Helically chiral Pd(ii) complexes containing intramolecular PdPd metallophilicity as circularly polarized molecular phosphors.
Lin, Jinqiang; Xie, Mo; Zhang, Xiaobao; Gao, Qin; Chang, Xiaoyong; Zou, Chao; Lu, Wei; Chemical communications (Cambridge, England) 57 (2021) 1627–1630; doi:10.1039/d0cc08188d

data_7127830
_publ_section_title
;
 Helically chiral Pd(ii) complexes containing intramolecular PdPd
 metallophilicity as circularly polarized molecular phosphors.
;
_journal_issue                   13
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1627
_journal_page_last               1630
_journal_paper_doi               10.1039/d0cc08188d
_journal_volume                  57
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C64 H50 N4 Pd2, 1.24(C H Cl3), 0.76(C4 H10 O)'
_chemical_formula_sum            'C68.22 H58.66 Cl3.78 N4 O0.74 Pd2'
_chemical_formula_weight         1293.13
_space_group_crystal_system      hexagonal
_space_group_IT_number           171
_space_group_name_Hall           'P 62'
_space_group_name_H-M_alt        'P 62'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-14 deposited with the CCDC.	2021-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.5184(11)
_cell_length_b                   20.5184(11)
_cell_length_c                   13.0844(7)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.19
_cell_measurement_theta_min      2.52
_cell_volume                     4770.6(4)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTO 100 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            38611
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.390
_diffrn_reflns_theta_min         2.523
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1418 before and 0.0687 after correction. The Ratio of minimum to maximum transmission is 0.7395. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       block
_exptl_crystal_F_000             1974
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.660
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details
;
 Flack x determined using 2125 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         5835
_refine_ls_number_restraints     1199
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0818
_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^)+(0.1204P)^2^+25.1448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2120
_refine_ls_wR_factor_ref         0.2207
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                5170
_reflns_number_total             5835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc08188d3.cif
_cod_data_source_block           cxy0705_0m
_cod_depositor_comments
'Adding full bibliography for 7127830--7127831.cif.'
_cod_original_cell_volume        4770.6(6)
_cod_database_code               7127830
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C9-C12 = C9A-C12A = C9A-C13A = C9-C13
 1.54 with sigma of 0.02
 C9A-C8A = C9-C8 = C9-C10 = C9A-C10A = C11A-C10A = C11-C10 = C8A-C11A = C8-C11
 = C8-C7 = C8A-C7A
 1.52 with sigma of 0.02
 C7-C5 = C7A-C5A = C4A-C10A = C4-C10
 1.5 with sigma of 0.02
 C15-C14 = C15A-C14A = C14-C1 = C1A-C14A = C16-C15 = C16A-C15A = C17A-C16A =
 C17-C16
 1.39 with sigma of 0.02
