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_7248435
_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         '2(C35 H34 Ir O2 P Se), H2 O'
_chemical_formula_sum            'C70 H70 Ir2 O5 P2 Se2'
_chemical_formula_weight         1595.631
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-09-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-05 deposited with the CCDC.	2024-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                86.012(3)
_cell_angle_beta                 86.316(2)
_cell_angle_gamma                82.180(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6583(3)
_cell_length_b                   18.2265(6)
_cell_length_c                   19.3876(6)
_cell_measurement_reflns_used    17391
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      73.9770
_cell_measurement_theta_min      4.5630
_cell_volume                     3019.12(17)
_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      99.9(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.7110
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9927
_diffrn_measured_fraction_theta_max 0.9702
_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    -20.00  81.00   1.00    1.00    --   40.55 -99.00-180.00  101
  2  \w     23.00 117.00   1.00    1.00    --   40.55  77.00  30.00   94
  3  \w    -29.00  64.00   1.00    1.00    --   40.55 -57.00 -90.00   93
  4  \w     36.00 132.00   1.00    1.00    --  106.89 -77.00  60.00   96
  5  \w     41.00 115.00   1.00    1.00    --  106.89 -61.00 -60.00   74
  6  \w     39.00 128.00   1.00    1.00    --  106.89 -61.00-180.00   89
  7  \w     84.00 136.00   1.00    1.00    --  106.89  61.00  60.00   52
  8  \w     84.00 156.00   1.00    1.00    --  106.89  45.00 -30.00   72
  9  \w     82.00 158.00   1.00    1.00    --  106.89  77.00   0.00   76
 10  \w     31.00 129.00   1.00    1.00    --  106.89 -30.00  60.00   98
 11  \w     83.00 157.00   1.00    1.00    --  106.89  45.00 -90.00   74
 12  \w     67.00 121.00   1.00    1.00    --  106.89-125.00 -30.00   54
 13  \w     12.00 114.00   1.00    1.00    --   40.55  57.00 -30.00  102
 14  \w     12.00 114.00   1.00    1.00    --   40.55  57.00 150.00  102
 15  \w     12.00 114.00   1.00    1.00    --   40.55  57.00-120.00  102
 16  \w     74.00 158.00   1.00    1.00    --  106.89  77.00  30.00   84
 17  \w     78.00 158.00   1.00    1.00    --  106.89  61.00-150.00   80
 18  \w     34.00 121.00   1.00    1.00    --  106.89-125.00   0.00   87
 19  \w     74.00 158.00   1.00    1.00    --  106.89  77.00 -30.00   84
 20  \w     74.00 158.00   1.00    1.00    --  106.89  77.00 -90.00   84
 21  \w     54.00 158.00   1.00    1.00    --  106.89  15.00-180.00  104
 22  \w   -114.00 -55.00   1.00    1.00    --  -40.55-153.00 -38.00   59
;
_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      0.0464059000
_diffrn_orient_matrix_UB_12      -0.0160935000
_diffrn_orient_matrix_UB_13      0.0754903000
_diffrn_orient_matrix_UB_21      0.1735195000
_diffrn_orient_matrix_UB_22      -0.0027481000
_diffrn_orient_matrix_UB_23      -0.0242923000
_diffrn_orient_matrix_UB_31      -0.0096369000
_diffrn_orient_matrix_UB_32      0.0839047000
_diffrn_orient_matrix_UB_33      0.0086860000
_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  0.0349
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.9927
_diffrn_reflns_Laue_measured_fraction_max 0.9702
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33217
_diffrn_reflns_point_group_measured_fraction_full 0.9927
_diffrn_reflns_point_group_measured_fraction_max 0.9702
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         73.98
_diffrn_reflns_theta_min         3.46
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.693
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.502
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1548.695
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.027
_refine_diff_density_max         1.2972
_refine_diff_density_min         -1.2753
_refine_diff_density_rms         0.1852
_refine_ls_d_res_high            0.8021
_refine_ls_d_res_low             12.7894
_refine_ls_goodness_of_fit_ref   1.0508
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    119
_refine_ls_number_parameters     774
_refine_ls_number_reflns         11878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0508
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+22.7998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              22
_reflns_limit_k_min              -21
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                10977
_reflns_number_total             11878
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ra00926f2.cif
_cod_data_source_block           Crystal321
_cod_original_cell_volume        3019.12(16)
_cod_database_code               7248435
_chemical_oxdiff_formula         C35H34O2IrSeP
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Sof: Se1B(0.65) Se1C(0.35) O2BA(0.65) O1B(0.65) O1C(0.35) C7B(0.35)
 O2C(0.35) C75B(0.65)
2.a Free rotating group:
 O3(H3c,H3d)
2.b Aromatic/amide H refined with riding coordinates:
 C45A(H45A), C45B(H45B), C26A(H26A), C46B(H46B), C24B(H24B), C33A(H33A),
 C25B(H25B), C23A(H23A), C44A(H44A), C25A(H25A), C35B(H35B), C4A(H4A),
 C35A(H35A), C26B(H26B), C32A(H32A), C43B(H43B), C3B(H3B), C6A(H6A), C22A(H22A),
  C42A(H42A), C46A(H46A), C6B(H6B), C44B(H44B), C34A(H34A), C5A(H5A),
 C36A(H36A), C22B(H22B), C36B(H36B), C24A(H24A), C32B(H32B), C3A(H3A),
 C33B(H33B), C42B(H42B), C23B(H23B), C4B(H4B), C5B(H5B), C34B(H34B), C43A(H43A)
2.c Idealised Me refined as rotating group:
 C15A(H15d,H15e,H15f), C13A(H13d,H13e,H13f), C17B(H17a,H17b,H17c), C14A(H14d,
 H14e,H14f), C16A(H16d,H16e,H16f), C13B(H13a,H13b,H13c), C16B(H16a,H16b,H16c),
 C14B(H14a,H14b,H14c), C17A(H17d,H17e,H17f), C15B(H15a,H15b,H15c)
;
_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 2.914
_oxdiff_exptl_absorpt_empirical_full_min 0.564