Selenosalicylate; a little-studied heavy-element analogue of the versatile thiosalicylate ligand
Atiga, Simeon; Saunders, Graham C.; Henderson, William; RSC Advances 14 (2024) 12323–12336; doi:10.1039/D4RA00926F

data_7248434
_publ_section_title
;
 Selenosalicylate; a little-studied heavy-element analogue of the
 versatile thiosalicylate ligand
;
_journal_issue                   18
_journal_name_full               'RSC Advances'
_journal_page_first              12323
_journal_page_last               12336
_journal_paper_doi               10.1039/D4RA00926F
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C34 H38 O4 Rh2 Se2'
_chemical_formula_sum            'C34 H38 O4 Rh2 Se2'
_chemical_formula_weight         874.408
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-10-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-10-05 deposited with the CCDC.	2024-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.2080(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.24520(15)
_cell_length_b                   10.02131(11)
_cell_length_c                   14.11953(18)
_cell_measurement_reflns_used    8367
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      74.0230
_cell_measurement_theta_min      4.6660
_cell_volume                     1570.65(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.7110
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9982
_diffrn_measured_fraction_theta_max 0.9821
_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     17.00 106.00   1.00    1.00    --   40.55  38.00-150.00   89
  2  \w      4.00  96.00   1.00    1.00    --   40.55-125.00  60.00   92
  3  \w     35.00 134.00   1.00    1.22    --  106.89 -61.00  60.00   99
  4  \w     79.00 155.00   1.00    1.22    --  106.89  30.00 -60.00   76
  5  \w     75.00 158.00   1.00    1.22    --  106.89  77.00-150.00   83
  6  \w    110.00 158.00   1.00    1.22    --  106.89  30.00 150.00   48
  7  \w     80.00 106.00   1.00    1.22    --  106.89  30.00 150.00   26
  8  \w     12.00 114.00   1.00    1.00    --   40.55  57.00  60.00  102
  9  \w     12.00 114.00   1.00    1.00    --   40.55  57.00 -60.00  102
 10  \w     73.00 158.00   1.00    1.22    --  106.89 125.00  30.00   85
 11  \w     34.00 121.00   1.00    1.22    --  106.89-125.00  60.00   87
 12  \w     74.00 158.00   1.00    1.22    --  106.89  77.00  90.00   84
 13  \w     78.00 158.00   1.00    1.22    --  106.89  61.00   0.00   80
 14  \w    -32.00  69.00   1.00    1.00    --   40.55 -57.00 150.00  101
 15  \w      8.00 117.00   1.00    1.00    --   40.55  77.00  90.00  109
 16  \w     78.00 158.00   1.00    1.22    --  106.89  61.00-180.00   80
 17  \w     74.00 158.00   1.00    1.22    --  106.89  77.00 -60.00   84
 18  \w     74.00 158.00   1.00    1.22    --  106.89  77.00  30.00   84
 19  \w     31.00 139.00   1.00    1.22    --  106.89 -77.00-150.00  108
 20  \w      8.00  68.00   1.00    1.00    --   40.55  77.00-120.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0814875000
_diffrn_orient_matrix_UB_12      0.0877312000
_diffrn_orient_matrix_UB_13      -0.0522797000
_diffrn_orient_matrix_UB_21      0.0001894000
_diffrn_orient_matrix_UB_22      -0.1091396000
_diffrn_orient_matrix_UB_23      -0.0768005000
_diffrn_orient_matrix_UB_31      -0.1123049000
_diffrn_orient_matrix_UB_32      0.0634377000
_diffrn_orient_matrix_UB_33      -0.0599329000
_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  0.0449
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.9982
_diffrn_reflns_Laue_measured_fraction_max 0.9821
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15243
_diffrn_reflns_point_group_measured_fraction_full 0.9982
_diffrn_reflns_point_group_measured_fraction_max 0.9821
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         74.01
_diffrn_reflns_theta_min         4.68
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.446
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_description       block
_exptl_crystal_F_000             863.590
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.7055
_refine_diff_density_min         -1.0500
_refine_diff_density_rms         0.1801
_refine_ls_d_res_high            0.8019
_refine_ls_d_res_low             9.4512
_refine_ls_goodness_of_fit_ref   1.0342
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    28
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0342
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+1.0168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0532
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -13
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              -9
_reflns_number_gt                2842
_reflns_number_total             3131
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ra00926f2.cif
_cod_data_source_block           Crystal330
_cod_original_cell_volume        1570.65(4)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7248434
_chemical_oxdiff_formula         C36H45Rh2O4Se2
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C5(H5), C4(H4)
2.b Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C13(H13a,H13b,
 H13c), C16(H16a,H16b,H16c)
;
_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 3.061
_oxdiff_exptl_absorpt_empirical_full_min 0.656