Reversible High-Voltage N-Redox Chemistry in Metal–Organic Frameworks for High-Rate Anion-Intercalation Batteries
Lou, Xiaobing; Geng, Fushan; Hu, Bei; Li, Chao; Shen, Ming; Hu, Bingwen; ACS Applied Energy Materials 2 (2018) 413–; doi:10.1021/acsaem.8b01428

data_4515256
_publ_section_title
;
 Reversible High-Voltage N-Redox Chemistry in Metal--Organic Frameworks
 for High-Rate Anion-Intercalation Batteries
;
_journal_issue                   1
_journal_name_full               'ACS Applied Energy Materials'
_journal_page_first              413
_journal_paper_doi               10.1021/acsaem.8b01428
_journal_volume                  2
_journal_year                    2018
_chemical_formula_moiety         '2(C10 H8 N O2)'
_chemical_formula_sum            'C20 H16 N2 O4'
_chemical_formula_weight         348.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                92.633(2)
_cell_angle_beta                 106.665(3)
_cell_angle_gamma                97.402(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0016(3)
_cell_length_b                   10.0412(2)
_cell_length_c                   15.4610(6)
_cell_measurement_reflns_used    7702
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.1950
_cell_measurement_theta_min      4.4550
_cell_volume                     1322.56(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -28.00  15.00   1.00    1.00    --    0.00 -38.00-180.00   43
  2  \w     61.00  89.00   1.00    1.00    --    0.00  38.00-120.00   28
  3  \w    -89.00 -37.00   1.00    1.00    --    0.00 -38.00-180.00   52
  4  \w    -17.00  21.00   1.00    1.00    --    0.00 -57.00 120.00   38
  5  \w    -85.00 -42.00   1.00    1.00    --    0.00 -19.00-150.00   43
  6  \w    -20.00  17.00   1.00    1.00    --    0.00 -19.00-150.00   37
  7  \w    -79.00 -27.00   1.00    1.00    --    0.00 -57.00 120.00   52
  8  \w      7.00 128.00   1.00    2.00    --   95.80 -82.00 -30.00  121
  9  \w     76.00 183.00   1.00    2.00    --   95.80  30.00-150.00  107
 10  \w      9.00  70.00   1.00    2.00    --   95.80 -77.00 -90.00   61
 11  \w    134.00 178.00   1.00    2.00    --   95.80  30.00-180.00   44
 12  \w      7.00  99.00   1.00    2.00    --   95.80 -61.00 -30.00   92
 13  \w     29.00  72.00   1.00    2.00    --   95.80 -82.00-150.00   43
 14  \w     75.00 116.00   1.00    2.00    --   95.80 -82.00-150.00   41
 15  \w     19.00 126.00   1.00    2.00    --   95.80 -82.00 120.00  107
 16  \w      6.00 116.00   1.00    2.00    --   95.80 -45.00  90.00  110
 17  \w     15.00  41.00   1.00    2.00    --   95.80 -77.00 150.00   26
 18  \w    131.00 176.00   1.00    2.00    --   95.80  30.00 -90.00   45
 19  \w     67.00  98.00   1.00    2.00    --   95.80 -77.00 150.00   31
 20  \w      6.00  69.00   1.00    2.00    --   95.80 -61.00 -90.00   63
 21  \w     90.00 124.00   1.00    2.00    --   95.80 -82.00   0.00   34
 22  \w     41.00  91.00   1.00    2.00    --   95.80 -30.00   0.00   50
 23  \w     85.00 111.00   1.00    2.00    --   95.80  30.00 -90.00   26
 24  \w     72.00  97.00   1.00    2.00    --   95.80 -77.00 -90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1772540000
_diffrn_orient_matrix_UB_12      0.0188912000
_diffrn_orient_matrix_UB_13      0.0110842000
_diffrn_orient_matrix_UB_21      0.0344015000
_diffrn_orient_matrix_UB_22      -0.0014378000
_diffrn_orient_matrix_UB_23      0.1034457000
_diffrn_orient_matrix_UB_31      -0.0056061000
_diffrn_orient_matrix_UB_32      -0.1541467000
_diffrn_orient_matrix_UB_33      -0.0087845000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12374
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.074
_diffrn_reflns_theta_max         67.074
_diffrn_reflns_theta_min         4.457
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.875
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4646
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0789
_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^)+(0.1372P)^2^+0.4427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2322
_refine_ls_wR_factor_ref         0.2417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3849
_reflns_number_total             4646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ae8b01428_si_003.cif
_cod_data_source_block           exp_271
_cod_database_code               4515256
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.818
_shelx_estimated_absorpt_t_min   0.796
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Rigid bond restraints
 C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C3 \\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1A), C2(H2A), C3(H3), C4(H4), C5(H5), C8(H8), N2(H2B), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C18(H18)
4.b Tetrahedral OH refined with riding coordinates:
 O2(H2), O3(H3A)
;
_shelx_res_checksum              69410
_shelx_hkl_checksum              56587
_shelx_fab_checksum              49889
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.809
_oxdiff_exptl_absorpt_empirical_full_min 0.582