Magnetic behaviour of a spin-canted asymmetric lanthanide quinolate trimer.
Batista, Lester; Paul, Sagar; Molina-Jirón, Concepción; Jaén, Juan A; Fensker, Dieter; Fuhr, Olaf; Ruben, Mario; Wernsdorfer, Wolfgang; Moreno-Pineda, Eufemio; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12927–12935; doi:10.1039/d4dt01588f

data_7716649
_publ_section_title
;
 Magnetic behaviour of a spin-canted asymmetric lanthanide quinolate
 trimer.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12927
_journal_page_last               12935
_journal_paper_doi               10.1039/d4dt01588f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C63 H44 Dy3 N9 O14, 2.5(C2 H3 N)'
_chemical_formula_sum            'C68 H51.5 Dy3 N11.5 O14'
_chemical_formula_weight         1741.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-26 deposited with the CCDC.	2024-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                76.207(3)
_cell_angle_beta                 72.362(2)
_cell_angle_gamma                88.591(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6383(4)
_cell_length_b                   16.6621(6)
_cell_length_c                   18.2109(6)
_cell_measurement_reflns_used    30254
_cell_measurement_temperature    180
_cell_measurement_theta_max      31.84
_cell_measurement_theta_min      1.21
_cell_volume                     3264.0(2)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.1, Darmstadt 2022
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      180
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
 854 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44608
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.209
_diffrn_source                   Axo_Mo
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_target            Mo
_diffrn_source_type              'microfocus sealed X-ray tube'
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    3.474
_exptl_absorpt_correction_T_max  0.8403
_exptl_absorpt_correction_T_min  0.5933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         15673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0168P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0477
_refine_ls_wR_factor_ref         0.0487
_reflns_d_resolution_high        0.659
_reflns_d_resolution_low         16.837
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              17
_reflns_limit_h_min              -9
_reflns_limit_k_max              24
_reflns_limit_k_min              -24
_reflns_limit_l_max              27
_reflns_limit_l_min              -27
_reflns_number_gt                11004
_reflns_number_total             15673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01588f2.cif
_cod_data_source_block           em-dy
_cod_depositor_comments          'Adding full bibliography for 7716649.cif.'
_cod_original_formula_sum        'C68 H51.50 Dy3 N11.50 O14'
_cod_database_code               7716649
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.845
_shelx_estimated_absorpt_t_min   0.624
_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, All O(H,H) groups
2. Others
 Fixed Sof: N12(0.5) C68(0.5) C69(0.5) H69A(0.5) H69B(0.5) H69C(0.5)
3.a Rotating group:
 O14(H14A,H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24),
  C25(H25), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C46(H46), C47(H47),
  C48(H48), C50(H50), C51(H51), C52(H52), C55(H55), C56(H56), C57(H57),
 C59(H59), C60(H60), C61(H61)
3.c Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C65(H65A,H65B,H65C)
;
_shelx_res_checksum              11656
_shelx_hkl_checksum              35496
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '60.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '8.0 cm'
_stoe_detector_size_y            '7.7 cm'
_stoe_evaluation_integration_a   8.0
_stoe_evaluation_integration_b   0.1
_stoe_evaluation_integration_ems 0.011
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 91.1
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 65.3
_stoe_evaluation_lana_max_2theta_desired 65.3
_stoe_evaluation_lana_mean_redundancy 2.6
_stoe_evaluation_lana_number_refls_after_or 57075
_stoe_evaluation_lana_number_refls_outliers 3737
_stoe_evaluation_lana_number_refls_total 60812
_stoe_evaluation_lana_number_refls_unique 21792
_stoe_evaluation_lana_number_refls_written 57075
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group -1
_stoe_evaluation_lana_table
;
2Theta           5.1   12.3   19.5   26.7   33.9   41.1   48.3   55.5   62.7
<Resolution>    6.07   3.13   2.04   1.54   1.21   1.01   0.87   0.76   0.70
N(total)         348   1497   3557   4945   7186  10502  12587  13319   6871
<Redundancy>     3.8    3.6    3.7    3.0    2.8    3.0    2.7    2.4    1.9
Complet. [%%]   100.0  100.0   99.9   96.9   98.8   99.9   99.9   99.5   64.2
<I/sigma>       63.6   39.9   26.8   18.5    9.8    6.1    3.5    1.9    1.0
R(int)         0.014  0.013  0.016  0.019  0.030  0.042  0.067  0.113  0.199
;
_stoe_measurement_identifier     EM-Dy
_stoe_measurement_max_exposure_per_frame '2.0 s'
_stoe_measurement_mean_exposure_per_frame '2.0 s'
_stoe_measurement_min_exposure_per_frame '2.0 s'
_stoe_measurement_total_exposure_time '28 min'
_stoe_measurement_total_frame_number 854
_stoe_measurement_total_run_number 14
_stoe_measurement_tube_power     '49.8 W'