Aggregation-induced emission of a bis(imino)acenaphthene zinc complex with tetraphenylethene units.
Fumoto, Takuma; Tanaka, Ryo; Ooyama, Yousuke; Dalton transactions (Cambridge, England : 2003) 52 (2023) 5047–5055; doi:10.1039/d2dt03525a

data_7712344
_publ_section_title
;
 Aggregation-induced emission of a bis(imino)acenaphthene zinc complex
 with tetraphenylethene units.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5047
_journal_page_last               5055
_journal_paper_doi               10.1039/d2dt03525a
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C64 H44 Cl2 N2 Pd, C H2 Cl2'
_chemical_formula_sum            'C65 H46 Cl4 N2 Pd'
_chemical_formula_weight         1103.24
_chemical_name_systematic        'C65 H46 N2 Cl4 Pd1'
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-13
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2022-10-27 deposited with the CCDC.	2023-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                102.491(2)
_cell_angle_beta                 92.7730(10)
_cell_angle_gamma                109.549(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3224(2)
_cell_length_b                   14.5950(3)
_cell_length_c                   19.1625(4)
_cell_measurement_reflns_used    38091
_cell_measurement_temperature    123.04(10)
_cell_measurement_theta_max      29.8360
_cell_measurement_theta_min      1.9100
_cell_volume                     3143.33(12)
_computing_cell_refinement       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.35a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.04(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.871
_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    -85.00 -19.00   0.50    4.00    --  -15.15 137.00 -69.00  132
  2  \w    -81.00 -19.00   0.50    4.00    --  -15.15 132.00 114.00  124
  3  \w     32.00  83.00   0.50    4.00    --   16.55-137.00-131.00  102
  4  \w     37.00  82.00   0.50    4.00    --   16.55-132.00  45.00   90
  5  \w    -45.00  62.00   0.50    4.00    --  -15.15  57.00 -90.00  214
  6  \w    -22.00  66.00   0.50    4.00    --  -15.15  19.00  60.00  176
  7  \w    -22.00  58.00   0.50    4.00    --  -15.15  19.00 120.00  160
  8  \w    -21.00  99.00   0.50    4.00    --   16.55  38.00-180.00  240
  9  \w    -21.00  97.00   0.50    4.00    --   16.55  38.00   0.00  236
 10  \w    -56.00  -2.00   0.50    4.00    --   16.55 -57.00-150.00  108
 11  \w    -21.00  96.00   0.50    4.00    --   16.55  77.00-180.00  234
 12  \w     13.00  46.00   0.50    4.00    --   16.55 -57.00-150.00   66
 13  \w    -22.00  96.00   0.50    4.00    --   16.55  77.00   0.00  236
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0094313000
_diffrn_orient_matrix_UB_12      -0.0475305000
_diffrn_orient_matrix_UB_13      0.0072300000
_diffrn_orient_matrix_UB_21      0.0088549000
_diffrn_orient_matrix_UB_22      0.0223712000
_diffrn_orient_matrix_UB_23      0.0375461000
_diffrn_orient_matrix_UB_31      -0.0602426000
_diffrn_orient_matrix_UB_32      -0.0085320000
_diffrn_orient_matrix_UB_33      -0.0007468000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            71494
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.822
_diffrn_reflns_theta_min         1.884
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.35a (Rigaku Oxford Diffraction, 2021)
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            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.115
_refine_diff_density_max         2.564
_refine_diff_density_min         -1.642
_refine_diff_density_rms         0.100
_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     735
_refine_ls_number_reflns         15712
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+1.2146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13388
_reflns_number_total             15712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03525a5.cif
_cod_data_source_block           exp_1365
_cod_depositor_comments
'Adding full bibliography for 7712343--7712344.cif.'
_cod_original_cell_volume        3143.33(11)
_cod_database_code               7712344
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C65H46N2PdCl4
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.866
_reflns_odcompleteness_completeness 98.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C65 \\sim C47: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C69 \\sim C51: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C68 \\sim C77: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C66 \\sim C48: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C67 \\sim C49: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
3. Others
 Sof(C70)=Sof(H70)=Sof(C71)=Sof(H71)=Sof(C72)=Sof(H72)=Sof(C73)=Sof(H73)=
 Sof(C74)=Sof(H74)=Sof(C75)=1-FVAR(1)
 Sof(C38)=Sof(H38)=Sof(C53)=Sof(C54)=Sof(H54)=Sof(C56)=Sof(H56)=Sof(C57)=
 Sof(H57)=Sof(C58)=Sof(H58)=FVAR(1)
 Sof(C50)=Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=Sof(C77)=
 Sof(H77)=Sof(C51)=Sof(H51)=1-FVAR(2)
 Sof(C46)=Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66)=Sof(C67)=Sof(H67)=Sof(C68)=
 Sof(H68)=Sof(C69)=Sof(H69)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C76(H76A,H76B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36),
 C37(H37), C40(H40), C41(H41), C43(H43), C44(H44), C65(H65), C66(H66), C67(H67),
  C68(H68), C69(H69), C55(H55), C60(H60), C61(H61), C62(H62), C63(H63),
 C64(H64), C38(H38), C54(H54), C56(H56), C57(H57), C58(H58), C70(H70), C71(H71),
  C72(H72), C73(H73), C74(H74), C47(H47), C48(H48), C49(H49), C77(H77), C51(H51)
4.c Fitted hexagon refined as free rotating group:
 C46(C65,C66,C67,C68,C69), C50(C47,C48,C49,C77,C51)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              75912
_shelx_fab_checksum              58394
_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 1.254
_oxdiff_exptl_absorpt_empirical_full_min 0.695