Palladium(II) ortho-cyano-aminothiophenolate (ocap) complexes
Hogarth, Graeme; Al-Jibori, Subhi A.; Al-Janabi, Ahmed; Irzoqi, Ahmed A.; Basak-Modi, Sucharita; Orton, Georgia; Ghosh, Shishir; Wagner, Christoph; Abdullah, Ali I. A.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02681C

data_7711753
_publ_section_title
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 Palladium(II) ortho-cyano-aminothiophenolate (ocap) complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02681C
_journal_year                    2022
_chemical_formula_moiety         'C24 H30 O6'
_chemical_formula_sum            'C24 H30 O6'
_chemical_formula_weight         414.502
_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     dual
_audit_creation_date             2022-08-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_audit_update_record
;
2022-08-16 deposited with the CCDC.	2022-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.999(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5737(1)
_cell_length_b                   8.7917(1)
_cell_length_c                   18.8453(2)
_cell_measurement_reflns_used    23938
_cell_measurement_temperature    100.1(5)
_cell_measurement_theta_max      74.5820
_cell_measurement_theta_min      4.0280
_cell_volume                     2075.31(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.1(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9809
_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    -74.00  25.00   0.50    0.12    --  -47.95  85.00 -44.00  198
  2  \w    -24.00  74.00   0.50    0.12    --   47.95 -85.00-163.00  196
  3  \w   -127.00 -28.00   0.50    0.50    -- -101.00  85.00 -44.00  198
  4  \w   -173.00 -79.00   0.50    0.50    -- -101.00 -85.00-163.00  188
  5  \w     31.00 130.00   0.50    0.50    --  103.25 -85.00-163.00  198
  6  \w     86.00 176.00   0.50    0.50    --  103.25  85.00 -44.00  180
  7  \w   -120.00 -74.00   0.50    0.12    --  -47.95-125.00   0.00   92
  8  \w   -120.00 -74.00   0.50    0.12    --  -47.95-125.00 -90.00   92
  9  \w     33.00 119.00   0.50    0.12    --   47.95  57.00 -30.00  172
 10  \w     33.00 119.00   0.50    0.12    --   47.95  57.00  30.00  172
 11  \w     19.00  96.00   0.50    0.12    --   47.95-125.00 150.00  154
 12  \w   -115.00 -26.00   0.50    0.50    -- -101.00  15.00 -30.00  178
 13  \w   -173.00 -84.00   0.50    0.50    -- -101.00 -94.00 -30.00  178
 14  \w   -174.00 -88.00   0.50    0.50    -- -101.00 -30.00  90.00  172
 15  \w   -173.00 -84.00   0.50    0.50    -- -101.00 -61.00 -90.00  178
 16  \w     28.00 116.00   0.50    0.50    --  103.25 -30.00-180.00  176
 17  \w     91.00 175.00   0.50    0.50    --  103.25  45.00-120.00  168
 18  \w     91.00 178.00   0.50    0.50    --  103.25  30.00  90.00  174
 19  \w     91.00 178.00   0.50    0.50    --  103.25  30.00  30.00  174
 20  \w     32.00 116.00   0.50    0.50    --  103.25 -45.00 -90.00  168
 21  \w     31.00 111.00   0.50    0.50    --  103.25-125.00-180.00  160
 22  \w     91.00 178.00   0.50    0.50    --  103.25  30.00   0.00  174
 23  \w     31.00 106.00   0.50    0.50    --  103.25 -94.00  90.00  150
 24  \w     91.00 175.00   0.50    0.50    --  103.25  45.00 -90.00  168
 25  \w     33.00 119.00   0.50    0.12    --   47.95  57.00 120.00  172
 26  \w     25.00 120.00   0.50    0.12    --   47.95  77.00-180.00  190
 27  \w     25.00 120.00   0.50    0.12    --   47.95  77.00  60.00  190
 28  \w     25.00 120.00   0.50    0.12    --   47.95  77.00 150.00  190
 29  \w     25.00 120.00   0.50    0.12    --   47.95  77.00-120.00  190
 30  \w     81.00 143.00   0.50    0.50    --  103.25  77.00-180.00  124
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1142234000
_diffrn_orient_matrix_UB_12      0.0355466000
_diffrn_orient_matrix_UB_13      -0.0320019000
_diffrn_orient_matrix_UB_21      0.0024080000
_diffrn_orient_matrix_UB_22      0.1511339000
_diffrn_orient_matrix_UB_23      0.0414759000
_diffrn_orient_matrix_UB_31      0.0455138000
_diffrn_orient_matrix_UB_32      0.0812385000
_diffrn_orient_matrix_UB_33      -0.0631715000
_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  0.0905
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9809
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38356
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9809
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         75.35
_diffrn_reflns_theta_min         4.07
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.42a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       needle
_exptl_crystal_F_000             891.005
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.4682
_refine_diff_density_min         -0.3342
_refine_diff_density_rms         0.0604
_refine_ls_d_res_high            0.7968
_refine_ls_d_res_low             10.8659
_refine_ls_goodness_of_fit_ref   1.0390
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    47
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0390
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.0154
_refine_ls_shift/su_mean         0.0005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+1.0289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -15
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              -11
_reflns_number_gt                3827
_reflns_number_total             4212
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt02681c2.cif
_cod_data_source_block           CYZ-140-1C
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7711753
_reflns_odcompleteness_completeness 99.97
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C8(H8), C6'(H6'), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4a,H4b), C5(H5a,H5b), C4'(H4'a,H4'b), C9'(H9'a,H9'b), C8'(H8'a,H8'b),
 C9(H9a,H9b), C5'(H5'a,H5'b), C10'(H10a,H10b), C10(H10c,H10d)
2.c Aromatic/amide H refined with riding coordinates:
 C7'(H7'), C7(H7)
2.d Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C11'(H11d,H11e,H11f)
2.e Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_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 3.398
_oxdiff_exptl_absorpt_empirical_full_min 0.239