Unveiling protonated form of 2,6-di-m-phenylpyridine embedded isosmaragdyrin analogue and its organo-Pd(ii) complex
Pradhan, Sourav Ranjan; Murugavel, M.; Chitranshi, Sangya; Kim, Gakhyun; Kim, Dongho; Das, Mainak; Srinivasan, A.; New Journal of Chemistry 47 (2023) 19987–19992; doi:10.1039/D3NJ03432A

data_7062814
_publ_section_title
;
 Unveiling protonated form of 2,6-di-m-phenylpyridine embedded
 isosmaragdyrin analogue and its organo-Pd(ii) complex
;
_journal_issue                   43
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19987
_journal_page_last               19992
_journal_paper_doi               10.1039/D3NJ03432A
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C52 H37 Cl F5 N3 Pd, 0.5[CH2Cl2], 0.35[C6H14]'
_chemical_formula_sum            'C54.6 H42.9 Cl2 F5 N3 Pd'
_chemical_formula_weight         1013.32
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-10-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-01 deposited with the CCDC.	2023-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                92.4420(10)
_cell_angle_beta                 111.581(2)
_cell_angle_gamma                102.638(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7701(2)
_cell_length_b                   13.7846(2)
_cell_length_c                   14.2357(2)
_cell_measurement_reflns_used    26604
_cell_measurement_temperature    112.6(5)
_cell_measurement_theta_max      76.3630
_cell_measurement_theta_min      3.3740
_cell_volume                     2252.78(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      112.60
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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    -63.00 -13.00   0.50    0.75    --    0.00 146.00-147.00  100
  2  \w    -50.00  -2.00   0.50    0.75    --    0.00 125.00  46.00   96
  3  \w     82.00 163.00   0.50    3.00    --  102.08 146.00-147.00  162
  4  \w     39.00 118.00   0.50    3.00    --  102.08-125.00 -32.00  158
  5  \w     94.00 166.00   0.50    3.00    --  102.08 125.00  46.00  144
  6  \w     41.00 132.00   0.50    3.00    --  102.08-146.00 161.00  182
  7  \w    -67.00   1.00   0.50    0.75    --    0.00 -19.00   0.00  136
  8  \w     -1.00  67.00   0.50    0.75    --    0.00  19.00-150.00  136
  9  \w    -61.00  10.00   0.50    0.75    --    0.00 -57.00 -90.00  142
 10  \w    -10.00  61.00   0.50    0.75    --    0.00  57.00 120.00  142
 11  \w     -1.00  65.00   0.50    0.75    --    0.00  37.00   0.00  132
 12  \w     34.00 109.00   0.50    3.00    --  102.08 -94.00 -60.00  150
 13  \w     39.00 105.00   0.50    3.00    --  102.08 -45.00 -30.00  132
 14  \w     91.00 164.00   0.50    3.00    --  102.08  61.00 -60.00  146
 15  \w     39.00 118.00   0.50    3.00    --  102.08-125.00-180.00  158
 16  \w     39.00 105.00   0.50    3.00    --  102.08 -45.00  30.00  132
 17  \w    100.00 170.00   0.50    3.00    --  102.08  15.00  30.00  140
 18  \w     39.00 118.00   0.50    3.00    --  102.08-125.00 150.00  158
 19  \w     40.00 114.00   0.50    3.00    --  102.08 -61.00 120.00  148
 20  \w    101.00 169.00   0.50    3.00    --  102.08  30.00-120.00  136
 21  \w     34.00 109.00   0.50    3.00    --  102.08 -94.00-120.00  150
 22  \w     39.00 105.00   0.50    3.00    --  102.08 -45.00 120.00  132
 23  \w     36.00 103.00   0.50    3.00    --  102.08 -30.00  30.00  134
 24  \w     94.00 166.00   0.50    3.00    --  102.08 125.00  90.00  144
 25  \w     36.00 103.00   0.50    3.00    --  102.08 -30.00-150.00  134
 26  \w     40.00 114.00   0.50    3.00    --  102.08 -61.00 -60.00  148
 27  \w    100.00 165.00   0.50    3.00    --  102.08  45.00 -90.00  130
 28  \w     34.00 104.00   0.50    3.00    --  102.08 -15.00 150.00  140
 29  \w     34.00 109.00   0.50    3.00    --  102.08 -94.00 -30.00  150
 30  \w    100.00 170.00   0.50    3.00    --  102.08  15.00   0.00  140
 31  \w    -65.00   1.00   0.50    0.75    --    0.00 -37.00-180.00  132
 32  \w    -62.00  22.00   0.50    0.75    --    0.00 -77.00 120.00  168
 33  \w    -22.00  62.00   0.50    0.75    --    0.00  77.00 -60.00  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1376
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31042
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         3.370
_exptl_absorpt_coefficient_mu    4.938
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            greenish
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       prism
_exptl_crystal_F_000             1033
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         4.197
_refine_diff_density_min         -2.009
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         8219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0945
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2425
_refine_ls_wR_factor_ref         0.2454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7722
_reflns_number_total             8219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj03432a2.cif
_cod_data_source_block           as_ism_pdcl2_1r
_cod_depositor_comments
'Adding full bibliography for 7062813--7062814.cif.'
_cod_original_formula_sum        'C54.60 H42.90 Cl2 F5 N3 Pd'
_cod_database_code               7062814
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C23(H23), C13(H13), C28(H28), C9(H9), C8(H8), C18(H18), C19(H19),
 C4(H4), C24(H24), C25(H25), C3(H3), C20(H20), C2(H2), C14(H14), C40(H40),
 C31(H31), C42(H42), C33(H33)
2.b Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C35(H35A,H35B,H35C), C44(H44A,H44B,H44C), C45(H45A,H45B,
 H45C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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
;