Impact of Ligand Chlorination and Counterion Tuning on High-Field Spin Relaxation in a Series of V(IV) Complexes
Martinez, Roxanna; Jackson, Cassidy E.; Üngör, Ökten; van Tol, Johan; Zadrozny, Joseph; Dalton Transactions  (2023) –; doi:10.1039/D3DT01274C

data_7713483
_publ_section_title
;
 Impact of Ligand Chlorination and Counterion Tuning on High-Field Spin
 Relaxation in a Series of V(IV) Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01274C
_journal_year                    2023
_chemical_formula_moiety         'C18 H6 Cl6 O6 V, 2(C12 H28 N) 1.7[C4H8O]'
_chemical_formula_sum            'C42 H62 Cl6 N2 O6 V'
_chemical_formula_weight         954.57
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Air-sensitive,Moisture-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-07-07 deposited with the CCDC.	2023-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   15.2509(4)
_cell_length_b                   15.2509(4)
_cell_length_c                   18.9173(6)
_cell_measurement_reflns_used    9044
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      29.00
_cell_measurement_theta_min      2.65
_cell_volume                     3810.49(19)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      104.52
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            227182
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         1.542
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6377
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1562 before and 0.0977 after correction.
The Ratio of minimum to maximum transmission is 0.8543.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       block
_exptl_crystal_F_000             1503
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: HMDSO, THF'
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 2302 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         5840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0482P)^2^+1.6329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5400
_reflns_number_total             5840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01274c2.cif
_cod_data_source_block           Complex5_104K
_cod_original_cell_volume        3810.5(2)
_cod_database_code               7713483
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.925
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N008(H008)
2.b Secondary CH2 refined with riding coordinates:
 C00I(H00A,H00B), C00J(H00C,H00D), C00K(H00E,H00F), C00L(H00G,H00H), C00M(H00I,
 H00J), C00N(H00K,H00L), C00O(H00M,H00N), C00P(H00O,H00P), C00R(H00T,H00U)
2.c Aromatic/amide H refined with riding coordinates:
 C00B(H00Z), C00C(H00), C00F(H0AA)
2.d Idealised Me refined as rotating group:
 C00Q(H00Q,H00R,H00S), C00S(H00V,H00W,H00X), C00T(H00Y,H,HA)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 71.3 electrons were 
found in a volume of 153.0\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.7[C4H8O] per Formula Unit 
which account for 68 electrons 
per unit cell.
;
_shelx_res_checksum              83640
_shelx_fab_checksum              6605
_olex2_submission_special_instructions 'No special instructions were received'