Aggregation of phosphorescent Pd(II) and Pt(II) complexes with lipophilic counter-anions in non-polar solvents.
Zhou, Ning; Zou, Chao; Suo, Sa; Liu, Yuliang; Lin, Jinqiang; Zhang, Xiaobao; Shi, Minglin; Chang, Xiaoyong; Lu, Wei; Dalton transactions (Cambridge, England : 2003) 52 (2023) 5503–5513; doi:10.1039/d2dt03415h

data_7712700
_publ_section_title
;
 Aggregation of phosphorescent Pd(II) and Pt(II) complexes with lipophilic
 counter-anions in non-polar solvents.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5503
_journal_page_last               5513
_journal_paper_doi               10.1039/d2dt03415h
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C42 H77 O6 S, C24 H21 N4 O Pd, C H2 Cl2'
_chemical_formula_sum            'C67 H100 Cl2 N4 O7 Pd S'
_chemical_formula_weight         1282.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-10-20 deposited with the CCDC.	2023-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.4740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3719(2)
_cell_length_b                   58.8373(16)
_cell_length_c                   13.8630(4)
_cell_measurement_reflns_used    9828
_cell_measurement_temperature    200
_cell_measurement_theta_max      68.36
_cell_measurement_theta_min      3.00
_cell_volume                     6828.4(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'Bruker PHOTO 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'BrukerD8 venture microsource'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       70
_diffrn_reflns_limit_k_min       -70
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            82855
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.357
_diffrn_reflns_theta_min         3.004
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.606
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1130 before and 0.0608 after correction. The Ratio of minimum to maximum transmission is 0.6240. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       block
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.855
_refine_diff_density_min         -1.298
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.480(7)
_refine_ls_extinction_coef       0.00043(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1491
_refine_ls_number_reflns         24494
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+12.4340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1140
_reflns_Friedel_coverage         0.964
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                23728
_reflns_number_total             24494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03415h2.cif
_cod_data_source_block           cxy0833_0m
_cod_depositor_comments
'Adding full bibliography for 7712699--7712700.cif.'
_cod_database_code               7712700
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.357
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.520(8)
 0.480(8)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C79(H79A,H79B), C54(H54A,H54B), C66(H66A,H66B), C75(H75A,H75B), C67(H67A,
 H67B), C80(H80A,H80B), C83(H83A,H83B), C53(H53A,H53B), C81(H81A,H81B),
 C71(H71A,H71B), C73(H73A,H73B), C69(H69A,H69B), C68(H68A,H68B), C55(H55A,H55B),
  C62(H62A,H62B), C58(H58A,H58B), C60(H60A,H60B), C56(H56A,H56B), C72(H72A,
 H72B), C57(H57A,H57B), C59(H59A,H59B), C61(H61A,H61B), C70(H70A,H70B),
 C85(H85A,H85B), C84(H84A,H84B), C74(H74A,H74B), C88(H88A,H88B), C82(H82A,H82B),
  C76(H76A,H76B), C86(H86A,H86B), C63(H63A,H63B), C87(H87A,H87B), C89(H89A,
 H89B), C95(H95A,H95B), C96(H96A,H96B), C108(H10A,H10B), C121(H12A,H12B),
 C99(H99A,H99B), C122(H12C,H12D), C124(H12E,H12F), C109(H10C,H10D), C123(H12G,
 H12H), C110(H11A,H11B), C98(H98A,H98B), C112(H11C,H11D), C125(H12I,H12J),
 C101(H10E,H10F), C97(H97A,H97B), C126(H12K,H12L), C116(H11E,H11F), C114(H11G,
 H11H), C115(H11I,H11J), C103(H10G,H10H), C127(H12M,H12N), C117(H11K,H11L),
 C105(H10I,H10J), C102(H10K,H10L), C100(H10M,H10N), C111(H11M,H11N), C129(H12O,
 H12P), C128(H12Q,H12R), C118(H11O,H11P), C104(H10O,H10P), C130(H13A,H13B),
 C113(H11Q,H11R), C131(H13C,H13D), C49(H49A,H49B), C50(H50A,H50B)
3.b Aromatic/amide H refined with riding coordinates:
 C91(H91), C92(H92), C133(H133), C134(H134), C37(H37), C45(H45), C30(H30),
 C27(H27), C46(H46), C28(H28), C40(H40), C33(H33), C31(H31), C41(H41), C29(H29),
  C32(H32), C17(H17), C16(H16), C9(H9), C8(H8), C7(H7), C6(H6), C3(H3),
 C22(H22), C5(H5), C21(H21), C4(H4), C13(H13)
3.c Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C77(H77A,H77B,H77C), C90(H90A,H90B,H90C), C119(H11S,H11T,
 H11U), C106(H10Q,H10R,H10S), C132(H13E,H13F,H13G), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C39(H39A,H39B,H39C), C23(H23A,H23B,H23C), C15(H15A,H15B,
 H15C), C24(H24A,H24B,H24C)
;
_olex2_submission_special_instructions 'No special instructions were received'