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_7716688
_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         'C36 H20 Cl4 Cu2 N4 O14 V2'
_chemical_formula_sum            'C36 H20 Cl4 Cu2 N4 O14 V2'
_chemical_formula_weight         1103.32
_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   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                114.387(3)
_cell_angle_beta                 94.858(2)
_cell_angle_gamma                111.117(2)
_cell_formula_units_Z            1
_cell_length_a                   9.6581(2)
_cell_length_b                   10.7180(3)
_cell_length_c                   10.7586(3)
_cell_measurement_reflns_used    17467
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.9920
_cell_measurement_theta_min      2.1500
_cell_volume                     909.78(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_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      N~2~
_diffrn_ambient_temperature      150.00(10)
_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 0.836
_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    -18.00  76.00   0.50    1.00    --    3.98  77.00-180.00  188
  2  \w    -69.00  16.00   0.50    1.00    --    3.98 -10.00 -26.00  170
  3  \w     -8.00  77.00   0.50    1.00    --    3.98  10.00 146.00  170
  4  \w    -68.00  14.00   0.50    1.00    --    3.98 -38.00  60.00  164
  5  \w    -77.00  17.00   0.50    1.00    --   -4.92 -77.00   0.00  188
  6  \w    -18.00  35.00   0.50    1.00    --    3.98 -99.00  30.00  106
  7  \w    -18.00  35.00   0.50    1.00    --    3.98 -99.00 120.00  106
  8  \w    -18.00  35.00   0.50    1.00    --    3.98 -99.00 -60.00  106
  9  \w    -18.00  35.00   0.50    1.00    --    3.98 -99.00-180.00  106
 10  \w    -79.00   0.00   0.50    1.00    --   -4.92 -19.00-150.00  158
;
_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      0.0034973000
_diffrn_orient_matrix_UB_12      0.0691732000
_diffrn_orient_matrix_UB_13      0.0048746000
_diffrn_orient_matrix_UB_21      0.0808351000
_diffrn_orient_matrix_UB_22      0.0278111000
_diffrn_orient_matrix_UB_23      0.0091593000
_diffrn_orient_matrix_UB_31      -0.0125560000
_diffrn_orient_matrix_UB_32      -0.0309388000
_diffrn_orient_matrix_UB_33      -0.0745661000
_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  0.0314
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24914
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.050
_diffrn_reflns_theta_min         2.162
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.026
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0317P)^2^+0.7281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4361
_reflns_number_total             4859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01346h2.cif
_cod_data_source_block           10-22-f2_auto
_cod_depositor_comments
'Adding full bibliography for 7716686--7716689.cif.'
_cod_database_code               7716688
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Cu V'
_reflns_odcompleteness_completeness 100.00
_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
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C6(H6), C11(H11), C15(H15), C13(H13), C2(H2)
;
_shelx_res_checksum              39659
_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 1.663
_oxdiff_exptl_absorpt_empirical_full_min 0.707