3d-4f magnetic exchange interactions and anisotropy in a series of heterobimetallic vanadium(IV)-lanthanide(III) Schiff base complexes
Kotrle, Kamil; Nemec, Ivan; Moncol, Jan; Cizmar, Erik; Herchel, Radovan; Dalton Transactions  (2021) –; doi:10.1039/D1DT01944A

data_7708099
_publ_section_title
;
 3d-4f magnetic exchange interactions and anisotropy in a series of
 heterobimetallic vanadium(IV)-lanthanide(III) Schiff base complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT01944A
_journal_year                    2021
_chemical_formula_moiety         'C19 H22 Er N5 O15 V'
_chemical_formula_sum            'C19 H22 Er N5 O15 V'
_chemical_formula_weight         778.61
_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
_audit_creation_date             2021-05-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-13 deposited with the CCDC.	2021-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.3123(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7195(3)
_cell_length_b                   16.4891(3)
_cell_length_c                   10.05652(18)
_cell_measurement_reflns_used    8176
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.1310
_cell_measurement_theta_min      2.6500
_cell_volume                     2602.30(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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     -8.00  41.00   0.50    0.60    --   44.18 -46.00  -9.00   98
  2  \w      9.00  62.00   0.50    0.60    --   44.18 -54.00 -90.00  106
  3  \w     15.00  40.00   0.50    0.60    --   44.18 -43.00-180.00   50
  4  \w     -9.00  37.00   0.50    0.60    --   44.18 -32.00-180.00   92
  5  \w     86.00 112.00   0.50    2.50    --   95.94  42.00-120.00   52
  6  \w    119.00 162.00   0.50    2.50    --   95.94  42.00-120.00   86
  7  \w     83.00 139.00   0.50    2.50    --   95.94  25.00-120.00  112
  8  \w     65.00 111.00   0.50    0.60    --   44.18 138.00 -60.00   92
  9  \w     68.00  93.00   0.50    0.60    --   44.18 138.00 -30.00   50
 10  \w     66.00 109.00   0.50    0.60    --   44.18 138.00  30.00   86
 11  \w     78.00 152.00   0.50    2.50    --   95.94  46.00 140.00  148
 12  \w     73.00  98.00   0.50    2.50    --   95.94 -96.00 120.00   50
 13  \w     23.00  58.00   0.50    2.50    --   95.94 -96.00 120.00   70
 14  \w     30.00  56.00   0.50    2.50    --   95.94 -50.00 -30.00   52
 15  \w     32.00  83.00   0.50    2.50    --   95.94 -68.00-120.00  102
 16  \w     30.00 110.00   0.50    2.50    --   95.94-117.00 -60.00  160
 17  \w     27.00  86.00   0.50    0.60    --   44.18  46.00 140.00  118
 18  \w    -26.00  29.00   0.50    0.60    --  -42.62  21.00  90.00  110
 19  \w    -27.00  18.00   0.50    0.60    --  -42.62  21.00 -30.00   90
 20  \w    -54.00 -29.00   0.50    2.50    --  -94.38  59.00 -60.00   50
 21  \w    -53.00 -28.00   0.50    2.50    --  -94.38  50.00   0.00   50
 22  \w    -57.00 -32.00   0.50    2.50    --  -94.38  50.00  30.00   50
 23  \w    -69.00 -40.00   0.50    2.50    --  -94.38  59.00  60.00   58
 24  \w    -69.00 -37.00   0.50    2.50    --  -94.38  59.00 120.00   64
 25  \w    -82.00 -26.00   0.50    2.50    --  -94.38  68.00  60.00  112
 26  \w    -43.00 -18.00   0.50    0.60    --  -42.62  46.00 140.00   50
 27  \w    -19.00   7.00   0.50    0.60    --   44.18 -21.00 -30.00   52
 28  \w     -2.00  26.00   0.50    0.60    --   44.18 -21.00 -90.00   56
 29  \w    -90.00 -65.00   0.50    0.60    --  -42.62 -46.00  -9.00   50
 30  \w   -116.00 -81.00   0.50    2.50    --  -94.38 -33.00 -60.00   70
 31  \w   -126.00 -88.50   0.50    2.50    --  -94.38 -46.00  -9.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15025
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.273
_diffrn_reflns_theta_min         2.816
_exptl_absorpt_coefficient_mu    9.583
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.987
_exptl_crystal_description       prism
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.255
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4732
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0463P)^2^+7.5952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4419
_reflns_number_total             4732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01944a2.cif
_cod_data_source_block           4_VEr
_cod_database_code               7708099
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N4-O15 \\sim N4-O14 \\sim N4-O15A \\sim N4-O14A
 with sigma of 0.02
 N4-O13 \\sim N4-O13B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O13 \\sim O13B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(O15) = Uanis(O15A) = Uanis(O14) = Uanis(O14A)
4. Others
 Sof(O14A)=Sof(O15A)=Sof(O13B)=1-FVAR(1)
 Sof(O13)=Sof(O14)=Sof(O15)=FVAR(1)
5.a Rotating group:
 O3(H3A,H3B)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C13(H13), C14(H14), C15(H15)
5.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              45750
_shelx_hkl_checksum              38118
_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
;