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_4515257
_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         'C36 H35 N5 O9 Zn2, 3(C3 H7 N O)'
_chemical_formula_sum            'C45 H56 N8 O12 Zn2'
_chemical_formula_weight         1031.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.0270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3952(2)
_cell_length_b                   18.0382(2)
_cell_length_c                   18.1058(2)
_cell_measurement_reflns_used    24104
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.9410
_cell_measurement_theta_min      4.8700
_cell_volume                     4917.64(10)
_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_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     49.00  77.00   1.00    2.00    --    0.00  38.00  90.00   28
  2  \w    -39.00  18.00   1.00    2.00    --    0.00 -38.00  30.00   57
  3  \w    -78.00  18.00   1.00    2.00    --    0.00 -38.00 -60.00   96
  4  \w    -13.00  76.00   1.00    2.00    --    0.00  38.00 -90.00   89
  5  \w    -23.00  24.00   1.00    2.00    --    0.00 -19.00  60.00   47
  6  \w    -88.00 -49.00   1.00    2.00    --    0.00 -38.00  30.00   39
  7  \w     23.00  49.00   1.00    5.00    --   95.80 -82.00  30.00   26
  8  \w    100.00 132.00   1.00    5.00    --   95.80  77.00 -90.00   32
  9  \w      8.00 112.00   1.00    5.00    --   95.80 -82.00 120.00  104
 10  \w     82.00 109.00   1.00    5.00    --   95.80 -82.00  60.00   27
 11  \w      7.00 123.00   1.00    5.00    --   95.80 -15.00 -30.00  116
 12  \w      6.00 119.00   1.00    5.00    --   95.80 -61.00-150.00  113
 13  \w     78.00 105.00   1.00    5.00    --   95.80 -82.00 -90.00   27
 14  \w     76.00 103.00   1.00    5.00    --   95.80 -82.00  30.00   27
 15  \w     12.00  38.00   1.00    5.00    --   95.80 -82.00 -90.00   26
 16  \w     94.00 121.00   1.00    5.00    --   95.80 -82.00-180.00   27
 17  \w     14.00  40.00   1.00    5.00    --   95.80 -82.00-180.00   26
 18  \w      9.00  95.00   1.00    5.00    --   95.80 -61.00 120.00   86
 19  \w     11.00 123.00   1.00    5.00    --   95.80 -15.00-150.00  112
 20  \w      7.00 125.00   1.00    5.00    --   95.80 -82.00 -30.00  118
 21  \w     25.00 114.00   1.00    5.00    --   95.80 -61.00 -30.00   89
 22  \w     34.00 102.00   1.00    5.00    --   95.80 -30.00 -30.00   68
 23  \w    120.00 178.00   1.00    5.00    --   95.80  30.00 -30.00   58
 24  \w     91.00 116.00   1.00    5.00    --   95.80 -61.00   0.00   25
 25  \w     22.00 116.00   1.00    5.00    --   95.80 -82.00-150.00   94
 26  \w     74.00  99.00   1.00    5.00    --   95.80 -82.00 150.00   25
 27  \w     92.00 119.00   1.00    5.00    --   95.80  77.00 -60.00   27
;
_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      -0.0102370000
_diffrn_orient_matrix_UB_12      0.0515976000
_diffrn_orient_matrix_UB_13      0.0653916000
_diffrn_orient_matrix_UB_21      0.0926066000
_diffrn_orient_matrix_UB_22      0.0328147000
_diffrn_orient_matrix_UB_23      0.0010763000
_diffrn_orient_matrix_UB_31      -0.0423194000
_diffrn_orient_matrix_UB_32      0.0596296000
_diffrn_orient_matrix_UB_33      -0.0573472000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54987
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.498
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.765
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34434
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.039
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0970P)^2^+13.2650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.1808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7635
_reflns_number_total             8768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ae8b01428_si_002.cif
_cod_data_source_block           exp_88
_cod_database_code               4515257
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.667
_shelx_estimated_absorpt_t_min   0.585
_reflns_odcompleteness_completeness 99.96
_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 C(H,H,H) groups
2.a Riding coordinates:
 C38(H38), C40(H40)
2.b Me refined with riding coordinates:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), C3(H3A), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C28(H28), C31(H31), C34(H34), C43(H43)
;
_shelx_res_checksum              85224
_shelx_hkl_checksum              11364
_shelx_fab_checksum              34910
_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 3.350
_oxdiff_exptl_absorpt_empirical_full_min 0.511