 C69-C68 = C67-C66
 1.54 with sigma of 0.02
 O1-C67 = O1-C68
 1.42 with sigma of 0.02
 O1-C66
 2.45 with sigma of 0.04
 O1-C69
 2.45 with sigma of 0.04
 H66A-O1
 2.41 with sigma of 0.01
 H69B-H68A
 2.47 with sigma of 0.01
 Cl2-C65A \\sim Cl3-C65A \\sim Cl1-C65A
 with sigma of 0.02
 Pd1-N1 \\sim Pd1A-N1A
 with sigma of 0.02
 Pd1-N2 \\sim Pd1A-N2A
 with sigma of 0.02
 Pd1-C19 \\sim Pd1A-C19A
 with sigma of 0.02
 Pd1-C24 \\sim Pd1A-C24
 with sigma of 0.02
 N1-C1 \\sim N1A-C1A
 with sigma of 0.02
 N1-C17 \\sim N1A-C17A
 with sigma of 0.02
 N2-C2 \\sim N2A-C2A
 with sigma of 0.02
 N2-C3 \\sim N2A-C3A
 with sigma of 0.02
 C1-C2 \\sim C1A-C2A
 with sigma of 0.02
 C1-C14 \\sim C1A-C14A
 with sigma of 0.02
 C2-C6 \\sim C2A-C6A
 with sigma of 0.02
 C3-C4 \\sim C3A-C4A
 with sigma of 0.02
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 C4-C10 \\sim C4A-C10A
 with sigma of 0.02
 C5-C6 \\sim C5A-C6A
 with sigma of 0.02
 C5-C7 \\sim C5A-C7A
 with sigma of 0.02
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 C8-C9 \\sim C8A-C9A
 with sigma of 0.02
 C8-C11 \\sim C8A-C11A
 with sigma of 0.02
 C9-C10 \\sim C9A-C10A
 with sigma of 0.02
 C9-C12 \\sim C9A-C12A
 with sigma of 0.02
 C9-C13 \\sim C9A-C13A
 with sigma of 0.02
 C10-C11 \\sim C10A-C11A
 with sigma of 0.02
 C14-C15 \\sim C14A-C15A
 with sigma of 0.02
 C15-C16 \\sim C15A-C16A
 with sigma of 0.02
 C16-C17 \\sim C16A-C17A
 with sigma of 0.02
 C17-C18 \\sim C17A-C18A
 with sigma of 0.02
 C18-C19 \\sim C18A-C19A
 with sigma of 0.02
 C18-C23 \\sim C18A-C23A
 with sigma of 0.02
 C19-C20 \\sim C19A-C20A
 with sigma of 0.02
 C20-C21 \\sim C20A-C21A
 with sigma of 0.02
 C21-C22 \\sim C21A-C22A
 with sigma of 0.02
 C22-C23 \\sim C22A-C23A
 with sigma of 0.02
 Pd1-C1 \\sim Pd1A-C1A
 with sigma of 0.04
 Pd1-C2 \\sim Pd1A-C2A
 with sigma of 0.04
 Pd1-C3 \\sim Pd1A-C3A
 with sigma of 0.04
 Pd1-C17 \\sim Pd1A-C17A
 with sigma of 0.04
 Pd1-C18 \\sim Pd1A-C18A
 with sigma of 0.04
 Pd1-C20 \\sim Pd1A-C20A
 with sigma of 0.04
 N1-N2 \\sim N1A-N2A
 with sigma of 0.04
 N1-C2 \\sim N1A-C2A
 with sigma of 0.04
 N1-C14 \\sim N1A-C14A
 with sigma of 0.04
 N1-C16 \\sim N1A-C16A
 with sigma of 0.04
 N1-C18 \\sim N1A-C18A
 with sigma of 0.04
 N1-C19 \\sim N1A-C19A
 with sigma of 0.04
 N1-C24 \\sim N1A-C24
 with sigma of 0.04
 N2-C1 \\sim N2A-C1A
 with sigma of 0.04
 N2-C4 \\sim N2A-C4A
 with sigma of 0.04
 N2-C6 \\sim N2A-C6A
 with sigma of 0.04
 N2-C19 \\sim N2A-C19A
 with sigma of 0.04
 N2-C24 \\sim N2A-C24
 with sigma of 0.04
 C1-C6 \\sim C1A-C6A
 with sigma of 0.04
 C1-C15 \\sim C1A-C15A
 with sigma of 0.04
 C1-C17 \\sim C1A-C17A
 with sigma of 0.04
 C2-C3 \\sim C2A-C3A
 with sigma of 0.04
 C2-C5 \\sim C2A-C5A
 with sigma of 0.04
 C2-C14 \\sim C2A-C14A
 with sigma of 0.04
 C3-C5 \\sim C3A-C5A
 with sigma of 0.04
 C3-C10 \\sim C3A-C10A
 with sigma of 0.04
 C4-C6 \\sim C4A-C6A
 with sigma of 0.04
 C4-C7 \\sim C4A-C7A
 with sigma of 0.04
 C4-C9 \\sim C4A-C9A
 with sigma of 0.04
 C4-C11 \\sim C4A-C11A
 with sigma of 0.04
 C5-C8 \\sim C5A-C8A
 with sigma of 0.04
 C5-C10 \\sim C5A-C10A
 with sigma of 0.04
 C6-C7 \\sim C6A-C7A
 with sigma of 0.04
 C7-C9 \\sim C7A-C9A
 with sigma of 0.04
 C7-C11 \\sim C7A-C11A
 with sigma of 0.04
