Pure heterometallic spodium bonding
Rozhkov, Anton V.; Tupikina, Elena Yu.; Tugashov, Kirill I.; Kukushkin, Vadim Yu.; CrystEngComm 26 (2024) 5607–5616; doi:10.1039/D4CE00825A

data_7249337
_publ_section_title
;
 Pure heterometallic spodium bonding
;
_journal_issue                   39
_journal_name_full               CrystEngComm
_journal_page_first              5607
_journal_page_last               5616
_journal_paper_doi               10.1039/D4CE00825A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C22 H14 F10 Hg O4 Pt'
_chemical_formula_sum            'C22 H14 F10 Hg O4 Pt'
_chemical_formula_weight         928.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-02 deposited with the CCDC.	2024-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.276(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8245(3)
_cell_length_b                   6.2102(2)
_cell_length_c                   15.9199(4)
_cell_measurement_reflns_used    4765
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.6430
_cell_measurement_theta_min      4.3330
_cell_volume                     1153.75(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_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    -68.00  20.00   0.50    0.20    --  -47.38  74.00 131.00  176
  2  \w    -24.00  20.00   0.50    0.20    --   47.38 -74.00   3.00   88
  3  \w     23.00  51.00   0.50    0.20    --   47.38 -74.00   3.00   56
  4  \w     73.00 105.00   0.50    0.20    --   47.38  74.00 131.00   64
  5  \w    -95.00 -40.00   0.50    0.80    -- -106.00  74.00 131.00  110
  6  \w   -168.00-127.00   0.50    0.80    -- -106.00 -74.00   3.00   82
  7  \w    110.00 177.00   0.50    0.80    --  113.25  74.00 131.00  134
  8  \w     48.00  93.00   0.50    0.80    --  113.25 -74.00   3.00   90
  9  \w    -97.00 -72.00   0.50    0.20    --  -47.38 -74.00   3.00   50
 10  \w     75.00 102.00   0.50    0.20    --   47.38 125.00   0.00   54
 11  \w     74.00 119.00   0.50    0.20    --   47.38 125.00 -30.00   90
 12  \w    -64.00 -38.00   0.50    0.80    -- -106.00  61.00 120.00   52
 13  \w    -69.00 -34.00   0.50    0.80    -- -106.00  61.00 -30.00   70
 14  \w     44.00  70.00   0.50    0.80    --  113.25-125.00   0.00   52
 15  \w    121.00 178.00   0.50    0.80    --  113.25  30.00  90.00  114
 16  \w     45.00  72.00   0.50    0.80    --  113.25 -94.00-180.00   54
 17  \w     51.00 104.00   0.50    0.80    --  113.25 -94.00-150.00  106
 18  \w     75.00 103.00   0.50    0.80    --  113.25 -94.00 -90.00   56
 19  \w     42.00  67.00   0.50    0.80    --  113.25 -61.00-150.00   50
 20  \w     43.00  70.00   0.50    0.80    --  113.25 -61.00  30.00   54
 21  \w    101.00 127.00   0.50    0.80    --  113.25  45.00  90.00   52
 22  \w    148.00 175.00   0.50    0.80    --  113.25  45.00  90.00   54
 23  \w    150.00 175.00   0.50    0.80    --  113.25  30.00  30.00   50
 24  \w    123.00 149.00   0.50    0.80    --  113.25  30.00  30.00   52
 25  \w     75.00 106.00   0.50    0.80    --  113.25-125.00   0.00   62
 26  \w     46.00  71.00   0.50    0.80    --  113.25 -94.00 -90.00   50
 27  \w     45.00  70.00   0.50    0.80    --  113.25 -74.00   3.00   50
 28  \w     -5.00  21.00   0.50    0.20    --  -47.38  19.00 120.00   52
 29  \w    -12.00  28.00   0.50    0.20    --  -47.38  19.00  90.00   80
 30  \w    -24.00  22.00   0.50    0.20    --   47.38 -19.00  60.00   92
 31  \w   -158.00-129.00   0.50    0.80    -- -106.00 -15.00-150.00   58
 32  \w   -125.00 -93.00   0.50    0.80    -- -106.00 -15.00-150.00   64
 33  \w    -58.00 -33.00   0.50    0.80    -- -106.00 125.00   0.00   50
 34  \w   -163.00-137.00   0.50    0.80    -- -106.00 -61.00 -90.00   52
 35  \w   -131.00 -84.00   0.50    0.80    -- -106.00 -77.00 -60.00   94
 36  \w   -142.00 -94.00   0.50    0.80    -- -106.00 -15.00 -90.00   96
 37  \w   -141.00 -93.00   0.50    0.80    -- -106.00 -30.00-150.00   96
 38  \w   -126.00 -91.00   0.50    0.80    -- -106.00 -61.00 -90.00   70
 39  \w   -105.00 -73.00   0.50    0.80    -- -106.00 125.00   0.00   64
 40  \w   -133.00-107.00   0.50    0.80    -- -106.00 -45.00  60.00   52
 41  \w     92.00 133.00   0.50    0.80    --  113.25  77.00 150.00   82
 42  \w     48.00  74.00   0.50    0.80    --  113.25-125.00 150.00   52
 43  \w    148.00 174.00   0.50    0.80    --  113.25  77.00 120.00   52
 44  \w    105.00 137.00   0.50    0.80    --  113.25  77.00 120.00   64
 45  \w     42.00  67.00   0.50    0.80    --  113.25 -61.00  60.00   50
 46  \w     69.00  95.00   0.50    0.80    --  113.25 -77.00  90.00   52
 47  \w    135.00 170.00   0.50    0.80    --  113.25  61.00-120.00   70
 48  \w    138.00 169.00   0.50    0.80    --  113.25  77.00 150.00   62
 49  \w     65.00  91.00   0.50    0.80    --  113.25 -94.00  30.00   52
 50  \w     86.00 111.00   0.50    0.80    --  113.25-125.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0288959000
_diffrn_orient_matrix_UB_12      -0.0766633000
_diffrn_orient_matrix_UB_13      0.0860927000
_diffrn_orient_matrix_UB_21      0.0845363000
_diffrn_orient_matrix_UB_22      -0.1889518000
_diffrn_orient_matrix_UB_23      0.0000737000
_diffrn_orient_matrix_UB_31      0.0971236000
_diffrn_orient_matrix_UB_32      0.1412463000
_diffrn_orient_matrix_UB_33      0.0470103000
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6349
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.849
_diffrn_reflns_theta_min         4.340
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.988
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.671
_exptl_crystal_description       prism
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.001
_refine_diff_density_min         -1.537
_refine_diff_density_rms         0.303
_refine_ls_extinction_coef       0.00075(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0652P)^2^+0.4526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1233
_reflns_number_total             1336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00825a2.cif
_cod_data_source_block           030-057_rav-864
_cod_depositor_comments
'Adding full bibliography for 7249336--7249337.cif.'
_cod_database_code               7249337
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 H14 F10 Hg O4 Pt'
_shelx_estimated_absorpt_t_max   0.533
_shelx_estimated_absorpt_t_min   0.327
_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. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              66450
_shelx_hkl_checksum              32122
_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 2.415
_oxdiff_exptl_absorpt_empirical_full_min 0.426