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_4133185
_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
'C16 H30 O19 S2 V6, 1.5(C H2 Cl2), 2(C16 H36 N)'
_chemical_formula_sum            'C49.5 H105 Cl3 N2 O19 S2 V6'
_chemical_formula_weight         1508.50
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 116.691(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.438(4)
_cell_length_b                   16.021(2)
_cell_length_c                   17.035(2)
_cell_measurement_reflns_used    7211
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.30
_cell_measurement_theta_min      2.24
_cell_volume                     6934.2(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46834
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.039
_diffrn_reflns_theta_min         1.503
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0873 before and 0.0574 after correction. The Ratio of minimum to maximum transmission is 0.8593. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       block
_exptl_crystal_F_000             3148
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8392
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0778P)^2^+12.8271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6676
_reflns_number_total             8392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08780_si_001.cif
_cod_data_source_block           3
_cod_original_cell_volume        6933.9(17)
_cod_database_code               4133185
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.744
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All C(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl-C4 \\sim C9-Cl3
 with sigma of 0.02
 C19B-C6 \\sim C5AA-C4AA
 with sigma of 0.02
 Cl2-C9 \\sim C9-Cl3
 with sigma of 0.02
 Cl1-C4 \\sim C4-Cl
 with sigma of 0.02
 C4AA-C3AA \\sim C7-C5 \\sim C6-C8
 with sigma of 0.02
 C5AA-C4AA \\sim C19B-C7
 with sigma of 0.02
 C3AA-C4AA \\sim C5-C7 \\sim C8-C6
 with sigma of 0.02
 C4AA-C5AA \\sim C7-C25 \\sim C6-C19B
 with sigma of 0.02
3. Others
 Sof(H00G)=Sof(H00H)=Sof(C00Z)=Sof(H00W)=Sof(H00X)=Sof(C010)=Sof(H01A)=
 Sof(H01B)=Sof(C011)=Sof(H01C)=Sof(H01D)=Sof(H01E)=1-FVAR(1)
 Sof(H00E)=Sof(H00F)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(C2AA)=Sof(H2AA)=
 Sof(H2AB)=Sof(H2AC)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=FVAR(1)
 Fixed Sof: S04(0.33333) Cl(0.5) Cl1(0.5) HC(0.33333) HD(0.33333) HE(0.33333)
 HF(0.33333) HG(0.33333) H3AA(0.33333) C4(0.5) H4A(0.5) H4B(0.5) C5(0.33333)
 H5B(0.33333) H5A(0.33333) S1(0.33333) C6(0.33333) H6A(0.33333) H6B(0.33333)
 C7(0.33333) H7A(0.33333) H7B(0.33333) C8(0.33333) H8A(0.33333) H8B(0.33333)
 C19B(0.33333) H19A(0.33333) H19B(0.33333) H19C(0.33333) C4AA(0.33333)
 H4AA(0.33333) H4AB(0.33333) C3AA(0.33333) H3AB(0.33333) H3AC(0.33333)
 S9(0.33333) C9(0.25) H9A(0.25) H9B(0.25) Cl3(0.25) Cl2(0.25) C5AA(0.33333)
 H5AA(0.33333) H5AB(0.33333) H5AC(0.33333) C25(0.33333)
4.a Secondary CH2 refined with riding coordinates:
 C00I(H00Y,H), C00K(H00Z,HA), C00L(H00,HB), C00M(HC,HD), C00M(HE,HF), C00M(HG,
 H3AA), C00N(H00A,H00B), C00O(H00C,H00D), C00P(H00G,H00H), C00P(H00E,H00F),
 C00Q(H00I,H00J), C00R(H00K,H00L), C00S(H00M,H00N), C00T(H00O,H00P), C0(H0A,
 H0B), C2(H2A,H2B), C00Z(H00W,H00X), C010(H01A,H01B), C4(H4A,H4B), C5(H5B,H5A),
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C0AA(H0AA,H0AB), C1AA(H1AA,H1AB),
 C4AA(H4AA,H4AB), C3AA(H3AB,H3AC), C9(H9A,H9B), C27(H27A,H27B)
4.b Idealised Me refined as rotating group:
 C00U(H00Q,H00R,H00S), C00W(H00T,H00U,H00V), C011(H01C,H01D,H01E), C19B(H19A,
 H19B,H19C), C2AA(H2AA,H2AB,H2AC), C5AA(H5AA,H5AB,H5AC), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              61098
_shelx_hkl_checksum              17895
_olex2_submission_special_instructions 'No special instructions were received'