Thermo-responsive emission induced by different delocalized excited-states in isomorphous Pd(ii) and Pt(ii) one-dimensional chains.
Saito, Tomoya; Yoshida, Masaki; Segawa, Kaito; Saito, Daisuke; Takayama, Junichi; Hiura, Satoshi; Murayama, Akihiro; Lakshan, Nishshanka M.; Sameera, W. M. C.; Kobayashi, Atsushi; Kato, Masako; Chemical science 15 (2024) 14497–14505; doi:10.1039/d4sc04497e

data_1572346
_publ_section_title
;
 Thermo-responsive emission induced by different delocalized
 excited-states in isomorphous Pd(ii) and Pt(ii) one-dimensional chains.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              14497
_journal_page_last               14505
_journal_paper_doi               10.1039/d4sc04497e
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C13 H6 F2 K N3 O Pd'
_chemical_formula_sum            'C13 H8 F2 K N3 O Pd'
_chemical_formula_weight         405.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-05-24 deposited with the CCDC.	2024-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.908(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6862(9)
_cell_length_b                   10.2795(5)
_cell_length_c                   6.6908(3)
_cell_measurement_reflns_used    4813
_cell_measurement_temperature    180
_cell_measurement_theta_max      75.0470
_cell_measurement_theta_min      2.2630
_cell_volume                     1349.01(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      180
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_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   -104.00 -79.00   0.50    2.02    --  -42.55-166.00 -27.00   50
  2  \w   -125.00-100.00   0.50    3.82    --  -84.50-166.00 -27.00   50
  3  \w     23.00  48.00   0.50    2.02    --   42.55-115.00 119.00   50
  4  \w     63.00 113.00   0.50    3.82    --  109.88-115.00 119.00  100
  5  \w     82.00 129.00   0.50    3.82    --  109.88-166.00 -27.00   94
  6  \w     37.00 107.00   0.50    3.82    --  109.88 -94.00 -60.00  140
  7  \w     53.00  78.00   0.50    3.82    --  109.88 -45.00 -30.00   50
  8  \w     31.00  56.00   0.50    3.82    --  109.88 -30.00  60.00   50
  9  \w     37.00  63.00   0.50    3.82    --  109.88 -45.00  90.00   52
 10  \w     32.00  61.00   0.50    3.82    --  109.88 -30.00 150.00   58
 11  \w     36.00  64.00   0.50    3.82    --  109.88 -45.00 120.00   56
 12  \w     33.00  65.00   0.50    3.82    --  109.88 -30.00 120.00   64
 13  \w    119.00 178.00   0.50    3.82    --  109.88  30.00  30.00  118
 14  \w     94.00 149.00   0.50    3.82    --  109.88 115.00-151.00  110
 15  \w     72.00 112.00   0.50    2.02    --   42.55 125.00-180.00   80
 16  \w     56.00  81.00   0.50    2.02    --   42.55 166.00  -5.00   50
 17  \w     77.00 114.00   0.50    2.02    --   42.55 125.00  90.00   74
 18  \w     90.00 116.00   0.50    3.82    --  109.88  30.00  30.00   52
 19  \w     22.00 117.00   0.50    2.02    --   42.55  37.00 120.00  190
 20  \w     38.00  87.00   0.50    3.82    --  109.88 -94.00 120.00   98
 21  \w     31.00  56.00   0.50    3.82    --  109.88 -30.00 -90.00   50
 22  \w     31.00  66.00   0.50    3.82    --  109.88 -30.00-180.00   70
 23  \w    -90.00 -21.00   0.50    2.02    --  -42.55 115.00-151.00  138
 24  \w    -85.00 -60.00   0.50    3.82    --  -84.50 115.00-151.00   50
 25  \w    -32.00  -6.00   0.50    3.82    --  -84.50  30.00-180.00   52
 26  \w    -64.00 -12.00   0.50    3.82    --  -84.50  30.00  60.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0149256000
_diffrn_orient_matrix_UB_12      -0.1425864000
_diffrn_orient_matrix_UB_13      0.0513446000
_diffrn_orient_matrix_UB_21      -0.0716853000
_diffrn_orient_matrix_UB_22      0.0395894000
_diffrn_orient_matrix_UB_23      0.0543383000
_diffrn_orient_matrix_UB_31      -0.0284528000
_diffrn_orient_matrix_UB_32      -0.0236344000
_diffrn_orient_matrix_UB_33      -0.2186624000
_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  0.0437
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6890
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.174
_diffrn_reflns_theta_min         4.509
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.112
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.123
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_description       needle
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.414
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.890
_refine_diff_density_min         -1.686
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2435
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0883
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+45.9817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.1976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2267
_reflns_number_total             2435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04497e2.cif
_cod_data_source_block           Pd-dFppy_180K
_cod_depositor_comments
'Adding full bibliography for 1572345--1572356.cif.'
_cod_database_code               1572346
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'K Pd C13 N3 H8 F2 O'
_chemical_oxdiff_usercomment     180K
_shelx_estimated_absorpt_t_max   0.645
_shelx_estimated_absorpt_t_min   0.068
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{N1, C11A}
{C11, N1A}
3. Uiso/Uaniso restraints and constraints
C11A \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim F1A \\sim F2A \\sim C6
\\sim C11 \\sim C10 \\sim C9 \\sim C8 \\sim C7 \\sim F1 \\sim F2: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
Uanis(N1) = Uanis(C11A)
Uanis(C11) = Uanis(N1A)
4. Rigid body (RIGU) restrains
 C11A, C1, C2, C3, C4, C5, F1A, F2A, C6, C11, C10, C9, C8, C7, F1, F2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H1B)=Sof(H7)=Sof(H9)=Sof(H10A)=Sof(F1A)=Sof(F2A)=Sof(N1A)=Sof(C11A)=1-
 FVAR(1)
 Sof(H1A)=Sof(H2)=Sof(H4)=Sof(H10)=Sof(F1)=Sof(F2)=Sof(N1)=Sof(C11)=FVAR(1)
 Sof(K1A)=Sof(O1A)=1-FVAR(2)
 Sof(K1)=Sof(O1)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C1(H1B), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10),
 C10(H10A)
;
_shelx_res_checksum              37599
_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 1.721
_oxdiff_exptl_absorpt_empirical_full_min 0.707