Mechanochemical Synthesis and Micro-Electron Diffraction Analysis of Rare Earth-Aminopolycarboxylate Coordination Compounds
Celik, Ecem; LeMagueres, Pierre; Reinheimer, Eric W.; Carter, Korey Prescott; Forbes, Tori; CrystEngComm  (2025) –; doi:10.1039/D5CE00935A

data_7251268
_publ_section_title
;
 Mechanochemical Synthesis and Micro-Electron Diffraction Analysis of Rare
 Earth-Aminopolycarboxylate Coordination Compounds
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE00935A
_journal_year                    2025
_chemical_formula_moiety         'C5 H12 Cl La N O7, Cl'
_chemical_formula_sum            'C5 H12 Cl2 La N O7'
_chemical_formula_weight         407.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-09-17
_audit_creation_method
;
Olex2 1.5-ac7-014
(compiled 2025.02.27 svn.r6f4c0eaf for Rigaku Oxford Diffraction, GUI svn.r7171)
;
_audit_update_record
;
2025-09-25 deposited with the CCDC.	2025-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.45(8)
_cell_length_b                   15.87(9)
_cell_length_c                   16.42(15)
_cell_measurement_reflns_used    2959
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.8960
_cell_measurement_theta_min      0.1190
_cell_volume                     2463(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.100a 64-bit (release 06-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac7-014 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-014 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-ED
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.915
_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    -50.00  40.00   0.25    0.25    --    0.00   0.00   0.00  360
  2  \w    -40.00  60.00   0.25    0.12    --    0.00   0.00   0.00  400
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0008551000
_diffrn_orient_matrix_UB_12      -0.0006244000
_diffrn_orient_matrix_UB_13      0.0013118000
_diffrn_orient_matrix_UB_21      0.0024594000
_diffrn_orient_matrix_UB_22      0.0001006000
_diffrn_orient_matrix_UB_23      0.0005757000
_diffrn_orient_matrix_UB_31      -0.0005247000
_diffrn_orient_matrix_UB_32      0.0014508000
_diffrn_orient_matrix_UB_33      0.0005286000
_diffrn_radiation_monochromator  'transmission electron microscope'
_diffrn_radiation_probe          electron
_diffrn_radiation_type           'transmission electron microscope'
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.3008
_diffrn_reflns_av_unetI/netI     0.1613
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17875
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.899
_diffrn_reflns_theta_min         0.099
_diffrn_source                   'transmission electron microscope'
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.98a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    2.200
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       2154(41)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   2.230
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2302
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      2.188
_refine_ls_R_factor_all          0.2290
_refine_ls_R_factor_gt           0.2030
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4412
_refine_ls_wR_factor_ref         0.4491
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1864
_reflns_number_total             2302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00935a2.cif
_cod_data_source_block           merged_1016_1019
_cod_original_cell_volume        2464(34)
_cod_database_code               7251268
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'La O C H N'
_diffrn_oxdiff_scatteringfactors_ed
;
UCLA (2022) https://srv.mbi.ucla.edu/faes/data
;
_diffrn_oxdiff_ac3_digest_hkl    01d623080971eb451aaf0244b240dfde959370
_diffrn_oxdiff_digest_hkl
;
019b5198d915ba2f89f8e7fa7f47a21a7c0732
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Rotating group:
 O3(H3A,H3B), O2(H2A,H2B), O1(H1A,H1B)
3.b Secondary CH2 refined with riding coordinates:
 C00D(H00A,H00B), C2(H2C,H2D), C3(H3C,H3D)
;
_shelx_res_checksum              62073
_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 4.878
_oxdiff_exptl_absorpt_empirical_full_min 0.316