Palladium complex of macrocyclic selenium ligand: Catalyst for dehydroxymethylation of dihydroxy compounds
Joshi, Hemant; Kumar, Sunil; Singh, Sohan; Mahala, Suman; Janjani, Prachi; Rajagopala Reddy, S.; Rom, Tanmay; Paul, Avijit; Roy, Partha; Dalton Transactions  (2023) –; doi:10.1039/D3DT00375B

data_7712536
_publ_section_title
;
 Palladium complex of macrocyclic selenium ligand: Catalyst for
 dehydroxymethylation of dihydroxy compounds
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00375B
_journal_year                    2023
_chemical_formula_moiety         'C11 H13 O Se0.5'
_chemical_formula_sum            'C11 H13 O Se0.5'
_chemical_formula_weight         200.69
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-09-15
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2022-07-25 deposited with the CCDC.	2023-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.412(2)
_cell_length_b                   23.1159(13)
_cell_length_c                   4.7170(4)
_cell_measurement_reflns_used    818
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      64.6250
_cell_measurement_theta_min      4.7990
_cell_volume                     2007.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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     -6.00  61.00   1.00    1.00    --   25.57  57.00   0.00   67
  2  \w      5.00  31.00   1.00    1.00    --   25.57  57.00  60.00   26
  3  \w     65.00  91.00   1.00    1.00    --   25.57  57.00   0.00   26
  4  \w     54.00 141.00   1.00    2.00    --   66.78  61.00 -30.00   87
  5  \w      1.00  69.00   1.00    2.00    --   66.78 -94.00  60.00   68
  6  \w     -4.00  62.00   1.00    2.00    --   66.78 -94.00 -60.00   66
  7  \w    122.00 177.00   1.00    1.50    --  108.00 138.00 -60.00   55
  8  \w     92.00 175.00   1.00    1.50    --  108.00 138.00-120.00   83
  9  \w     77.00 145.00   1.00    1.50    --  108.00  65.00 -60.00   68
 10  \w     72.00 166.00   1.00    1.50    --  108.00  77.00   0.00   94
 11  \w    122.00 178.00   1.00    1.50    --  108.00 104.00 -90.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0806289000
_diffrn_orient_matrix_UB_12      0.0008155000
_diffrn_orient_matrix_UB_13      -0.0870558000
_diffrn_orient_matrix_UB_21      -0.0214820000
_diffrn_orient_matrix_UB_22      0.0153338000
_diffrn_orient_matrix_UB_23      0.3067798000
_diffrn_orient_matrix_UB_31      0.0060452000
_diffrn_orient_matrix_UB_32      0.0648192000
_diffrn_orient_matrix_UB_33      -0.0715059000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            3480
_diffrn_reflns_theta_full        66.71
_diffrn_reflns_theta_max         66.71
_diffrn_reflns_theta_min         3.82
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.611
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.547
_exptl_crystal_size_min          0.501
_refine_diff_density_max         2.254
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1345
_refine_ls_R_factor_gt           0.0999
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1464P)^2^+7.5883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2731
_refine_ls_wR_factor_ref         0.3115
_reflns_number_gt                1181
_reflns_number_total             1802
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt00375b2.cif
_cod_data_source_block           pab_ag_136_rt_cu
_cod_original_formula_sum        'C11 H13 O Se0.50'
_cod_database_code               7712536
_chemical_oxdiff_formula         'c h n o'
_reflns_odcompleteness_completeness 97.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C4(H4), C5(H5), C11(H11)
;
_olex2_date_sample_data_collection 2021-09-14
_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 3.768
_oxdiff_exptl_absorpt_empirical_full_min 0.527