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_7249336
_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 Pd'
_chemical_formula_sum            'C22 H14 F10 Hg O4 Pd'
_chemical_formula_weight         839.32
_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                 99.161(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8573(9)
_cell_length_b                   6.2066(5)
_cell_length_c                   15.9257(12)
_cell_measurement_reflns_used    2809
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.4250
_cell_measurement_theta_min      4.3320
_cell_volume                     1157.08(16)
_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 0.980
_diffrn_measured_fraction_theta_max 0.960
_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     48.00  73.00   0.50    0.40    --   47.12  76.00-114.00   50
  2  \w    101.00 129.00   0.50    1.40    --  105.95  30.00-150.00   56
  3  \w    139.00 174.00   0.50    1.40    --  105.95  30.00-150.00   70
  4  \w    153.00 178.00   0.50    1.40    --  105.95  30.00-180.00   50
  5  \w    113.00 139.00   0.50    1.40    --  105.95  30.00-180.00   52
  6  \w     85.00 161.00   0.50    1.40    --  105.95  76.00-114.00  152
  7  \w    153.00 178.00   0.50    1.40    --  105.95  45.00 150.00   50
  8  \w    107.00 132.00   0.50    1.40    --  105.95  45.00 150.00   50
  9  \w     36.00  67.00   0.50    1.40    --  105.95 -61.00  30.00   62
 10  \w     33.00  95.00   0.50    1.40    --  105.95 -76.00 118.00  124
 11  \w    -15.00  67.00   0.50    0.40    --   47.12 -76.00 118.00  164
 12  \w     78.00 120.00   0.50    0.40    --   47.12 125.00  90.00   84
 13  \w    -67.00 -34.00   0.50    1.40    -- -105.95  61.00  30.00   66
 14  \w   -103.00 -70.00   0.50    1.40    -- -105.95  77.00  90.00   66
 15  \w    -67.00 -34.00   0.50    1.40    -- -105.95  77.00  90.00   66
 16  \w    -49.00  21.00   0.50    0.40    --  -47.12  76.00-114.00  140
 17  \w    -92.00 -43.00   0.50    1.40    -- -105.95  76.00-114.00   98
 18  \w   -177.00 -97.00   0.50    1.40    -- -105.95 -61.00  60.00  160
 19  \w   -173.00-147.00   0.50    1.40    -- -105.95 -76.00 118.00   52
 20  \w    -92.00 -26.00   0.50    0.40    --  -47.12 -76.00 118.00  132
;
_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      -0.0615578000
_diffrn_orient_matrix_UB_12      0.2059656000
_diffrn_orient_matrix_UB_13      0.0227878000
_diffrn_orient_matrix_UB_21      0.0768016000
_diffrn_orient_matrix_UB_22      0.0070953000
_diffrn_orient_matrix_UB_23      0.0876355000
_diffrn_orient_matrix_UB_31      0.0875952000
_diffrn_orient_matrix_UB_32      0.1379428000
_diffrn_orient_matrix_UB_33      -0.0373729000
_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  0.0620
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3301
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.390
_diffrn_reflns_theta_min         4.335
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.045
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20948
_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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.409
_exptl_crystal_description       prism
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.020
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0787P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1172
_reflns_number_total             1210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00825a2.cif
_cod_data_source_block           0ver0-24446_zmv-018
_cod_depositor_comments
'Adding full bibliography for 7249336--7249337.cif.'
_cod_database_code               7249336
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 H14 F10 Hg O4 Pd'
_shelx_estimated_absorpt_t_max   0.702
_shelx_estimated_absorpt_t_min   0.208
_olex2_refinement_description
;
1. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              24326
_shelx_hkl_checksum              19464
_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 4.670
_oxdiff_exptl_absorpt_empirical_full_min 0.400