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_7716689
_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         'C44 H40 Cu2 N4 O10 V2'
_chemical_formula_sum            'C44 H40 Cu2 N4 O10 V2'
_chemical_formula_weight         1013.76
_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             2024-05-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-18 deposited with the CCDC.	2024-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                86.312(2)
_cell_angle_beta                 80.4060(10)
_cell_angle_gamma                72.478(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0873(2)
_cell_length_b                   13.3569(3)
_cell_length_c                   17.7604(3)
_cell_measurement_reflns_used    19126
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      30.9940
_cell_measurement_theta_min      2.3620
_cell_volume                     2026.72(8)
_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      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  35.00   0.50    0.54    --    4.00 -99.00  90.00  106
  2  \w    -18.00  35.00   0.50    0.54    --    4.00 -99.00  60.00  106
  3  \w    -67.00  18.00   0.50    0.54    --    4.00 -57.00 -90.00  170
  4  \w    -18.00  35.00   0.50    0.54    --    4.00 -99.00-150.00  106
  5  \w    -18.00  19.00   0.50    0.54    --    4.00 -99.00-180.00   74
  6  \w    -67.00  18.00   0.50    0.54    --    4.00 -57.00 -30.00  170
  7  \w     -7.00  76.00   0.50    0.54    --    4.00  38.00 150.00  166
  8  \w     -7.00  76.00   0.50    0.54    --    4.00  38.00  30.00  166
  9  \w    -10.00  76.00   0.50    0.54    --    4.00  57.00-120.00  172
;
_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      0.0155634000
_diffrn_orient_matrix_UB_12      0.0154281000
_diffrn_orient_matrix_UB_13      -0.0387561000
_diffrn_orient_matrix_UB_21      0.0269910000
_diffrn_orient_matrix_UB_22      -0.0534745000
_diffrn_orient_matrix_UB_23      -0.0107345000
_diffrn_orient_matrix_UB_31      -0.0767686000
_diffrn_orient_matrix_UB_32      0.0020628000
_diffrn_orient_matrix_UB_33      -0.0048641000
_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  0.1223
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38210
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.991
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64791
_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            'clear greenish'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_refine_diff_density_max         1.956
_refine_diff_density_min         -1.440
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         7386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0677
_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^)+(0.0637P)^2^+16.0600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6346
_reflns_number_total             7386
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9955\% 
around [0.00 1.00 0.00] (reciprocal) or [-0.40 0.92 -0.01] (direct)
;
_cod_data_source_file            d4dt01346h2.cif
_cod_data_source_block           cuv_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7716686--7716689.cif.'
_cod_database_code               7716689
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C44 H40 O7 N4 Cu2 V2'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9960(5)
 0.0040(5)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C00J(H00A,H00B), C00L(H00C,H00D), C01E(H01I,H01J), C01F(H01K,H01L)
3.b Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00P(H00P), C00Q(H00Q), C013(H013), C014(H014), C015(H015),
 C016(H016), C018(H018), C019(H019), C01B(H01D), C01C(H01E), C01H(H01P),
 C01I(H01Q), C01J(H01R), C01K(H01S), C01L(H01T), C01M(H01U), C01N(H01V),
 C01O(H01W), C01Q(H01Z)
3.c Idealised Me refined as rotating group:
 C01A(H01A,H01B,H01C), C01D(H01F,H01G,H01H), C01G(H01M,H01N,H01O), C01P(H01X,
 H01Y,H)
;
_shelx_res_checksum              41414
_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 2.075
_oxdiff_exptl_absorpt_empirical_full_min 0.651
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2