 C8-C10 \\sim C8A-C10A
 with sigma of 0.04
 C8-C12 \\sim C8A-C12A
 with sigma of 0.04
 C8-C13 \\sim C8A-C13A
 with sigma of 0.04
 C9-C11 \\sim C9A-C11A
 with sigma of 0.04
 C10-C12 \\sim C10A-C12A
 with sigma of 0.04
 C10-C13 \\sim C10A-C13A
 with sigma of 0.04
 C12-C13 \\sim C12A-C13A
 with sigma of 0.04
 C14-C16 \\sim C14A-C16A
 with sigma of 0.04
 C15-C17 \\sim C15A-C17A
 with sigma of 0.04
 C16-C18 \\sim C16A-C18A
 with sigma of 0.04
 C17-C19 \\sim C17A-C19A
 with sigma of 0.04
 C17-C23 \\sim C17A-C23A
 with sigma of 0.04
 C18-C20 \\sim C18A-C20A
 with sigma of 0.04
 C18-C22 \\sim C18A-C22A
 with sigma of 0.04
 C19-C21 \\sim C19A-C21A
 with sigma of 0.04
 C19-C23 \\sim C19A-C23A
 with sigma of 0.04
 C19-C24 \\sim C19A-C24
 with sigma of 0.04
 C20-C22 \\sim C20A-C22A
 with sigma of 0.04
 C21-C23 \\sim C21A-C23A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Pd1) \\sim Ueq, Uanis(Pd1A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C12A) = Uanis(C12)
Uanis(C9A) = Uanis(C9)
Uanis(C13A) = Uanis(C13)
Uanis(C10A) = Uanis(C10)
Uanis(C4A) = Uanis(C4)
Uanis(C5) = Uanis(C5A)
Uanis(C7A) = Uanis(C7)
Uanis(C8) = Uanis(C8A)
Uanis(C11A) = Uanis(C11)
Uanis(C3A) = Uanis(C3)
Uanis(N2) = Uanis(N2A)
Uanis(C2) = Uanis(C2A)
Uanis(C6) = Uanis(C6A)
Uanis(C1) = Uanis(C1A)
Uanis(C14A) = Uanis(C14)
Uanis(C15) = Uanis(C15A)
Uanis(C16A) = Uanis(C16)
Uanis(C17) = Uanis(C17A)
Uanis(N1) = Uanis(N1A)
Uanis(C18A) = Uanis(C18)
Uanis(C23) = Uanis(C23A)
Uanis(C22A) = Uanis(C22)
Uanis(C21) = Uanis(C21A)
Uanis(C20) = Uanis(C20A)
Uanis(C19) = Uanis(C19A)
Uanis(Pd1) = Uanis(Pd1A)
Uanis(O1) = Uanis(C65A)
4. Others
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(O1)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C67)=Sof(H67A)=Sof(H67B)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=Sof(C65A)=Sof(H65A)=FVAR(1)
 Sof(Pd1A)=Sof(N1A)=Sof(N2A)=Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=
 Sof(C5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8A)=
 Sof(C9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14A)=
 Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(C18A)=
 Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=
 Sof(C23A)=Sof(H23A)=1-FVAR(2)
 Sof(Pd1)=Sof(N1)=Sof(N2)=Sof(C1)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(C5)=
 Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(C10)=
 Sof(H10)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=
 Sof(C16)=Sof(H16)=Sof(C17)=Sof(C18)=Sof(C19)=Sof(C20)=Sof(H20)=Sof(C21)=
 Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C10(H10), C65A(H65A), C8A(H8A), C10A(H10A)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C11(H11A,H11B), C7A(H7AA,H7AB), C11A(H11C,H11D), C68(H68A,H68B),
 C67(H67A,H67B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C14(H14), C15(H15), C16(H16), C20(H20), C21(H21), C22(H22),
 C23(H23), C57(H57), C58(H58), C59(H59), C60(H60), C3A(H3A), C6A(H6A),
 C14A(H14A), C15A(H15A), C16A(H16A), C20A(H20A), C21A(H21A), C22A(H22A),
 C23A(H23A)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C12A(H12D,H12E,H12F), C13A(H13D,
 H13E,H13F), C66(H66A,H66B,H66C), C69(H69A,H69B,H69C)
;
_olex2_submission_special_instructions 'No special instructions were received'