The sequential structural transformation of a heptanuclear zinc cluster towards hierarchical porous carbon for supercapacitor applications
Li, Tian; Wang, Yi-Fan; Yin, Zheng; Li, Jian; Peng, Xu; Zeng, Ming-Hua; Chemical Science  (2022) –; doi:10.1039/D2SC03987G

data_1567558
_publ_section_title
;
 The sequential structural transformation of a heptanuclear zinc cluster
 towards hierarchical porous carbon for supercapacitor applications
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC03987G
_journal_year                    2022
_chemical_formula_moiety         'C60 H78 N6 O18 Zn7, 2(N1 O3)'
_chemical_formula_sum            'C60 H78 N8 O24 Zn7'
_chemical_formula_weight         1752.89
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2022-03-07 deposited with the CCDC.	2022-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.0680(2)
_cell_length_b                   14.0680(2)
_cell_length_c                   23.3614(4)
_cell_measurement_reflns_used    6512
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.4620
_cell_measurement_theta_min      3.6170
_cell_volume                     4004.00(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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      6.00  63.00   0.50    0.05    --   43.05 -57.00-120.00  114
  2  \w     30.00  93.00   0.50    0.05    --   43.05-121.00 -88.00  126
  3  \w     36.00 106.00   0.50    0.18    --  109.88 -94.00 -90.00  140
  4  \w     54.00 117.00   0.50    0.18    --  109.88-153.00 112.00  126
  5  \w     45.00  94.00   0.50    0.18    --  109.88-102.00 169.00   98
  6  \w    107.00 173.00   0.50    0.18    --  109.88  61.00  90.00  132
  7  \w     96.00 176.00   0.50    0.18    --  109.88 125.00 -60.00  160
  8  \w    -79.00 -54.00   0.50    0.18    --  -90.25 121.00  -5.00   50
  9  \w   -100.00 -38.00   0.50    0.05    --  -43.05-178.00 -30.00  124
 10  \w   -120.00 -74.00   0.50    0.18    --  -90.25 -73.00 153.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0807135000
_diffrn_orient_matrix_UB_12      0.0002833000
_diffrn_orient_matrix_UB_13      -0.0444323000
_diffrn_orient_matrix_UB_21      -0.0824072000
_diffrn_orient_matrix_UB_22      -0.0187925000
_diffrn_orient_matrix_UB_23      0.0481579000
_diffrn_orient_matrix_UB_31      0.0517522000
_diffrn_orient_matrix_UB_32      0.1251073000
_diffrn_orient_matrix_UB_33      0.0073240000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13565
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.031
_diffrn_reflns_theta_min         3.628
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_refine_diff_density_max         1.171
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2758
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0551
_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^)+(0.1128P)^2^+3.1992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2482
_reflns_number_total             2758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03987g2.cif
_cod_data_source_block           zn7
_cod_original_cell_volume        4004.00(13)
_cod_database_code               1567558
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H O N Zn'
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C10, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 3.039
_oxdiff_exptl_absorpt_empirical_full_min 0.667