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_7708101
_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 Dy N5 O15 V'
_chemical_formula_sum            'C19 H22 Dy N5 O15 V'
_chemical_formula_weight         773.85
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-12
_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                 96.3710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0536(3)
_cell_length_b                   16.8695(3)
_cell_length_c                   9.9480(2)
_cell_measurement_reflns_used    172105
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.08
_cell_volume                     2510.66(8)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.3 (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 1.84, Darmstadt 2018
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS3R 300K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
 3262 frames, detector distance = 50 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe Stadivari with Incoatec Ag HB'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.2 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_type           'Ag K\a'
_diffrn_radiation_wavelength     0.56083
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            44181
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        19.664
_diffrn_reflns_theta_max         20.518
_diffrn_reflns_theta_min         2.187
_diffrn_source                   'Incoatec HB I\ms 2.0'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_type              'Incoatec Ag tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.814
_exptl_absorpt_correction_T_max  0.9655
_exptl_absorpt_correction_T_min  0.3099
_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, Acta Chimica Slovaca, 9, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.047
_exptl_crystal_description       plate
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.900
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5130
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+4.6313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4699
_reflns_number_total             5130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01944a2.cif
_cod_data_source_block           3_VDy
_cod_database_code               7708101
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.736
_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
2. Shared sites
{C10A, C10B}
3. Restrained distances
 O3-H3B
 0.85 with sigma of 0.01
 O3-H3A
 0.85 with sigma of 0.01
 H3A-H3B
 1.35 with sigma of 0.02
 C9A-C10A \\sim C9B-C10B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C10A) = Uanis(C10B)
5. Others
 Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(C10B)=Sof(H10C)=
 Sof(H10D)=1-FVAR(1)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=
 Sof(H10B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C8A(H8AA,H8AB), C9A(H9AA,H9AB), C10A(H10A,H10B), C8B(H8BA,H8BB), C9B(H9BA,
 H9BB), C10B(H10C,H10D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C13(H13), C14(H14), C15(H15)
6.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              71105
_shelx_hkl_checksum              68163
_olex2_submission_special_instructions 'No special instructions were received'