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_7042666
_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 Br4 Hg2 N4 Se, C2 H6 O S'
_chemical_formula_sum            'C34 H36 Br4 Hg2 N4 O S Se'
_chemical_formula_weight         1348.51
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'P 3*'
_space_group_name_H-M_alt        'R 3:r'
_symmetry_space_group_name_Hall  'P 3*'
_symmetry_space_group_name_H-M   'R 3 :R'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1lvgjf
_audit_creation_date             2017-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-04-05 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                116.8770(10)
_cell_angle_beta                 116.8770(10)
_cell_angle_gamma                116.8770(10)
_cell_formula_units_Z            3
_cell_length_a                   19.153(3)
_cell_length_b                   19.153(3)
_cell_length_c                   19.153(3)
_cell_measurement_reflns_used    10506
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.1
_cell_volume                     3158.6(9)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_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      100.0
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.1162
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9631
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         2.751
_exptl_absorpt_coefficient_mu    12.021
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessings, 1995'
_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    2.127
_exptl_crystal_description       block
_exptl_crystal_F_000             1878
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.973
_refine_diff_density_min         -2.309
_refine_diff_density_rms         0.229
_refine_ls_abs_structure_details
;
 Flack x determined using 3676 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.034(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         9631
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0408P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                8862
_reflns_number_total             9631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04505g2.cif
_cod_data_source_block           complex-c1
_cod_original_cell_volume        3158.7(14)
_cod_database_code               7042666
_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 C(H,H,H) groups
2. Restrained distances
 S1-C34B \\sim S1-C34A \\sim S1-C33B \\sim S1-C33A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C33A) = Uanis(C33B) = Uanis(C34A) = Uanis(C34B)
4. Others
 Sof(C33B)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34B)=Sof(H34A)=Sof(H34B)=
 Sof(H34C)=1-FVAR(1)
 Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34A)=Sof(H34D)=Sof(H34E)=
 Sof(H34F)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C15(H15A,H15B), C17(H17A,H17B), C26(H26A,H26B), C18(H18A,
 H18B), C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C11(H11), C10(H10), C24(H24), C21(H21), C12(H12), C22(H22),
 C5(H5), C6(H6), C28(H28), C14(H14), C31(H31), C32(H32), C23(H23), C30(H30),
 C29(H29), C13(H13)
5.c Idealised Me refined as rotating group:
 C33B(H33A,H33B,H33C), C34B(H34A,H34B,H34C), C33A(H33D,H33E,H33F), C34A(H34D,
 H34E,H34F)
;
_olex2_submission_special_instructions 'No special instructions were received'