Bilayered lanthanide squarate hydrates (Ln = Eu to Lu) and magnetization reversal barriers of 21 K for Ln = Tm and 57 K for Yb.
Takano, Rina; Masuda, Koki; Cho, Keigo; Kitagawa, Yasutaka; Ishida, Takayuki; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d2dt03878a

data_7713218
_publ_section_title
;
 Bilayered lanthanide squarate hydrates (Ln = Eu to Lu) and magnetization
 reversal barriers of 21 K for Ln = Tm and 57 K for Yb.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt03878a
_journal_year                    2023
_chemical_formula_moiety         'C12 H16 Eu2 O20'
_chemical_formula_sum            'C12 H16 Eu2 O20'
_chemical_formula_weight         784.17
_chemical_name_common            '[Eu2(C4O4)3(H2O)8]n'
_chemical_name_systematic        'europium(III) squarate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-09
_audit_creation_method
;
Olex2 1.5-ac5-018
(compiled 2021.09.08 svn.r13c46975 for Rigaku Oxford Diffraction, GUI svn.r6396)
;
_audit_update_record
;
2022-11-10 deposited with the CCDC.	2023-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.017(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9363(9)
_cell_length_b                   8.2215(5)
_cell_length_c                   10.1229(7)
_cell_measurement_reflns_used    2856
_cell_measurement_temperature    296.3(3)
_cell_measurement_theta_max      30.0130
_cell_measurement_theta_min      2.9500
_cell_volume                     987.93(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.3(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.841
_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     49.00  84.00   0.50    5.42    --   -5.40  45.00 150.00   70
  2  \w    -94.00  83.00   0.50    5.42    --   -5.40  45.00  90.00  354
  3  \w    -46.00  26.00   0.50    5.42    --   -5.40  45.00 150.00  144
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0153061000
_diffrn_orient_matrix_UB_12      -0.0790105000
_diffrn_orient_matrix_UB_13      0.0198603000
_diffrn_orient_matrix_UB_21      0.0575420000
_diffrn_orient_matrix_UB_22      -0.0233886000
_diffrn_orient_matrix_UB_23      0.0065992000
_diffrn_orient_matrix_UB_31      0.0054219000
_diffrn_orient_matrix_UB_32      0.0252249000
_diffrn_orient_matrix_UB_33      0.0673162000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7654
_diffrn_reflns_point_group_measured_fraction_full 0.869
_diffrn_reflns_point_group_measured_fraction_max 0.664
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.077
_diffrn_reflns_theta_min         2.477
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    6.397
_exptl_absorpt_correction_T_max  0.06682
_exptl_absorpt_correction_T_min  0.04018
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.90a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.636
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.379
_exptl_crystal_size_mid          0.328
_exptl_crystal_size_min          0.049
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         1.489
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.10(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         3858
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0689P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1112
_reflns_Friedel_coverage         0.576
_reflns_Friedel_fraction_full    0.743
_reflns_Friedel_fraction_max     0.486
_reflns_number_gt                3114
_reflns_number_total             3858
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03878a2.cif
_cod_data_source_block           eu_sq_210810
_cod_database_code               7713218
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C7H6EuO9
_shelx_estimated_absorpt_t_max   0.745
_shelx_estimated_absorpt_t_min   0.195
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Eu1-H16A \\sim Eu1-H16B
 with sigma of 0.02
 Eu2-H18A \\sim Eu2-H18B
 with sigma of 0.02
 Eu1-H15A \\sim Eu1-H15B
 with sigma of 0.02
 Eu2-H19A \\sim Eu2-H19B
 with sigma of 0.02
3.a Free rotating group:
 O15(H15A,H15B), O16(H16A,H16B), O18(H18A,H18B), O19(H19A,H19B)
3.b Rotating group:
 O13(H13A,H13B), O14(H14A,H14B), O17(H17A,H17B), O20(H20A,H20B)
;
_shelx_res_checksum              37304
_olex2_submission_original_sample_id Eu_squarate
_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 1.494
_oxdiff_exptl_absorpt_empirical_full_min 0.821