Heterocyclic-2-thione derivatives of metals incorporating cyclopalladated azobenzenes of variable nuclearity and N,S-bridged 1D polymer of [bis(pyridine-2-thiolato)mercury(ii)]
Lobana, Tarlok S.; Sandhu, Amanpreet K.; Hundal, Geeta; Jasinski, Jerry P.; New Journal of Chemistry 46 (2022) 2722–2729; doi:10.1039/D1NJ05564J

data_7061235
_publ_section_title
;
 Heterocyclic-2-thione derivatives of metals incorporating cyclopalladated
 azobenzenes of variable nuclearity and N,S-bridged 1D polymer of
 [bis(pyridine-2-thiolato)mercury(ii)]
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2722
_journal_page_last               2729
_journal_paper_doi               10.1039/D1NJ05564J
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C62 H58 N12 O2 Pd3 S4, 3(C7 H8)'
_chemical_formula_sum            'C83 H82 N12 O2 Pd3 S4'
_chemical_formula_weight         1727.04
_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             2021-12-23
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2021-12-30 deposited with the CCDC.	2022-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                74.00(3)
_cell_angle_beta                 74.57(3)
_cell_angle_gamma                81.37(3)
_cell_formula_units_Z            1
_cell_length_a                   11.166(2)
_cell_length_b                   13.242(3)
_cell_length_c                   14.462(3)
_cell_measurement_reflns_used    6937
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     1974.6(8)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28845
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.508
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       block
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         6937
_refine_ls_number_restraints     775
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0440P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0845
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5077
_reflns_number_total             6937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05564j2.cif
_cod_data_source_block           GTSL57
_cod_depositor_comments
'Adding full bibliography for 7061231--7061235.cif.'
_cod_database_code               7061235
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.899
_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
 C2_2-C3_2 = C2_2-C7_2 = C4_2-C5_2
 1.39 with sigma of 0.02
 C1_1-C2_1
 1.51 with sigma of 0.02
 C2_1-C3_1 = C2_1-C7_1 = C4_1-C5_1
 1.39 with sigma of 0.02
 C3_1-C4_1 = C5_1-C6_1 = C6_1-C7_1
 1.38 with sigma of 0.02
 C3_2-C4_2 = C5_2-C6_2 = C6_2-C7_2
 1.38 with sigma of 0.02
 C1_2-C2_2
 1.51 with sigma of 0.02
 C3_1-C5_1
 2.39 with sigma of 0.04
 C2_1-C6_1
 2.41 with sigma of 0.04
 C4_1-C6_1 = C5_1-C7_1
 2.4 with sigma of 0.04
 C2_1-C4_1
 2.42 with sigma of 0.04
 C1_1-C3_1 = C1_1-C7_1
 2.52 with sigma of 0.04
 C1_2-C3_2 = C1_2-C7_2
 2.52 with sigma of 0.04
 C2_2-C4_2
 2.42 with sigma of 0.04
 C2_2-C6_2
 2.41 with sigma of 0.04
 C4_2-C6_2 = C5_2-C7_2
 2.4 with sigma of 0.04
 C3_2-C5_2
 2.39 with sigma of 0.04
 C1_1-C7_1 \\sim C1_1-C3_1
 C1_2-C7_2 \\sim C1_2-C3_2
 with sigma of 0.04
 C1_1-C2_1
 C1_2-C2_2
 with sigma of 0.02
 C2_1-C3_1 \\sim C3_1-C4_1 \\sim C4_1-C5_1 \\sim C5_1-C6_1 \\sim C6_1-C7_1
\\sim C7_1-C2_1
 C2_2-C3_2 \\sim C3_2-C4_2 \\sim C4_2-C5_2 \\sim C5_2-C6_2 \\sim C6_2-C7_2
\\sim C7_2-C2_2
 with sigma of 0.02
 C2_1-C6_1 \\sim C2_1-C4_1 \\sim C7_1-C5_1 \\sim C3_1-C7_1 \\sim C4_1-C6_1
\\sim C3_1-C5_1
 C2_2-C6_2 \\sim C2_2-C4_2 \\sim C7_2-C5_2 \\sim C3_2-C7_2 \\sim C4_2-C6_2
\\sim C3_2-C5_2
 with sigma of 0.04
 C11-C12 \\sim C11A-C12A
 with sigma of 0.02
 C12-C13 \\sim C12A-C13A
 with sigma of 0.02
 C9-C10 \\sim C9A-C10A
 with sigma of 0.02
 C11-C13 \\sim C11A-C13A
 with sigma of 0.04
 C8-C10 \\sim C8-C10A
 with sigma of 0.04
 C8-C12 \\sim C8-C12A
 with sigma of 0.04
 C8-C9 \\sim C8-C9A
 with sigma of 0.02
 C8-C13 \\sim C8-C13A
 with sigma of 0.02
 C10-C12 \\sim C10A-C12A
 with sigma of 0.04
 C10-C11 \\sim C10A-C11A
 with sigma of 0.02
 C9-C11 \\sim C9A-C11A
 with sigma of 0.04
 C2-C7 \\sim C2A-C7A
 with sigma of 0.02
 C2-C4 \\sim C2A-C4
 with sigma of 0.04
 C2-C6 \\sim C2A-C6
 with sigma of 0.04
 O1-C2 \\sim O1-C2A
 with sigma of 0.02
 O1-C7 \\sim O1-C7A
 with sigma of 0.04
 C2-C3 \\sim C2A-C3A
 with sigma of 0.02
 O1-C3 \\sim O1-C3A
 with sigma of 0.04
 C3-C4 \\sim C3A-C4
 with sigma of 0.02
 C6-C7 \\sim C6-C7A
 with sigma of 0.02
 C3-C7 \\sim C3A-C7A
 with sigma of 0.04
3. Restrained planarity
 C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1
 C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2
 with sigma of 0.1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1A
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O1A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2A)=Sof(C3A)=
 Sof(H3A)=Sof(H4B)=Sof(C7A)=Sof(H7A)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=1-FVAR(1)
 Sof(O1)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(H4A)=
 Sof(C7)=Sof(H7)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=
 Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=FVAR(1)
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C2(0.5) C3(0.5) H3(0.5) C4(0.5)
 H4(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) C7(0.5) H7(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C24(H24A,H24B), C25(H25A,H25B)
7.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C)
7.c Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3(H3), C3A(H3A), C4(H4B), C4(H4A), C7(H7), C7A(H7A), C9(H9),
 C9A(H9A), C10(H10), C10A(H10A), C11A(H11A), C12(H12), C12A(H12A), C13(H13),
 C13A(H13A), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C26(H26),
 C27(H27), C28(H28), C29(H29), C30(H30), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7),
  C3(H3), C4(H4), C5(H5), C6(H6), C7(H7)
7.d Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7)
7.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              95803
_olex2_submission_special_instructions 'No special instructions were received'