Metal‒organic framework-derived Co9S8 embedded in N, O and S-tridoped carbon nanomaterials as an efficient oxygen bifunctional electrocatalyst
Zhao, Jin-Yan; Wang, Rui; Wang, Shan; Lv, Ya-Ru; Xu, Hong; Zang, Shuang-Quan; Journal of Materials Chemistry A 7 (2019) 7389–; doi:10.1039/C8TA12116H

data_7237256
_publ_section_title
;
 Metal--organic framework-derived Co9S8 embedded in N, O and S-tridoped
 carbon nanomaterials as an efficient oxygen bifunctional electrocatalyst
;
_journal_issue                   13
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              7389
_journal_paper_doi               10.1039/C8TA12116H
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C33 H29 Co N3 O8 S'
_chemical_formula_sum            'C33 H29 Co N3 O8 S'
_chemical_formula_weight         686.58
_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             2018-09-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-13 deposited with the CCDC.	2019-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                64.375(3)
_cell_angle_beta                 83.258(5)
_cell_angle_gamma                74.434(5)
_cell_formula_units_Z            2
_cell_length_a                   9.1585(7)
_cell_length_b                   15.3205(6)
_cell_length_c                   15.4803(4)
_cell_measurement_reflns_used    7125
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.7270
_cell_measurement_theta_min      3.3140
_cell_volume                     1886.61(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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 0.989
_diffrn_measured_fraction_theta_max 0.959
_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     50.00  89.00   0.50    0.54    --    0.00  57.00-180.00   78
  2  \w    -85.00 -44.00   0.50    0.54    --    0.00 -38.00 -60.00   82
  3  \w    -28.00  15.00   0.50    0.54    --    0.00  57.00-180.00   86
  4  \w    -30.00  29.00   0.50    0.54    --    0.00 -38.00 -60.00  118
  5  \w     -4.00  86.00   0.50    0.54    --    0.00  57.00 -90.00  180
  6  \w    103.00 187.00   0.50    1.80    --   97.60  45.00 -90.00  168
  7  \w     55.00 182.00   0.50    1.80    --   97.60  15.00-120.00  254
  8  \w     11.00 126.00   0.50    1.80    --   97.60 -30.00 120.00  230
  9  \w     75.00 101.00   0.50    1.80    --   97.60 -82.00 -60.00   52
 10  \w     90.00 116.00   0.50    1.80    --   97.60 -82.00-150.00   52
 11  \w    110.00 135.00   0.50    1.80    --   97.60 -82.00  60.00   50
 12  \w      9.00  35.00   0.50    1.80    --   97.60 -82.00 -90.00   52
 13  \w     12.00 106.00   0.50    1.80    --   97.60 -82.00  60.00  188
 14  \w      9.00 127.00   0.50    1.80    --   97.60 -61.00  60.00  236
 15  \w     32.00  58.00   0.50    1.80    --   97.60 -82.00 -60.00   52
 16  \w     38.00 135.00   0.50    1.80    --   97.60 -82.00 -90.00  194
 17  \w     63.00 134.00   0.50    1.80    --   97.60 -82.00-180.00  142
 18  \w     43.00 128.00   0.50    1.80    --   97.60 -30.00-120.00  170
 19  \w     57.00 100.00   0.50    1.80    --   97.60 -82.00   0.00   86
 20  \w     69.00 114.00   0.50    1.80    --   97.60 -41.00  18.00   90
 21  \w      9.00 122.00   0.50    1.80    --   97.60 -45.00 -90.00  226
 22  \w     89.00 115.00   0.50    1.80    --   97.60 -82.00  90.00   52
 23  \w     19.00 130.00   0.50    1.80    --   97.60 -82.00 120.00  222
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1655276000
_diffrn_orient_matrix_UB_12      0.0557461000
_diffrn_orient_matrix_UB_13      0.0055849000
_diffrn_orient_matrix_UB_21      -0.0520833000
_diffrn_orient_matrix_UB_22      -0.0511818000
_diffrn_orient_matrix_UB_23      -0.0532303000
_diffrn_orient_matrix_UB_31      -0.0194527000
_diffrn_orient_matrix_UB_32      -0.0865510000
_diffrn_orient_matrix_UB_33      0.0965283000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18569
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.318
_diffrn_reflns_theta_min         3.166
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.485
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       block
_exptl_crystal_F_000             710
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.245
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0785
_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^)+(0.1706P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2236
_refine_ls_wR_factor_ref         0.2425
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5240
_reflns_number_total             7288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ta12116h2.cif
_cod_data_source_block           20171107b5-1
_cod_database_code               7237256
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C H N O C  Co'
_shelx_estimated_absorpt_t_max   0.467
_shelx_estimated_absorpt_t_min   0.346
_reflns_odcompleteness_completeness 98.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H,H) groups
2.a Rotating group:
 O004(H00A,H00B)
2.b Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00I(H00I), C00L(H00L), C00M(H00M), C00O(H00O), C00Q(H00Q),
 C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z),
 C010(H010), C011(H011), C012(H012), C013(H013), C014(H014), C015(H015),
 C016(H016), C017(H017), C018(H018)
2.c Idealised Me refined as rotating group:
 C019(H01A,H01B,H01C), C01A(H01D,H01E,H01F)
;
_shelx_res_checksum              21815
_shelx_hkl_checksum              46753
_shelx_fab_checksum              7900
_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 2.547
_oxdiff_exptl_absorpt_empirical_full_min 0.415