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_4123347
_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 unk
_chemical_formula_moiety
'C34 H20 Co2 O10 S4, C2.81 H6.37 N0.94 O0.94, C2.71 H6.71 N0.71 O0.71, C2 H5 O0.71'
_chemical_formula_sum            'C41.52 H38.08 Co2 N1.64 O12.35 S4'
_chemical_formula_weight         1003.69
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-09-14
_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                   19.3867(7)
_cell_length_b                   19.3867(7)
_cell_length_c                   20.8268(15)
_cell_measurement_reflns_used    9399
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.89
_cell_measurement_theta_min      2.30
_cell_volume                     6778.9(6)
_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      100.0
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            130979
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.114
_diffrn_reflns_theta_min         1.213
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             3093
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 4327 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.002(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         9985
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0506P)^2^+6.2779P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9462
_reflns_number_total             9985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja512437u_si_003.cif
_cod_data_source_block           tn12_170
_cod_depositor_comments
;Adding full bibliography for 4123347--4123349.cif.

The following automatic conversions were performed:

data name '_exptl_absorpt_process_detail' was replaced with
'_exptl_absorpt_process_details' as specified in the replacement file
'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        6778.9(7)
_cod_database_code               4123347
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.695
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1W1-H1WA = O1W2-H1WC = O1W1-H1WB = O1W2-H1WD
 0.84 with sigma of 0.02
 C1E1-C2E1
 1.41 with sigma of 0.01
 C1E1-O1E1
 1.47 with sigma of 0.01
 N1D1-C2D1 = N1D1-C3D1 = N1D2-C2D2 = N1D2-C3D2
 1.42 with sigma of 0.02
 N1D1-C1D1 = N1D2-C1D2
 1.35 with sigma of 0.02
 C1D1-O1D1 = C1D2-O1D2
 1.22 with sigma of 0.02
 C2E1-O1E1
 2.33 with sigma of 0.02
 O1E1-C1E1 \\sim O1E1-C0AA
 with sigma of 0.02
 C1E1-C10 \\sim C0AA-C2E1
 with sigma of 0.02
 O1E1-C10 \\sim O1E1-C2E1
 with sigma of 0.02
3. Rigid bond restraints
 O1D1, C1D1, N1D1, C2D1, C3D1, O1D2, C1D2, N1D2, C2D2, C3D2, O1E1, C1E1, C10,
 C0AA, C2E1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1D1 \\sim C1D1 \\sim N1D1 \\sim C2D1 \\sim C3D1 \\sim O1D2 \\sim C1D2 \\sim
N1D2 \\sim C2D2 \\sim C3D2 \\sim O1E1 \\sim C1E1 \\sim C10 \\sim C0AA \\sim
C2E1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C3D1 \\sim N1D1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N1D2 \\sim C2D2 \\sim C3D2: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C1E1) = Uanis(C0AA)
Uanis(C2E1) = Uanis(C10)
Uanis(C3D1) = Uanis(N1D1)
Uanis(N1D2) = Uanis(C2D2) = Uanis(C3D2)
5. Same fragment restrains
{O1D1, C1D1, N1D1, C2D1, C3D1}
as
{O1D2, C1D2, N1D2, C2D2, C3D2}
6. Others
 Sof(O1D1)=Sof(C1D1)=Sof(H1D1)=Sof(N1D1)=Sof(C2D1)=Sof(H2DA)=Sof(H2DB)=
 Sof(H2DC)=Sof(C3D1)=Sof(H3DA)=Sof(H3DC)=FVAR(1)
 Sof(O1D2)=Sof(C1D2)=Sof(H1D2)=Sof(N1D2)=FVAR(2)
 Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(C2E1)=Sof(H2EA)=Sof(H2EB)=Sof(H2EC)=1-FVAR(3)
 Sof(O1E1)=Sof(C1E1)=Sof(H1EA)=Sof(H1EB)=Sof(C10)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=FVAR(3)
 Fixed Sof: H3DB(0.75)
7.a Secondary CH2 refined with riding coordinates:
 C1E1(H1EA,H1EB), C0AA(H0AA,H0AB)
7.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)
7.c Idealised Me refined as rotating group:
 C2D1(H2DA,H2DB,H2DC), C3D1(H3DA,H3DB,H3DC), C2D2(H2DD,H2DE,H2DF), C3D2(H3DD,
 H3DE,H3DF), C10(H10A,H10B,H10C), C2E1(H2EA,H2EB,H2EC)
;
_olex2_submission_special_instructions 'No special instructions were received'