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_7042668
_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 H32 N4 Se, 0.51(H2 O), Br H0.98 O0.49, Br'
_chemical_formula_sum            'C32 H34 Br2 N4 O Se'
_chemical_formula_weight         729.41
_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   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc1lvgd9
_audit_creation_date             2017-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-03-23 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                96.350(5)
_cell_angle_beta                 99.617(5)
_cell_angle_gamma                99.243(5)
_cell_formula_units_Z            2
_cell_length_a                   11.4917(13)
_cell_length_b                   11.5144(12)
_cell_length_c                   12.3760(14)
_cell_measurement_reflns_used    5935
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.64
_cell_volume                     1577.6(3)
_computing_cell_refinement       'Bruker APEX-II'
_computing_data_collection       'Bruker APEX-II'
_computing_data_reduction        'Bruker APEX-II'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  ccdc_depositL2Br
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11391
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.293
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.754
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Bruker,2008)'
_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    1.535
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         5471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0657P)^2^+2.7256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4829
_reflns_number_total             5471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04505g2.cif
_cod_data_source_block           l2br
_cod_database_code               7042668
_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
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Br2B) = Uanis(Br31) = Uanis(Br21)
3. Others
 Sof(O1B)=Sof(H1BA)=Sof(H1BB)=1-FVAR(1)
 Sof(O1A)=Sof(H2B)=Sof(H1AA)=FVAR(1)
 Fixed Sof: Br1(0.1) Br2(0.05) Br2A(0.5) Br2B(0.25) Br3(0.05) Br21(0.02)
 Br31(0.03)
4.a Free rotating group:
 O1B(H1BA,H1BB), O1A(H2B,H1AA)
4.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C26(H26A,H26B), C16(H16A,H16B), C15(H15A,
 H15B), C1(H1A,H1B)
4.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C25(H25), C24(H24), C23(H23), C22(H22), C32(H32), C31(H31),
 C29(H29), C28(H28), C19(H19), C8(H8), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7),
 C13(H13), C12(H12), C11(H11), C10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'