Ultrafast post-synthetic modification of a pillared cobalt(ii)-based metal‒organic framework via sulfurization of its pores for high-performance supercapacitors
Abazari, Reza; Sanati, Soheila; Morsali, Ali; Slawin, Alexandra M. Z.; Carpenter-Warren, Cameron L.; Chen, Wei; Zheng, Anmin; Journal of Materials Chemistry A 7 (2019) 11953–; doi:10.1039/C9TA01628G

data_7237652
_publ_section_title
;
 Ultrafast post-synthetic modification of a pillared cobalt(ii)-based
 metal--organic framework via sulfurization of its pores for
 high-performance supercapacitors
;
_journal_issue                   19
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              11953
_journal_paper_doi               10.1039/C9TA01628G
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C64 H44 Co2 N8 O14, 3(C3 H7 N O)'
_chemical_formula_sum            'C73 H65 Co2 N11 O17'
_chemical_formula_weight         1486.22
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-20 deposited with the CCDC.	2019-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                112.424(9)
_cell_angle_beta                 99.484(8)
_cell_angle_gamma                106.304(9)
_cell_formula_units_Z            1
_cell_length_a                   9.8591(11)
_cell_length_b                   14.9188(15)
_cell_length_c                   15.0675(13)
_cell_measurement_reflns_used    4014
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.2470
_cell_measurement_theta_min      2.1930
_cell_volume                     1871.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9089
_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   -120.00  60.00   1.00  120.00    --  -29.54  54.00   0.00  180
  2  \w   -120.00  60.00   1.00  120.00    --  -29.54  54.00 120.00  180
  3  \w   -120.00  60.00   1.00  120.00    --  -29.54  54.00 240.00  180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0627707000
_diffrn_orient_matrix_UB_12      -0.0134878000
_diffrn_orient_matrix_UB_13      -0.0050761000
_diffrn_orient_matrix_UB_21      0.0326680000
_diffrn_orient_matrix_UB_22      0.0271702000
_diffrn_orient_matrix_UB_23      0.0531321000
_diffrn_orient_matrix_UB_31      -0.0345476000
_diffrn_orient_matrix_UB_32      -0.0465087000
_diffrn_orient_matrix_UB_33      0.0036535000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.1427
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23590
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.858
_diffrn_reflns_theta_min         1.639
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       prism
_exptl_crystal_F_000             770
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         11685
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1750
_refine_ls_R_factor_gt           0.0906
_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^)+(0.0755P)^2^+3.6351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2020
_refine_ls_wR_factor_ref         0.2382
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6402
_reflns_number_total             11685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ta01628g2.cif
_cod_data_source_block           reza84
_cod_database_code               7237652
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.904
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H2-N2
 0.98 with sigma of 0.05
 N3-H3
 0.98 with sigma of 0.05
3. Rigid body (RIGU) restrains
 O9, N6, C36, C37, H37A, H37B, H37C, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O9(0.5) N6(0.5) C36(0.5) H36(0.5) C37(0.5) H37A(0.5) H37B(0.5)
 H37C(0.5) C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12), C15(H15),
  C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C24(H24), C25(H25),
 C27(H27), C28(H28), C30(H30), C31(H31), C36(H36), C33(H33)
5.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C)
;
_shelx_res_checksum              61419
_olex2_exptl_crystal_mounting_method loop
_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 1.179
_oxdiff_exptl_absorpt_empirical_full_min 0.815