#------------------------------------------------------------------------------
#$Date: 2024-12-06 19:30:37 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296463 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/93/7249336.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7249336
loop_
_publ_author_name
'Rozhkov, Anton V.'
'Tupikina, Elena Yu.'
'Tugashov, Kirill I.'
'Kukushkin, Vadim Yu.'
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     48.00  73.00   0.50    0.40    --   47.12  76.00-114.00   50
  2  ω    101.00 129.00   0.50    1.40    --  105.95  30.00-150.00   56
  3  ω    139.00 174.00   0.50    1.40    --  105.95  30.00-150.00   70
  4  ω    153.00 178.00   0.50    1.40    --  105.95  30.00-180.00   50
  5  ω    113.00 139.00   0.50    1.40    --  105.95  30.00-180.00   52
  6  ω     85.00 161.00   0.50    1.40    --  105.95  76.00-114.00  152
  7  ω    153.00 178.00   0.50    1.40    --  105.95  45.00 150.00   50
  8  ω    107.00 132.00   0.50    1.40    --  105.95  45.00 150.00   50
  9  ω     36.00  67.00   0.50    1.40    --  105.95 -61.00  30.00   62
 10  ω     33.00  95.00   0.50    1.40    --  105.95 -76.00 118.00  124
 11  ω    -15.00  67.00   0.50    0.40    --   47.12 -76.00 118.00  164
 12  ω     78.00 120.00   0.50    0.40    --   47.12 125.00  90.00   84
 13  ω    -67.00 -34.00   0.50    1.40    -- -105.95  61.00  30.00   66
 14  ω   -103.00 -70.00   0.50    1.40    -- -105.95  77.00  90.00   66
 15  ω    -67.00 -34.00   0.50    1.40    -- -105.95  77.00  90.00   66
 16  ω    -49.00  21.00   0.50    0.40    --  -47.12  76.00-114.00  140
 17  ω    -92.00 -43.00   0.50    1.40    -- -105.95  76.00-114.00   98
 18  ω   -177.00 -97.00   0.50    1.40    -- -105.95 -61.00  60.00  160
 19  ω   -173.00-147.00   0.50    1.40    -- -105.95 -76.00 118.00   52
 20  ω    -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       'ω 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/[σ²(Fo²)+(0.0787P)²] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Hg1D Hg 0.000000 0.500000 1.000000 0.0394(11) Uani 1 4 d S T P . .
Pd1 Pd 0.000000 0.000000 1.000000 0.0346(11) Uani 1 4 d S T P . .
F1D F -0.0371(4) 0.500000 0.7992(3) 0.0493(15) Uani 1 2 d S T P . .
O1 O 0.0231(4) 0.000000 1.1266(3) 0.0415(15) Uani 1 2 d S T P . .
F4D F 0.4213(4) 0.500000 0.9111(3) 0.0543(15) Uani 1 2 d S T P . .
O2 O -0.1659(4) 0.000000 1.0077(3) 0.0389(14) Uani 1 2 d S T P . .
F3D F 0.3395(5) 0.500000 0.7413(4) 0.0548(18) Uani 1 2 d S T P . .
F5D F 0.2738(4) 0.500000 1.0243(3) 0.0512(16) Uani 1 2 d S T P . .
F2D F 0.1108(4) 0.500000 0.6859(3) 0.0553(15) Uani 1 2 d S T P . .
C1 C 0.1202(7) 0.000000 1.2666(4) 0.0459(19) Uani 1 2 d S T P . .
H1A H 0.068746 0.113661 1.280402 0.069 Uiso 0.5 1 calc R U P A -1
H1B H 0.197376 0.026426 1.297194 0.069 Uiso 0.5 1 calc R U P A -1
H1C H 0.093010 -0.140087 1.283570 0.069 Uiso 0.5 1 calc R U P A -1
C1D C 0.1144(6) 0.500000 0.9143(4) 0.0392(17) Uani 1 2 d S T P . .
