Synthetic access to a phosphorescent non-palindromic pincer complex of palladium by a double oxidative addition - comproportionation sequence.
Feuerstein, Wolfram; Breher, Frank; Chemical communications (Cambridge, England) 56 (2020) 12589–12592; doi:10.1039/d0cc04065g

data_7127123
_publ_section_title
;
 Synthetic access to a phosphorescent non-palindromic pincer complex of
 palladium by a double oxidative addition - comproportionation sequence.
;
_journal_issue                   83
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12589
_journal_page_last               12592
_journal_paper_doi               10.1039/d0cc04065g
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C22 H16 N2 Ni'
_chemical_formula_sum            'C22 H16 N2 Ni'
_chemical_formula_weight         367.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-23
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;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-02-26 deposited with the CCDC.	2020-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.89(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.282(5)
_cell_length_b                   12.710(7)
_cell_length_c                   14.038(7)
_cell_measurement_reflns_used    8014
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.69
_cell_measurement_theta_min      2.16
_cell_volume                     1655.9(15)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
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_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
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_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11940
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.202
_diffrn_reflns_theta_min         2.162
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
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_diffrn_source_voltage           50
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_exptl_absorpt_correction_T_min  0.9228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
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_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0058(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0629P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2876
_reflns_number_total             4459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04065g3.cif
_cod_data_source_block           wf337
_cod_depositor_comments
'Adding full bibliography for 7127122--7127123.cif.'
_cod_database_code               7127123
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C7(H7), C22(H22), C18(H18), C2(H2), C3(H3), C21(H21), C16(H16),
 C20(H20), C19(H19), C4(H4), C9(H9), C8(H8), C15(H15), C13(H13), C14(H14)
;
_shelx_res_checksum              57075
_shelx_hkl_checksum              84782
_olex2_submission_special_instructions 'No special instructions were received'