Counterion Influence on Dynamic Spin Properties in a V(IV) Complex
Lin, Chun-Yi; Ngendahimana, Thacien; Eaton, Gareth; Eaton, Sandra S.; Zadrozny, Joseph; Chemical Science  (2019) –; doi:10.1039/C8SC04122A

data_1550053
_publ_section_title
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 Counterion Influence on Dynamic Spin Properties in a V(IV) Complex
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04122A
_journal_year                    2019
_chemical_formula_moiety         'C18 H12 O6 V, 2(C12 H28 N), 2(C4 H8 O)'
_chemical_formula_sum            'C50 H84 N2 O8 V'
_chemical_formula_weight         892.13
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-17 deposited with the CCDC.
2018-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.648(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8268(11)
_cell_length_b                   21.9164(19)
_cell_length_c                   17.7812(15)
_cell_measurement_reflns_used    9032
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.27
_cell_measurement_theta_min      2.19
_cell_volume                     4927.9(7)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.93
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34618
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.758
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_T_max  0.5910
_exptl_absorpt_correction_T_min  0.4588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1104 before and 0.0814 after correction. The Ratio of minimum to maximum transmission is 0.7763. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             1940
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, hexanes'
_exptl_crystal_size_max          0.403
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.184
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4629
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.230
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0657
_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^)+26.8263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1510
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4033
_reflns_number_total             4629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04122a2.cif
_cod_data_source_block           jz10_0m
_cod_database_code               1550053
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.905
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-C25 \\sim O4-C25A
 with sigma of 0.02
 C23-C24 \\sim C23-C24A
 with sigma of 0.02
 C25-C24 \\sim C25A-C24A
 with sigma of 0.02
 O4-C24 \\sim O4-C24A
 with sigma of 0.04
 C23-C25 \\sim C23-C25A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C24) = Uanis(C24A) = Uanis(C25) = Uanis(C25A)
4. Others
 Sof(H23C)=Sof(H23D)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C24A)=Sof(H24C)=
 Sof(H24D)=1-FVAR(1)
 Sof(H23A)=Sof(H23B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 FVAR(1)
5.a Ternary CH refined with riding coordinates:
 N1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C19(H19A,H19B), C11(H11A,H11B), C18(H18A,H18B), C14(H14A,
 H14B), C12(H12A,H12B), C15(H15A,H15B), C20(H20A,H20B), C16(H16A,H16B),
 C22(H22A,H22B), C23(H23A,H23B), C23(H23C,H23D), C25(H25A,H25B), C24(H24A,H24B),
  C25A(H25C,H25D), C24A(H24C,H24D)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C3(H3), C9(H9), C6(H6), C4(H4), C5(H5)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C)
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_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'