A bis(PCN) palladium pincer complex with a remarkably planar 2,5-diarylpyrazine core.
Leong, Derek W.; Shao, Yanwu; Ni, Zhen; Bhuvanesh, Nattamai; Ozerov, Oleg V.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6520–6523; doi:10.1039/d3dt04248k

data_7715559
_publ_section_title
;
 A bis(PCN) palladium pincer complex with a remarkably planar
 2,5-diarylpyrazine core.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6520
_journal_page_last               6523
_journal_paper_doi               10.1039/d3dt04248k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C28 H36 Cl2 N2 O2 P2 Pd2, 2(C4 H8 O)'
_chemical_formula_sum            'C36 H52 Cl2 N2 O4 P2 Pd2'
_chemical_formula_weight         922.43
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-20 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                102.1850(10)
_cell_angle_beta                 92.1130(10)
_cell_angle_gamma                92.8890(10)
_cell_formula_units_Z            1
_cell_length_a                   7.7920(2)
_cell_length_b                   10.0383(3)
_cell_length_c                   12.4545(4)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      70.022
_cell_measurement_theta_min      3.635
_cell_volume                     949.89(5)
_computing_cell_refinement
'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.'
_computing_data_reduction
'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.'
_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      110.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10512
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.017
_diffrn_reflns_theta_min         3.635
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.051
_exptl_absorpt_correction_T_max  0.3841
_exptl_absorpt_correction_T_min  0.1885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0929 before and 0.0408 after correction. The Ratio of minimum to maximum transmission is 0.4908. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       block
_exptl_crystal_F_000             470
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         3577
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0175
_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^)+(0.0146P)^2^+0.6197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3497
_reflns_number_total             3577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04248k2.cif
_cod_data_source_block           yws438
_cod_depositor_comments          'Adding full bibliography for 7715559.cif.'
_cod_database_code               7715559
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.327
_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
 C15-C16 \\sim C16-C17 \\sim C17-C18
 with sigma of 0.02
 O2-C15 \\sim O2-C18
 with sigma of 0.02
 O2-C16 \\sim O2-C17
 with sigma of 0.02
 C16-C18 \\sim C15-C17
 with sigma of 0.02
3. Rigid bond restraints
 O2, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2A, C15A, C16A, C17A, C18A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O2 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
O2A \\sim C15A \\sim C16A \\sim C17A \\sim C18A: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04
Uanis(O2) = Uanis(O2A)
5. Same fragment restrains
{O2, C15, C16, C17, C18} sigma for 1-2: 0.01, 1-3: 0.04
as
{O2A, C15A, C16A, C17A, C18A}
6. Others
 Sof(O2A)=Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(C16A)=Sof(H16C)=Sof(H16D)=
 Sof(C17A)=Sof(H17C)=Sof(H17D)=Sof(C18A)=Sof(H18C)=Sof(H18D)=1-FVAR(1)
 Sof(O2)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C17)=
 Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12)
7.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C15A(H15C,
 H15D), C16A(H16C,H16D), C17A(H17C,H17D), C18A(H18C,H18D)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8)
7.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C)
;
_shelx_res_checksum              79824
_olex2_submission_special_instructions 'No special instructions were received'