Triethanolamine stabilized non-alkyl Sn4Cd4 and alkyl Sn2Cd12 oxo clusters with distinct electrocatalytic activities
Wang, Di; Chen, Guang-Hui; Wang, San-Tai; Zhang, Jian; Zhang, Lei; Chemical Communications  (2022) –; doi:10.1039/D2CC00574C

data_7129874
_publ_section_title
;
 Triethanolamine stabilized non-alkyl Sn4Cd4 and alkyl Sn2Cd12 oxo
 clusters with distinct electrocatalytic activities
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00574C
_journal_year                    2022
_chemical_formula_moiety         'C36 H76 Cd4 F4 N6 O20 Sn4, 2(H2 O)'
_chemical_formula_sum            'C36 H80 Cd4 F4 N6 O22 Sn4'
_chemical_formula_weight         1949.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-02-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2022-03-03 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.059(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8087(9)
_cell_length_b                   17.2847(12)
_cell_length_c                   14.4581(9)
_cell_measurement_reflns_used    9098
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      60.0190
_cell_measurement_theta_min      2.7230
_cell_volume                     2849.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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     49.00 145.00   0.50    2.00    --   72.41  77.00-120.00  192
  2  \w    118.00 144.00   0.50    2.00    --   72.41  38.00 -90.00   52
  3  \w     59.00  98.00   0.50    2.00    --   72.41  38.00 -90.00   78
  4  \w     95.00 121.00   0.50    2.00    --   72.41 107.00 -85.00   52
  5  \w     83.00 116.00   0.50    2.00    --   72.41 125.00 -60.00   66
  6  \w    -74.00 -39.00   0.50    1.00    --   -1.25 -38.00  90.00   70
  7  \w    -32.00  11.00   0.50    1.00    --   -1.25 -38.00  90.00   86
  8  \w      5.00  99.00   0.50    2.00    --   72.41-107.00 176.00  188
  9  \w    -88.00 -39.00   0.50    2.00    --  -74.91 107.00 -85.00   98
 10  \w    -40.00  -2.00   0.50    2.00    --  -74.91  38.00 -60.00   76
 11  \w     -3.00  56.00   0.50    1.00    --   -1.25  57.00-120.00  118
 12  \w    -87.00 -61.00   0.50    2.00    --  -74.91 -57.00-180.00   52
 13  \w   -131.00 -88.00   0.50    2.00    --  -74.91 -99.00-120.00   86
 14  \w   -140.00 -79.00   0.50    2.00    --  -74.91-125.00  60.00  122
 15  \w   -116.00 -91.00   0.50    2.00    --  -74.91 -99.00  90.00   50
 16  \w   -135.00 -88.00   0.50    2.00    --  -74.91-107.00 176.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19019
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         56.908
_diffrn_reflns_theta_min         3.538
_exptl_absorpt_coefficient_mu    17.554
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    2.272
_exptl_crystal_description       block
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.869
_refine_diff_density_min         -1.644
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5804
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0641
_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^)+(0.1231P)^2^+12.0141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1742
_refine_ls_wR_factor_ref         0.1887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4495
_reflns_number_total             5804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00574c2.cif
_cod_data_source_block           d11-43-9_auto
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7129874
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O11A-C18
 1.4 with sigma of 0.02
 H4-H5C
 2.1 with sigma of 0.002
 H5C-H12A_$1
 2.1 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(H18C)=Sof(H18D)=Sof(O11A)=Sof(H11C)=1-FVAR(1)
 Sof(H18A)=Sof(H18B)=Sof(O11)=Sof(H11)=FVAR(1)
5.a Free rotating group:
 O5(H5C,H5D)
5.b Ternary CH refined with riding coordinates:
 O4(H4)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C12(H12A,H12B), C17(H17A,H17B), C7(H7A,H7B), C9(H9A,H9B),
 C15(H15A,H15B), C16(H16A,H16B), C8(H8A,H8B), C5(H5A,H5B), C10(H10A,H10B),
 C11(H11A,H11B), C6(H6A,H6B), C14(H14A,H14B), C13(H13A,H13B), C4(H4A,H4B),
 C2(H2A,H2B), C18(H18A,H18B), C18(H18C,H18D), C3(H3A,H3B)
5.d Tetrahedral OH refined with riding coordinates:
 O11(H11), O11A(H11C)
;
_shelx_res_checksum              12817
_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
;