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_4123349
_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_absolute_configuration ad
_chemical_formula_moiety
'C34 H20 Mn2 O10 S4, 1.78(C3 H7 N1 O1), 0.84(C2 H6 O)'
_chemical_formula_sum            'C40.94 H37.3 Mn2 N1.76 O12.59 S4'
_chemical_formula_weight         993.54
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   19.4690(7)
_cell_length_b                   19.4690(7)
_cell_length_c                   20.6804(8)
_cell_measurement_reflns_used    9445
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.37
_cell_measurement_theta_min      2.61
_cell_volume                     6788.5(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      100.01
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            9445
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.364
_diffrn_reflns_theta_min         2.608
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6704
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1217 before and 0.0656 after correction.
The Ratio of minimum to maximum transmission is 0.8985.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             3060
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.005(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         13845
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+3.2160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                12607
_reflns_number_total             13845
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja512437u_si_002.cif
_cod_data_source_block           tn13_170
_cod_depositor_comments
'Adding full bibliography for 4123347--4123349.cif.'
_cod_original_formula_sum        'C40.94 H37.30 Mn2 N1.76 O12.59 S4'
_cod_database_code               4123349
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H1WD of O1W2, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H1WC of O1W2, H1E1 of O1E1
2. Restrained distances
 O1W1-H1WA = O1W1-H1WB = O1W2-H1WD = O1W2-H1WC
 0.84 with sigma of 0.02
3. Others
 Sof(O1D1)=Sof(C1D1)=Sof(H1D1)=Sof(N1D1)=Sof(C2D1)=Sof(H2DA)=Sof(H2DB)=
 Sof(H2DC)=Sof(C3D1)=Sof(H3DA)=Sof(H3DB)=Sof(H3DC)=FVAR(1)
 Sof(O1D2)=Sof(C1D2)=Sof(H1D2)=Sof(N1D2)=Sof(C2D2)=Sof(H2DD)=Sof(H2DE)=
 Sof(H2DF)=Sof(C3D2)=Sof(H3DD)=Sof(H3DE)=Sof(H3DF)=FVAR(2)
 Sof(O1E1)=Sof(H1E1)=Sof(C1E1)=Sof(H1EA)=Sof(H1EB)=Sof(C2E1)=Sof(H2EA)=
 Sof(H2EB)=Sof(H2EC)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C1E1(H1EA,H1EB)
4.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25),
 C26(H26), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43), C45(H45),
  C46(H46), C1D1(H1D1), C1D2(H1D2)
4.c Idealised Me refined as rotating group:
 C2D1(H2DA,H2DB,H2DC), C3D1(H3DA,H3DB,H3DC), C2D2(H2DD,H2DE,H2DF), C3D2(H3DD,
 H3DE,H3DF), C2E1(H2EA,H2EB,H2EC)
4.d Idealised tetrahedral OH refined as rotating group:
 O1E1(H1E1)
;
_olex2_submission_special_instructions 'No special instructions were received'