Palladium(ii) N-heterocyclic allenylidene complexes with extended intercationic PdPd interactions and MMLCT phosphorescence.
Zou, Chao; Lin, Jinqiang; Suo, Sa; Xie, Mo; Chang, Xiaoyong; Lu, Wei; Chemical communications (Cambridge, England) 54 (2018) 5319–5322; doi:10.1039/c8cc01652f

data_7121566
_publ_section_title
;
 Palladium(ii) N-heterocyclic allenylidene complexes with extended
 intercationic PdPd interactions and MMLCT phosphorescence.
;
_journal_issue                   42
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5319
_journal_page_last               5322
_journal_paper_doi               10.1039/c8cc01652f
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C23 H19 N4 Pd, 2(F3 P0.5), C3 H7 N O'
_chemical_formula_sum            'C26 H26 F6 N5 O P Pd'
_chemical_formula_weight         675.89
_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             2017-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-25 deposited with the CCDC.
2018-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                109.005(3)
_cell_angle_beta                 99.386(3)
_cell_angle_gamma                92.908(4)
_cell_formula_units_Z            2
_cell_length_a                   6.5861(5)
_cell_length_b                   12.6581(10)
_cell_length_c                   17.1310(14)
_cell_measurement_reflns_used    4494
_cell_measurement_temperature    100
_cell_measurement_theta_max      65.236
_cell_measurement_theta_min      2.779
_cell_volume                     1323.96(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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
_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 0.971
_diffrn_measured_fraction_theta_max 0.971
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4324
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        65.356
_diffrn_reflns_theta_max         65.356
_diffrn_reflns_theta_min         2.779
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.887
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1379 before and 0.0816 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1293 before and 0.0798 after correction.
 The Ratio of minimum to maximum transmission is 0.51.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 20596 reflections, Rint = 0.0834
 (14272 with I > 3sig(I), Rint = 0.0776)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       needle
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.550
_refine_diff_density_min         -1.439
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4324
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.0999
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2463
_refine_ls_wR_factor_ref         0.2670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3376
_reflns_number_total             4324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01652f2.cif
_cod_data_source_block           cu_cxy0207_0m_4
_cod_depositor_comments
'Adding full bibliography for 7121566--7121567.cif.'
_cod_database_code               7121566
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.820
_shelx_estimated_absorpt_t_min   0.217
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.393(5)
 0.607(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N5-C26 = N5-C25
 1.45 with sigma of 0.02
 N5-C24
 1.45 with sigma of 0.02
 O1-C24
 1.25 with sigma of 0.02
 H26B-C24
 2.46 with sigma of 0.02
 C24-C25 \\sim C24-C26
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14),
 C15(H15), C16(H16), C20(H20), C21(H21), C24(H24)
5.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C)
;
_shelx_res_checksum              42647
_olex2_submission_special_instructions 'No special instructions were received'