C2 C 0.1223(6) 0.000000 1.1713(4) 0.0389(17) Uani 1 2 d S T P . .
C5 C -0.3638(6) 0.000000 0.9621(5) 0.049(2) Uani 1 2 d S T P . .
H5A H -0.362623 0.043918 1.021378 0.073 Uiso 0.5 1 calc R U P B -1
H5B H -0.396107 -0.145143 0.953667 0.073 Uiso 0.5 1 calc R U P B -1
H5C H -0.410634 0.101225 0.924289 0.073 Uiso 0.5 1 calc R U P B -1
C2D C 0.0767(6) 0.500000 0.8284(4) 0.0419(18) Uani 1 2 d S T P . .
C3D C 0.1504(9) 0.500000 0.7701(6) 0.046(2) Uani 1 2 d S T P . .
C5D C 0.3089(6) 0.500000 0.8841(5) 0.0443(19) Uani 1 2 d S T P . .
C6D C 0.2320(6) 0.500000 0.9407(5) 0.0448(18) Uani 1 2 d S T P . .
C3 C 0.2267(6) 0.000000 1.1429(5) 0.0421(18) Uani 1 2 d S T P . .
H3 H 0.293193 0.000000 1.184947 0.051 Uiso 1 2 calc R U P . .
C4D C 0.2683(6) 0.500000 0.7971(5) 0.0452(18) Uani 1 2 d S T P . .
C4 C -0.2429(6) 0.000000 0.9422(5) 0.0434(19) Uani 1 2 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -4.2923 7.6849 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Pd1 Hg1D Pd1 180.0 . 1_565 ?
C1D Hg1D Pd1 90.000(2) 5_567 . ?
C1D Hg1D Pd1 90.000(1) . 1_565 ?
C1D Hg1D Pd1 90.000(1) . . ?
C1D Hg1D Pd1 90.000(2) 5_567 1_565 ?
C1D Hg1D C1D 180.0 . 5_567 ?
Hg1D Pd1 Hg1D 180.0 . 1_545 ?
O1 Pd1 Hg1D 90.000(1) 5_557 1_545 ?
O1 Pd1 Hg1D 90.000(1) 5_557 . ?
O1 Pd1 Hg1D 90.000(1) . 1_545 ?
O1 Pd1 Hg1D 90.000(1) . . ?
O1 Pd1 O1 180.0 . 5_557 ?
O2 Pd1 Hg1D 90.000(1) 5_557 1_545 ?
O2 Pd1 Hg1D 90.000(1) 5_557 . ?
O2 Pd1 Hg1D 90.000(1) . 1_545 ?
O2 Pd1 Hg1D 90.000(1) . . ?
O2 Pd1 O1 94.84(18) 5_557 . ?
O2 Pd1 O1 94.84(18) . 5_557 ?
O2 Pd1 O1 85.16(18) . . ?
O2 Pd1 O1 85.16(18) 5_557 5_557 ?
O2 Pd1 O2 180.0 5_557 . ?
C2 O1 Pd1 122.1(4) . . ?
C4 O2 Pd1 122.5(5) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C2D C1D Hg1D 121.0(5) . . ?
C2D C1D C6D 116.9(6) . . ?
C6D C1D Hg1D 122.1(5) . . ?
O1 C2 C1 113.4(6) . . ?
O1 C2 C3 127.7(6) . . ?
C3 C2 C1 118.9(6) . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
F1D C2D C1D 119.5(6) . . ?
F1D C2D C3D 118.3(7) . . ?
C1D C2D C3D 122.3(7) . . ?
F2D C3D C2D 120.9(8) . . ?
F2D C3D C4D 118.7(8) . . ?
C2D C3D C4D 120.4(8) . . ?
F4D C5D C6D 121.3(7) . . ?
F4D C5D C4D 119.4(6) . . ?
