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_7248432
_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         'C43 H34 O2 P2 Pt Se'
_chemical_formula_sum            'C43 H34 O2 P2 Pt Se'
_chemical_formula_weight         918.733
_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             2020-10-12
_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                 92.1926(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.47661(14)
_cell_length_b                   17.9492(2)
_cell_length_c                   17.0666(3)
_cell_measurement_reflns_used    10274
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.8370
_cell_measurement_theta_min      4.5440
_cell_volume                     3513.08(8)
_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 0.9975
_diffrn_measured_fraction_theta_max 0.9766
_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    -97.00  -2.00   1.00    1.00    --  -40.55 125.00 -30.00   95
  2  \w     17.00 115.00   1.00    1.00    --   40.55  38.00-150.00   98
  3  \w     78.00 158.00   1.00    1.00    --  106.89  61.00 120.00   80
  4  \w     38.00 139.00   1.00    1.00    --  106.89 -77.00  60.00  101
  5  \w     74.00 158.00   1.00    1.00    --  106.89  77.00-150.00   84
  6  \w     73.00 158.00   1.00    1.00    --  106.89 125.00 120.00   85
  7  \w     16.00 115.00   1.00    1.00    --   40.55  38.00  60.00   99
  8  \w     12.00 114.00   1.00    1.00    --   40.55  57.00 -60.00  102
  9  \w     74.00 158.00   1.00    1.00    --  106.89  77.00  30.00   84
 10  \w     34.00 121.00   1.00    1.00    --  106.89-125.00 -30.00   87
 11  \w     81.00 158.00   1.00    1.00    --  106.89  45.00 -60.00   77
;
_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      -0.0626130000
_diffrn_orient_matrix_UB_12      0.0571272000
_diffrn_orient_matrix_UB_13      -0.0542132000
_diffrn_orient_matrix_UB_21      -0.0967185000
_diffrn_orient_matrix_UB_22      -0.0572784000
_diffrn_orient_matrix_UB_23      -0.0193655000
_diffrn_orient_matrix_UB_31      -0.0691053000
_diffrn_orient_matrix_UB_32      0.0286099000
_diffrn_orient_matrix_UB_33      0.0696242000
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.9975
_diffrn_reflns_Laue_measured_fraction_max 0.9766
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20367
_diffrn_reflns_point_group_measured_fraction_full 0.9975
_diffrn_reflns_point_group_measured_fraction_max 0.9766
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         73.98
_diffrn_reflns_theta_min         3.57
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.809
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.688
_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            'whiteish orange'
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       block
_exptl_crystal_F_000             1786.830
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.102
_refine_diff_density_max         1.0249
_refine_diff_density_min         -0.7778
_refine_diff_density_rms         0.1122
_refine_ls_d_res_high            0.8021
_refine_ls_d_res_low             12.3634
_refine_ls_goodness_of_fit_ref   1.0462
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     468
_refine_ls_number_reflns         6971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0462
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+2.3784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0574
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -14
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              -10
_reflns_number_gt                6228
_reflns_number_total             6971
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ra00926f2.cif
_cod_data_source_block           Crystal326
_cod_original_cell_volume        3513.09(8)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7248432
_chemical_oxdiff_formula         C25O2SePtP2H34
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: Se1A(0.9) O2A(0.9) O1A(0.9) C7A(0.9) O1B(0.1) Se1B(0.1) O2B(0.1)
 C7B(0.1)
3.a Aromatic/amide H refined with riding coordinates:
 C62(H62), C34(H34), C65(H65), C26(H26), C13(H13), C63(H63), C16(H16),
 C36(H36), C42(H42), C32(H32), C64(H64), C6(H6), C35(H35), C15(H15), C53(H53),
 C56(H56), C22(H22), C24(H24), C54(H54), C5(H5), C25(H25), C43(H43), C14(H14),
 C52(H52), C33(H33), C46(H46), C12(H12), C55(H55), C44(H44), C4(H4), C66(H66),
 C45(H45), C23(H23), C3(H3)
;
_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 2.365
_oxdiff_exptl_absorpt_empirical_full_min 0.629