Cation-dependent intrinsic electrical conductivity in isostructural tetrathiafulvalene-based microporous metal-organic frameworks.
Park, Sarah S.; Hontz, Eric R.; Sun, Lei; Hendon, Christopher H.; Walsh, Aron; Van Voorhis, Troy; Dincă, Mircea; Journal of the American Chemical Society 137 (2015) 1774–1777; doi:10.1021/ja512437u

data_4123348
_publ_section_title
;
 Cation-dependent intrinsic electrical conductivity in isostructural
 tetrathiafulvalene-based microporous metal-organic frameworks.
;
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1774
_journal_page_last               1777
_journal_paper_doi               10.1021/ja512437u
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C34 H18 Cd2 O10 S4, 2(C3 H7 N O), C2 H5 O'
_chemical_formula_sum            'C42 H37 Cd2 N2 O13 S4'
_chemical_formula_weight         1130.77
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-09-18
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.600(3)
_cell_length_b                   19.600(3)
_cell_length_c                   20.760(3)
_cell_measurement_reflns_used    9671
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.601
_cell_measurement_theta_min      2.859
_cell_volume                     6906.7(18)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            98597
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.663
_diffrn_reflns_theta_min         1.550
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.169
_exptl_absorpt_correction_T_max  0.9663
_exptl_absorpt_correction_T_min  0.8886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       niddle
_exptl_crystal_F_000             3402
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.012
_exptl_crystal_size_min          0.012
_refine_diff_density_max         1.948
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
;
 Flack x determined using 5448 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.025(8)
_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     589
_refine_ls_number_reflns         12956
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+13.7684P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0969
_reflns_Friedel_coverage         0.948
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                11889
_reflns_number_total             12956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja512437u_si_004.cif
_cod_data_source_block           fixedsarah
_cod_depositor_comments
'Adding full bibliography for 4123347--4123349.cif.'
_cod_original_cell_volume        6906(2)
_cod_database_code               4123348
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.944
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Shared sites
{N2S, N2SB}
3. Restrained distances
 O10-H10A = O10-H10B
 0.84 with sigma of 0.02
 N2S-C4S \\sim N2SB-C4SB
 with sigma of 0.02
 N2S-C6S \\sim N2SB-C6SB
 with sigma of 0.02
 N2S-C5S \\sim N2SB-C5SB
 with sigma of 0.02
 N2S-C5S \\sim N2S-C6S
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C1SA)
Uanis(C2) = Uanis(C2SA)
Uanis(O1) = Uanis(O1SA)
Uanis(O2S) = Uanis(O2SB)
Uanis(C4S) = Uanis(C4SB)
Uanis(C6S) = Uanis(C6SB) = Uanis(C5S) = Uanis(C5SB)
Uanis(N2S) = Uanis(N2SB)
Uanis(C2S) = Uanis(C3S) = Uanis(C5S) = Uanis(C6S)
5. Same fragment restrains
{C1SA, C2SA, O1SA}
as
{C1, C2, O1}
6. Others
 Sof(O2SB)=Sof(N2SB)=Sof(C4SB)=Sof(H4SB)=Sof(C5SB)=Sof(H5SA)=Sof(H5SB)=
 Sof(H5SC)=Sof(C6SB)=Sof(H6SA)=Sof(H6SB)=Sof(H6SC)=1-FVAR(1)
 Sof(N2S)=Sof(O2S)=Sof(C4S)=Sof(H4S)=Sof(C5S)=Sof(H5SD)=Sof(H5SE)=Sof(H5SF)=
 Sof(C6S)=Sof(H6SD)=Sof(H6SE)=Sof(H6SF)=FVAR(1)
 Sof(C1SA)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C2SA)=Sof(H2SD)=Sof(O1SA)=
 Sof(H1SD)=1-FVAR(2)
 Sof(C1)=Sof(H1C)=Sof(H1D)=Sof(H1E)=Sof(C2)=Sof(H2)=Sof(O1)=Sof(H1)=FVAR(2)
7.a Aromatic/amide H refined with riding coordinates:
 C1S(H1S), C10(H10), C11(H11), C13(H13), C14(H14), C17(H17), C18(H18),
 C1A(H1A), C1B(H1B), C22(H22), C23(H23), C25(H25), C26(H26), C29(H29), C30(H30),
  C32(H32), C33(H33), C4S(H4S), C4SB(H4SB), C2(H2), C2SA(H2SD)
7.b Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC), C5S(H5SD,H5SE,H5SF), C6S(H6SD,H6SE,
 H6SF), C5SB(H5SA,H5SB,H5SC), C6SB(H6SA,H6SB,H6SC), C1(H1C,H1D,H1E), C1SA(H1SA,
 H1SB,H1SC)
7.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O1SA(H1SD)
;
_olex2_submission_special_instructions 'No special instructions were received'