C6D C5D C4D 119.3(7) . . ?
F5D C6D C1D 119.5(7) . . ?
F5D C6D C5D 117.9(7) . . ?
C5D C6D C1D 122.6(7) . . ?
C2 C3 H3 117.1 . . ?
C2 C3 C4 125.8(6) . 5_557 ?
C4 C3 H3 117.1 5_557 . ?
F3D C4D C3D 120.7(7) . . ?
F3D C4D C5D 120.8(7) . . ?
C5D C4D C3D 118.5(7) . . ?
O2 C4 C5 114.0(7) . . ?
O2 C4 C3 127.0(7) . 5_557 ?
C3 C4 C5 118.9(6) 5_557 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hg1D Pd1 3.1033(3) . ?
Hg1D Pd1 3.1033(3) 1_565 ?
Hg1D C1D 2.071(7) . ?
Hg1D C1D 2.071(7) 5_567 ?
Pd1 O1 1.991(5) . ?
Pd1 O1 1.991(5) 5_557 ?
Pd1 O2 1.990(5) . ?
Pd1 O2 1.990(5) 5_557 ?
F1D C2D 1.355(8) . ?
O1 C2 1.274(8) . ?
F4D C5D 1.333(8) . ?
O2 C4 1.273(9) . ?
F3D C4D 1.320(10) . ?
F5D C6D 1.345(9) . ?
F2D C3D 1.348(11) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.522(9) . ?
C1D C2D 1.370(10) . ?
C1D C6D 1.391(10) . ?
C2 C3 1.383(10) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C5 C4 1.516(10) . ?
C2D C3D 1.373(13) . ?
C3D C4D 1.395(13) . ?
C5D C6D 1.380(11) . ?
C5D C4D 1.393(11) . ?
C3 H3 0.9500 . ?
C3 C4 1.399(11) 5_557 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Hg1D C1D C2D F1D 0.000(3) . . . . ?
Hg1D C1D C2D C3D 180.000(3) . . . . ?
Hg1D C1D C6D F5D 0.000(3) . . . . ?
Hg1D C1D C6D C5D 180.000(3) . . . . ?
Pd1 O1 C2 C1 180.000(3) . . . . ?
Pd1 O1 C2 C3 0.000(4) . . . . ?
Pd1 O2 C4 C5 180.000(2) . . . . ?
Pd1 O2 C4 C3 0.000(4) . . . 5_557 ?
F1D C2D C3D F2D 0.000(4) . . . . ?
F1D C2D C3D C4D 180.000(3) . . . . ?
O1 C2 C3 C4 0.000(5) . . . 5_557 ?
F4D C5D C6D F5D 0.000(4) . . . . ?
F4D C5D C6D C1D 180.000(3) . . . . ?
F4D C5D C4D F3D 0.000(4) . . . . ?
F4D C5D C4D C3D 180.000(3) . . . . ?
F2D C3D C4D F3D 0.000(3) . . . . ?
F2D C3D C4D C5D 180.000(3) . . . . ?
C1 C2 C3 C4 180.000(4) . . . 5_557 ?
C1D C2D C3D F2D 180.000(2) . . . . ?
C1D C2D C3D C4D 0.000(4) . . . . ?
C2D C1D C6D F5D 180.000(2) . . . . ?
C2D C1D C6D C5D 0.000(4) . . . . ?
C2D C3D C4D F3D 180.000(4) . . . . ?
C2D C3D C4D C5D 0.000(4) . . . . ?
C6D C1D C2D F1D 180.000(2) . . . . ?
C6D C1D C2D C3D 0.000(4) . . . . ?
C6D C5D C4D F3D 180.000(3) . . . . ?
C6D C5D C4D C3D 0.000(4) . . . . ?
C4D C5D C6D F5D 180.000(2) . . . . ?
C4D C5D C6D C1D 0.000(4) . . . . ?
