      0.0072801000
_diffrn_orient_matrix_UB_33      -0.0375082000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28195
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         3.511
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.674
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1520
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         5663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0192P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4540
_reflns_number_total             5663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra08065c2.cif
_cod_data_source_block           2396827
_cod_database_code               7249859
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.850
_shelx_estimated_absorpt_t_min   0.680
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C12(H12), C14(H14), C16(H16), C21(H21), C22(H22),
 C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C20(H20A,H20B,H20C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 44 electrons were 
found in a volume of 244\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.1[H2O] per Asymmetric Unit 
which account for 44 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              28667
_shelx_hkl_checksum              17456
_shelx_fab_checksum              99381
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.011
_oxdiff_exptl_absorpt_empirical_full_min 0.623