Highly phosphorescent organopalladium(ii) complexes with metal-metal-to-ligand charge-transfer excited states in fluid solutions.
Lin, Jinqiang; Zou, Chao; Zhang, Xiaobao; Gao, Qin; Suo, Sa; Zhuo, Qihang; Chang, Xiaoyong; Xie, Mo; Lu, Wei; Dalton transactions (Cambridge, England : 2003) 48 (2019) 10417–10421; doi:10.1039/c9dt02525a

data_7700311
_publ_section_title
;
 Highly phosphorescent organopalladium(ii) complexes with
 metal-metal-to-ligand charge-transfer excited states in fluid solutions.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10417
_journal_page_last               10421
_journal_paper_doi               10.1039/c9dt02525a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C66 H62 N4 Pd2'
_chemical_formula_sum            'C66 H62 N4 Pd2'
_chemical_formula_weight         1123.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-16 deposited with the CCDC.    2019-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                118.321(2)
_cell_angle_beta                 102.924(2)
_cell_angle_gamma                105.600(2)
_cell_formula_units_Z            2
_cell_length_a                   14.9357(9)
_cell_length_b                   15.1568(9)
_cell_length_c                   15.5763(9)
_cell_measurement_reflns_used    9617
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.59
_cell_volume                     2721.1(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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_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 0.997
_diffrn_measured_fraction_theta_max 0.993
_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  0.1049
_diffrn_reflns_av_unetI/netI     0.0971
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46175
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.663
_diffrn_reflns_theta_min         2.146
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  0.0644
_exptl_absorpt_correction_T_min  0.0236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1698 before and 0.1062 after correction. The Ratio of minimum to maximum transmission is 0.3665. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       prism
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.829
_refine_diff_density_min         -1.659
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         12632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0670
_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^)+(0.1010P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9240
_reflns_number_total             12632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02525a2.cif
_cod_data_source_block           cxy0587_0m
_cod_depositor_comments
'Adding full bibliography for 7700308--7700311.cif.'
_cod_database_code               7700311
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C10(H10), C13(H13), C15(H15),
 C16(H16), C29(H29), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37),
  C38(H38), C43(H43), C45(H45), C48(H48), C49(H49), C50(H50), C51(H51),
 C58(H58), C64(H64), C65(H65)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C), C56(H56A,H56B,H56C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C)
;
_olex2_submission_special_instructions 'No special instructions were received'