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_7713223
_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 O20 Tm2'
_chemical_formula_sum            'C12 H16 O20 Tm2'
_chemical_formula_weight         818.11
_chemical_name_common            '[Tm2(C4O4)3(H2O)8]n'
_chemical_name_systematic        'thulium(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     iterative
_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                 95.876(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9240(4)
_cell_length_b                   8.1318(2)
_cell_length_c                   9.9899(4)
_cell_measurement_reflns_used    5578
_cell_measurement_temperature    295.8(2)
_cell_measurement_theta_max      31.1030
_cell_measurement_theta_min      2.5040
_cell_volume                     963.57(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_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
'olex2.solve 1.5-ac5-018 (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.8(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.869
_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    -17.00  28.00   0.50    1.00    --  -15.72 -99.00  30.00   90
  2  \w    -27.00  28.00   0.50    1.00    --   14.78 -55.00-163.00  110
  3  \w     47.00  76.00   0.50    1.00    --   14.78 178.00-180.00   58
  4  \w    -11.00  90.00   0.50    1.00    --   14.78  55.00 -20.00  202
  5  \w      7.00  67.00   0.50    1.00    --  -15.72  19.00  30.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0548924000
_diffrn_orient_matrix_UB_12      -0.0019653000
_diffrn_orient_matrix_UB_13      0.0213995000
_diffrn_orient_matrix_UB_21      -0.0170262000
_diffrn_orient_matrix_UB_22      -0.0572811000
_diffrn_orient_matrix_UB_23      -0.0516881000
_diffrn_orient_matrix_UB_31      0.0164815000
_diffrn_orient_matrix_UB_32      -0.0658014000
_diffrn_orient_matrix_UB_33      0.0442965000
_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  0.0133
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6810
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.404
_diffrn_reflns_theta_min         2.505
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.257
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.35a (Rigaku Oxford Diffraction, 2021)
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    2.820
_exptl_crystal_description       prism
_exptl_crystal_F_000             772
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.873
_refine_diff_density_min         -1.334
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.766(19)
_refine_ls_extinction_coef       0.00152(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         3610
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0182
_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^)+(0.0337P)^2^+0.2347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0546
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.869
_reflns_number_gt                3297
_reflns_number_total             3610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03878a2.cif
_cod_data_source_block           tmoac_sq_20211213_autored
_cod_original_cell_volume        963.56(5)
_cod_database_code               7713223
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C12H16O20Tm2
_shelx_estimated_absorpt_t_max   0.607
_shelx_estimated_absorpt_t_min   0.181
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.234(19)
 0.766(19)
2. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 Tm2-H18A \\sim Tm2-H18B
 with sigma of 0.02
 Tm1-H15A \\sim Tm1-H15B
 with sigma of 0.02
 Tm2-H19A \\sim Tm2-H19B
 with sigma of 0.02
 Tm1-H16A \\sim Tm1-H16B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C1, C2, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Free rotating group:
 O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B), O18(H18A,H18B), O19(H19A,H19B)
6.b Rotating group:
 O13(H13A,H13B), O17(H17A,H17B), O20(H20A,H20B)
;
_shelx_res_checksum              74779
_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 2.220
_oxdiff_exptl_absorpt_empirical_full_min 0.730