Hg(II) and Pd(II) complexes with a new selenoether bridged biscarbene ligand: Efficient mono- and bis-arylation of methyl acrylate with a pincer biscarbene Pd(II) precatalyst
Dhiman, Rishu; Prashanth, Billa; Bawari, Deependra; Mandal, Ushnish; Verma, Aditya; Roychoudhury, Angshuman; Singh, Sanjay; Dalton Trans.  (2017) –; doi:10.1039/C6DT04505G

data_7042670
_publ_section_title
;
 Hg(II) and Pd(II) complexes with a new selenoether bridged biscarbene
 ligand: Efficient mono- and bis-arylation of methyl acrylate with a
 pincer biscarbene Pd(II) precatalyst
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C6DT04505G
_journal_year                    2017
_chemical_formula_moiety         'C32 H30 Br2 N4 Pd Se'
_chemical_formula_sum            'C32 H30 Br2 N4 Pd Se'
_chemical_formula_weight         815.78
_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
_audit_block_doi                 10.5517/ccdc.csd.cc1lvghd
_audit_creation_date             2017-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-23 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                75.555(7)
_cell_angle_beta                 69.682(7)
_cell_angle_gamma                64.940(7)
_cell_formula_units_Z            2
_cell_length_a                   11.8235(15)
_cell_length_b                   11.8672(14)
_cell_length_c                   12.6937(15)
_cell_measurement_reflns_used    4996
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.88
_cell_measurement_theta_min      2.18
_cell_volume                     1502.0(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX 2 (Bruker, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18842
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.723
_exptl_absorpt_coefficient_mu    4.519
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
        wR2(int) was 0.1045 before and 0.0638 after correction.
        The Ratio of minimum to maximum transmission is 0.8243. The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.442
_refine_diff_density_min         -1.614
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0701P)^2^+2.3667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4097
_reflns_number_total             5504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04505g2.cif
_cod_data_source_block           complexc3
_cod_database_code               7042670
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
 C26(H26A,H26B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C11(H11), C10(H10), C4(H4), C5(H5), C6(H6), C7(H7),
 C8(H8), C32(H32), C31(H31), C30(H30), C29(H29), C28(H28), C22(H22), C23(H23),
 C24(H24), C25(H25)
;
_olex2_submission_special_instructions 'No special instructions were received'