Selone behavior towards palladium(II) extraction with hydrophobic ionic liquids and mechanism studies
Wang, Chen; tong, yu; Huang, Yixian; Zhang, Hong; Yang, Yanzhao; RSC Adv.  (2015) –; doi:10.1039/C5RA06334E

data_7220984
_publ_section_title
;
 Selone behavior towards palladium(II) extraction with hydrophobic ionic
 liquids and mechanism studies
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA06334E
_journal_year                    2015
_chemical_formula_moiety         'C16 H28 Cl4 N4 Pd2 Se2'
_chemical_formula_sum            'C16 H28 Cl4 N4 Pd2 Se2'
_chemical_formula_weight         788.94
_chemical_name_systematic
bis(1-butyl-3-methyl-imidazole-2-selone)-dichloro-dipalladium
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-01 deposited with the CCDC.
2015-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.285(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6713(4)
_cell_length_b                   15.2764(4)
_cell_length_c                   13.6503(4)
_cell_measurement_reflns_used    325
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      15.03
_cell_measurement_theta_min      2.67
_cell_volume                     2571.60(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1915
_diffrn_reflns_av_unetI/netI     0.2662
_diffrn_reflns_laue_measured_fraction_full 0.970
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11871
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.667
_exptl_absorpt_coefficient_mu    4.656
_exptl_absorpt_correction_T_max  0.7071
_exptl_absorpt_correction_T_min  0.5418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.038
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.127
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         4518
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.2128
_refine_ls_R_factor_gt           0.0743
_refine_ls_shift/su_max          0.899
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1846
_reflns_number_total             4518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra06334e1.cif
_cod_data_source_block           p
_cod_database_code               7220984
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.707
_shelx_estimated_absorpt_t_min   0.542
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H16A,H16B,H16C} of C16, All C(H,H) groups
 At 1.5 times of:
  {H16D,H16E,H16F} of C16A, {H8AA,H8AB,H8AC} of C8A, {H8A,H8B,H8C} of C8,
  {H1A,H1B,H1C} of C1, {H9A,H9B,H9C} of C9
2. Restrained distances
 N2-C6A
 2.35 with sigma of 0.01
 C5A-C7A
 2.35 with sigma of 0.01
 C6A-C8A
 2.35 with sigma of 0.01
 C13A-C15A
 2.35 with sigma of 0.01
 C14A-N4
 2.35 with sigma of 0.01
 C16A-C14A
 2.35 with sigma of 0.01
 C13A-C14A
 1.55 with sigma of 0.01
 C13-C14
 1.55 with sigma of 0.01
 C15A-C14A
 1.55 with sigma of 0.01
 C16A-C15A
 1.55 with sigma of 0.01
 C7-C8
 1.55 with sigma of 0.01
 C8A-C7A
 1.55 with sigma of 0.01
 C15-C13
 2.35 with sigma of 0.01
 C15-C14
 1.55 with sigma of 0.01
 C16-C15
 1.55 with sigma of 0.01
 C16-C14
 2.35 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N2 \\sim C5 \\sim C5A \\sim C6 \\sim C6A \\sim C7 \\sim C7A \\sim C8 \\sim C8A:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.08
N3 \\sim C12: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.08
C13 \\sim C13A \\sim C14 \\sim C14A \\sim C15 \\sim C15A \\sim C16 \\sim C16A:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.08
Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: C5(0.5) H5A(0.5) H5B(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5) C6(0.5)
 H6A(0.5) H6B(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5) C7(0.5) H7A(0.5) H7B(0.5)
 C7A(0.5) H7AA(0.5) H7AB(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C8A(0.5)
 H8AA(0.5) H8AB(0.5) H8AC(0.5) C13(0.5) H13A(0.5) H13B(0.5) C13A(0.5) H13C(0.5)
 H13D(0.5) C14(0.5) H14A(0.5) H14B(0.5) C14A(0.5) H14C(0.5) H14D(0.5) C15(0.5)
 H15A(0.5) H15B(0.5) C15A(0.5) H15C(0.5) H15D(0.5) C16(0.5) H16A(0.5) H16B(0.5)
 H16C(0.5) C16A(0.5) H16D(0.5) H16E(0.5) H16F(0.5)
5.a Riding coordinates:
 C5(H5A,H5B), C5A(H5AA,H5AB), C6(H6A,H6B), C6A(H6AA,H6AB), C7(H7A,H7B),
 C7A(H7AA,H7AB), C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC), C10(H10), C13(H13A,H13B),
  C13A(H13C,H13D), C14(H14A,H14B), C14A(H14C,H14D), C15A(H15C,H15D), C16(H16A,
 H16B,H16C)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C11(H11)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C16A(H16D,H16E,H16F)
;
_olex2_submission_special_instructions 'No special instructions were received'