Fluorescent perylenylpyridine complexes: an experimental and theoretical study.
Expósito, J Emilio; Aullón, Gabriel; Bardají, Manuel; Miguel, Jesús A; Espinet, Pablo; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13326–13338; doi:10.1039/d0dt02494e

data_7705301
_publ_section_title
;
 Fluorescent perylenylpyridine complexes: an experimental and theoretical
 study.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13326
_journal_page_last               13338
_journal_paper_doi               10.1039/d0dt02494e
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C28 H19 N O Pd S2'
_chemical_formula_sum            'C28 H19 N O Pd S2'
_chemical_formula_weight         555.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-10 deposited with the CCDC.	2020-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8850(4)
_cell_length_b                   15.3326(3)
_cell_length_c                   7.25084(18)
_cell_measurement_reflns_used    3715
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2776
_cell_measurement_theta_min      2.4366
_cell_volume                     2210.70(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4757
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_details
;
  1 omega  -15.00   58.00   1.0000    5.0900
omega____ theta____ kappa____ phi______ frames
    -       12.4346    0.0000  -60.0000 73

  2 omega    9.00   36.00   1.0000    5.0900
omega____ theta____ kappa____ phi______ frames
    -       12.4346 -123.0000   20.0000 27

  3 omega  -71.00  -25.00   1.0000    5.0900
omega____ theta____ kappa____ phi______ frames
    -       12.4346    0.0000  -60.0000 46
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0172633000
_diffrn_orient_matrix_UB_12      -0.0285468000
_diffrn_orient_matrix_UB_13      -0.0606680000
_diffrn_orient_matrix_UB_21      0.0310395000
_diffrn_orient_matrix_UB_22      0.0122425000
_diffrn_orient_matrix_UB_23      0.0407112000
_diffrn_orient_matrix_UB_31      -0.0032749000
_diffrn_orient_matrix_UB_32      -0.0342552000
_diffrn_orient_matrix_UB_33      0.0651209000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8215
_diffrn_reflns_point_group_measured_fraction_full 0.757
_diffrn_reflns_point_group_measured_fraction_max 0.624
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.342
_diffrn_reflns_theta_min         2.441
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.2969
_exptl_crystal_size_mid          0.2528
_exptl_crystal_size_min          0.1921
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.23(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         3776
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0283P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.345
_reflns_Friedel_fraction_full    0.470
_reflns_Friedel_fraction_max     0.346
_reflns_number_gt                3205
_reflns_number_total             3776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02494e2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7705296--7705301.cif.'
_cod_database_code               7705301
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C28 H19 N O S2 Pd'
_chemical_oxdiff_usercomment     THF/hexano
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.77(4)
 0.23(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C8(H8), C9(H9), C20(H20), C19(H19), C18(H18), C16(H16),
 C15(H15), C14(H14), C22(H22), C24(H24), C25(H25)
3.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              57436
_olex2_submission_special_instructions 'No special instructions were received'