Improved conductivity of a new Co(ii)-MOF by assembled acetylene black for efficient hydrogen evolution reaction
Zhou, Wei; Wu, Ya-Pan; Wang, Xiao; Tian, Jun-Wu; Huang, Dan-Dan; Zhao, Jun; Lan, Ya-Qian; Li, Dong-Sheng; CrystEngComm 20 (2018) 4804–; doi:10.1039/C8CE00921J

data_7231181
_publ_section_title
;
 Improved conductivity of a new Co(ii)-MOF by assembled acetylene black
 for efficient hydrogen evolution reaction
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4804
_journal_paper_doi               10.1039/C8CE00921J
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C19 H12 Co1.5 N3 O7'
_chemical_formula_sum            'C19 H12 Co1.5 N3 O7'
_chemical_formula_weight         482.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-11-01 deposited with the CCDC.
2018-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.098(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3083(2)
_cell_length_b                   10.4819(2)
_cell_length_c                   22.1487(4)
_cell_measurement_reflns_used    5431
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.8950
_cell_measurement_theta_min      4.9750
_cell_volume                     2148.79(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9f (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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -37.00  30.00   0.50    0.69    --    0.00 -77.00  60.00  134
  2  \w    -33.00  31.00   0.50    0.69    --    0.00 -82.00 -30.00  128
  3  \w    -16.00  10.00   0.50    0.69    --    0.00 -82.00-180.00   52
  4  \w     35.00 118.00   0.50    2.78    --   94.90 -45.00-120.00  166
  5  \w    112.00 158.00   0.50    2.78    --   94.90  15.00  90.00   92
  6  \w    120.00 182.00   0.50    2.78    --   94.90  82.00 150.00  124
  7  \w     96.00 151.00   0.50    2.78    --   94.90  77.00   0.00  110
  8  \w     88.00 184.00   0.50    2.78    --   94.90  30.00 150.00  192
  9  \w     83.00 170.00   0.50    2.78    --   94.90  30.00 120.00  174
 10  \w     86.00 111.00   0.50    2.78    --   94.90  15.00  90.00   50
 11  \w      6.00 113.00   0.50    2.78    --   94.90 -61.00-120.00  214
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0637976000
_diffrn_orient_matrix_UB_12      -0.0832773000
_diffrn_orient_matrix_UB_13      -0.0479126000
_diffrn_orient_matrix_UB_21      -0.0523647000
_diffrn_orient_matrix_UB_22      0.0974434000
_diffrn_orient_matrix_UB_23      -0.0495772000
_diffrn_orient_matrix_UB_31      0.1447119000
_diffrn_orient_matrix_UB_32      0.0716978000
_diffrn_orient_matrix_UB_33      0.0117434000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10644
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.593
_diffrn_reflns_theta_max         66.593
_diffrn_reflns_theta_min         4.672
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.580
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       block
_exptl_crystal_F_000             974
_refine_diff_density_max         0.590
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         3795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0612
_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^)+(0.1160P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3313
_reflns_number_total             3795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00921j2.cif
_cod_data_source_block           co
_cod_depositor_comments          'Adding full bibliography for 7231181.cif.'
_cod_original_formula_sum        'C19 H12 Co1.50 N3 O7'
_cod_database_code               7231181
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.76
_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 O(H,H) groups
2.a Rotating group:
 O2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C15(H15), C10(H10), C5(H5), C19(H19), C16(H16), C18(H18), C11(H11),
 C14(H14), C13(H13)
;
_shelx_res_checksum              87678
_shelx_fab_checksum              33792
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 8.503
_oxdiff_exptl_absorpt_empirical_full_min 0.199