Orthogonal magnetic orbitals in high spin Cu-VO units: structure, magnetism and EPR study of anisotropic heterometallic complexes.
Deng, Qing-Song; Zhang, Yu-Shuang; Wang, Ye-Xin; Xie, Yi; Fu, Peng-Xiang; Gao, Song; Liu, Zheng; Jiang, Shang-Da; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13207–13215; doi:10.1039/d4dt01346h

data_7716687
_publ_section_title
;
 Orthogonal magnetic orbitals in high spin Cu-VO units: structure,
 magnetism and EPR study of anisotropic heterometallic complexes.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13207
_journal_page_last               13215
_journal_paper_doi               10.1039/d4dt01346h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C40 H32 Cu2 N4 O14 V2'
_chemical_formula_sum            'C40 H32 Cu2 N4 O14 V2'
_chemical_formula_weight         1021.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-31
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-05 deposited with the CCDC.	2024-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.576(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.1187(8)
_cell_length_b                   10.8875(4)
_cell_length_c                   18.4955(7)
_cell_measurement_reflns_used    6108
_cell_measurement_temperature    303.58(17)
_cell_measurement_theta_max      30.7900
_cell_measurement_theta_min      2.1400
_cell_volume                     3817.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.30a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.30a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.30a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      303.58(17)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.807
_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    -63.00  17.00   0.50    4.57    --   -4.92   0.00  60.00  160
  2  \w    -16.00  27.00   0.50    4.57    --   -4.92 -99.00  60.00   86
  3  \w      0.00  34.00   0.50    4.57    --    3.98 -99.00 -90.00   68
  4  \w    -61.00  -5.00   0.50    4.57    --    3.98 -57.00-120.00  112
;
_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      -0.0080965000
_diffrn_orient_matrix_UB_12      0.0611549000
_diffrn_orient_matrix_UB_13      -0.0133045000
_diffrn_orient_matrix_UB_21      0.0079560000
_diffrn_orient_matrix_UB_22      -0.0146227000
_diffrn_orient_matrix_UB_23      -0.0335483000
_diffrn_orient_matrix_UB_31      -0.0356595000
_diffrn_orient_matrix_UB_32      -0.0171477000
_diffrn_orient_matrix_UB_33      -0.0187850000
_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  0.0262
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.807
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14216
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.837
_diffrn_reflns_theta_min         2.149
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.653
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.30a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0542P)^2^+4.3266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3619
_reflns_number_total             4840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01346h2.cif
_cod_data_source_block           8-14-t4-z_auto
_cod_depositor_comments
'Adding full bibliography for 7716686--7716689.cif.'
_cod_database_code               7716687
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHONCuV
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C12(H12), C8(H8), C9(H9), C14(H14), C17(H17)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              66792
_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 1.530
_oxdiff_exptl_absorpt_empirical_full_min 0.723