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_7129875
_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         'C57 H114 Cd12 Cl4 N8 O29 Sn2'
_chemical_formula_sum            'C57 H114 Cd12 Cl4 N8 O29 Sn2'
_chemical_formula_weight         3103.54
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.1808(6)
_cell_length_b                   25.1808(6)
_cell_length_c                   27.0021(8)
_cell_measurement_reflns_used    7819
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      74.8680
_cell_measurement_theta_min      3.4650
_cell_volume                     17121.3(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector_area_resol_mean 10.3468
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_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    -52.00  37.00   1.00    7.50    --  -41.16  19.00 150.00   89
  2  \w   -113.00 -84.00   1.00    7.50    --  -41.16 -57.00   0.00   29
  3  \w    -39.00 -13.00   1.00    7.50    --  -41.16 -57.00   0.00   26
  4  \w     55.00 105.00   1.00   42.50    --  108.23-111.00-150.00   50
  5  \w    122.00 156.00   1.00   42.50    --  108.23 111.00 -30.00   34
  6  \w    105.00 173.00   1.00   42.50    --  108.23 111.00-150.00   68
  7  \w    109.00 175.00   1.00   42.50    --  108.23  77.00 -60.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17015
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.265
_diffrn_reflns_theta_min         3.510
_exptl_absorpt_coefficient_mu    29.697
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
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    2.408
_exptl_crystal_description       needle
_exptl_crystal_F_000             11904
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.162
_refine_diff_density_min         -1.857
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4368
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0858
_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^)+(0.1001P)^2^+606.3834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2210
_refine_ls_wR_factor_ref         0.2244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4017
_reflns_number_total             4368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00574c2.cif
_cod_data_source_block           2
_cod_original_cell_volume        17121.3(10)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               7129875
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.155
_shelx_estimated_absorpt_t_min   0.041
_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 C(H,H,H) groups
2. Restrained distances
 C2-C1 = C3-C2 = C4-C3
 1.54 with sigma of 0.002
 C7-C8 = C7A-C8
 1.54 with sigma of 0.002
 C11A-C12 = C11-C12
 1.54 with sigma of 0.002
 C16-C15
 1.54 with sigma of 0.002
 C5-C6
 1.54 with sigma of 0.002
 C9A-C10 = C9-C10
 1.54 with sigma of 0.002
 C13-C14
 1.54 with sigma of 0.002
 C1-C3
 2.52 with sigma of 0.04
 C2-C4
 2.52 with sigma of 0.04
3. Restrained planarity
 C1, C2, C3, C4
 with sigma of 0.1
4. Rigid bond restraints
 N4, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C5, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C9A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O9)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C11A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
6. Rigid body (RIGU) restrains
 C4, C3, C2, C1, Sn1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
7. Others
 Fixed Sof: Cd2(0.65) Cd1(0.65) O8(0.25) H10A(0.5) H10B(0.5) H10C(0.5)
 H10D(0.5) C9(0.5) H9A(0.5) H9B(0.5) H12A(0.5) H12B(0.5) H12C(0.5) H12D(0.5)
 C11(0.5) H11A(0.5) H11B(0.5) H8AA(0.5) H8AB(0.5) H8BC(0.5) H8BD(0.5) C7(0.5)
 H7A(0.5) H7B(0.5) O9(0.5) Cd1A(0.35) Cd2A(0.35) C9A(0.5) H9AA(0.5) H9AB(0.5)
 C7A(0.5) H7AA(0.5) H7AB(0.5) C11A(0.5) H11C(0.5) H11D(0.5) C1(0.5) H1A(0.5)
 H1B(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C3(0.5) H3A(0.5) H3B(0.5) C2(0.5)
 H2A(0.5) H2B(0.5)
8.a Riding coordinates:
 C4(H4A,H4B,H4C)
8.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C13(H13A,H13B), C10(H10A,H10B), C10(H10C,H10D), C15(H15A,
 H15B), C14(H14A,H14B), C6(H6A,H6B), C9(H9A,H9B), C5(H5A,H5B), C12(H12A,H12B),
 C12(H12C,H12D), C11(H11A,H11B), C8(H8AA,H8AB), C8(H8BC,H8BD), C7(H7A,H7B),
 C9A(H9AA,H9AB), C7A(H7AA,H7AB), C11A(H11C,H11D), C1(H1A,H1B), C3(H3A,H3B),
 C2(H2A,H2B)
;
_shelx_res_checksum              2608
_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
;