Addressing Multiple Resistive States of Polyoxovanadates: Conductivity as a Function of Individual Molecular Redox States.
Linnenberg, Oliver; Moors, Marco; Notario-Estévez, Almudena; López, Xavier; de Graaf, Coen; Peter, Sophia; Baeumer, Christoph; Waser, Rainer; Monakhov, Kirill Yu; Journal of the American Chemical Society 140 (2018) 16635–16640; doi:10.1021/jacs.8b08780

data_4133189
_publ_section_title
;
 Addressing Multiple Resistive States of Polyoxovanadates: Conductivity as
 a Function of Individual Molecular Redox States.
;
_journal_issue                   48
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16635
_journal_page_last               16640
_journal_paper_doi               10.1021/jacs.8b08780
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety
'(V6 O19 S2 C14 H26), 2(C16 H36 N), 2 (C H2 Cl2)'
_chemical_formula_sum            'C48 H102 Cl4 N2 O19 S2 V6'
_chemical_formula_weight         1522.91
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   25.7726(11)
_cell_length_b                   25.7726(11)
_cell_length_c                   26.9789(12)
_cell_measurement_reflns_used    8960
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.88
_cell_measurement_theta_min      2.26
_cell_volume                     15519.3(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SMART V5.631 (?, 2016)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            63695
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.434
_diffrn_reflns_theta_min         1.764
_diffrn_source_current           600.0
_diffrn_source_power             30.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1254 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.8613.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             6285
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         7090
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0875P)^2^+55.0368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1644
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5529
_reflns_number_total             7090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08780_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        15519.3(15)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C48 H102 N2 O19 S2 V6 Cl4'
_cod_database_code               4133189
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.820
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2A,H2BA,H2BB} of C2, All C(H,H) groups, All C(H,H,H,H)
  groups
 At 1.5 times of:
  {H1AA,H1AB,H1AC} of C1A, {H12A,H12B,H12C} of C12, {H13A,H13B,H13C} of C13,
  {H1DA,H1DB,H1DC} of C1D, {H8A,H8B,H8C} of C8, {H17A,H17B,H17C} of C17, {H1A,
  H1B,H1C} of C1, {H10A,H10B,H10C} of C10, {H0AA,H0AB,H0AC} of C0AA, {H10D,H10E,
  H10F} of C10A
2. Rigid bond restraints
 C14, C10A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Sof(H2BA)=Sof(H2BB)=Sof(C9)=Sof(H9A)=Sof(H9B)=1-FVAR(1)
 Sof(H2A)=Sof(C7)=Sof(H7)=FVAR(1)
 Sof(H3BE)=Sof(H3BF)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=1-FVAR(2)
 Sof(H3AC)=Sof(H3AD)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C5A)=Sof(H5AA)=
 Sof(H5AB)=Sof(C16)=Sof(H16A)=Sof(H16B)=FVAR(2)
 Sof(H2AC)=Sof(H2AD)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C1)=Sof(H1A)=Sof(H1B)=
 Sof(H1C)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=1-FVAR(3)
 Sof(H2AA)=Sof(H2AB)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=FVAR(3)
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(C4)=Sof(H4)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=1-FVAR(4)
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(C1D)=Sof(H1DA)=
 Sof(H1DB)=Sof(H1DC)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=FVAR(4)
 Sof(H14)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=1-FVAR(5)
 Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C10)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=FVAR(5)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C19(H19A,H19B), C1AA(H1AD,H1AE), C2AA(H2AC,H2AD), C2AA(H2AA,
 H2AB), C3AA(H3AA,H3AB), C1B(H1BA,H1BB), C2(H2BA,H2BB), C3(H3AC,H3AD), C3(H3BE,
 H3BF), C4B(H4BA,H4BB), C5B(H5BA,H5BB), C6B(H6BA,H6BB), C9(H9A,H9B), C6(H6A,
 H6B), C5(H5A,H5B), C5A(H5AA,H5AB), C16(H16A,H16B), C4A(H4AA,H4AB), C18(H18A,
 H18B), C6A(H6AA,H6AB), C1C(H1CA,H1CB), C1E(H1EA,H1EB)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C7(H7)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C1(H1A,H1B,H1C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C17(H17A,H17B,H17C), C1A(H1AA,H1AB,H1AC), C1D(H1DA,H1DB,H1DC), C10A(H10D,H10E,
 H10F), C10(H10A,H10B,H10C), C0AA(H0AA,H0AB,H0AC)
;
_shelx_res_checksum              36286
_shelx_hkl_checksum              905
_shelx_fab_checksum              23153
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'