Synthesis and electropolymerization of N-heterocyclic carbene complexes of Pd(ii) and Pt(ii) from an emissive imidazolium salt with a terthiophene backbone.
Wang, Weiran; Guo, Hongyu; Jones, Richard A.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14440–14449; doi:10.1039/c9dt03363g

data_7701073
_publ_section_title
;
 Synthesis and electropolymerization of N-heterocyclic carbene complexes
 of Pd(ii) and Pt(ii) from an emissive imidazolium salt with a
 terthiophene backbone.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14440
_journal_page_last               14449
_journal_paper_doi               10.1039/c9dt03363g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C15 H13 N2 S3, I'
_chemical_formula_sum            'C15 H13 I N2 S3'
_chemical_formula_weight         444.35
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-14 deposited with the CCDC.    2019-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                73.117(3)
_cell_angle_beta                 73.645(4)
_cell_angle_gamma                87.820(4)
_cell_formula_units_Z            4
_cell_length_a                   10.5465(14)
_cell_length_b                   12.5852(17)
_cell_length_c                   13.9485(18)
_cell_measurement_reflns_used    22028
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      54.94
_cell_measurement_theta_min      4.37
_cell_volume                     1698.0(4)
_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      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724 CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         2.186
_exptl_absorpt_coefficient_mu    2.249
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_description       prism
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.250
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         7766
_refine_ls_number_restraints     244
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+3.6733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1045
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6661
_reflns_number_total             7766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03363g2.cif
_cod_data_source_block           TThIMeHI
_cod_depositor_comments
'Adding full bibliography for 7701073--7701076.cif.'
_cod_database_code               7701073
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.662
_shelx_estimated_absorpt_t_min   0.662
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S6-C24 \\sim S6A-C24
 with sigma of 0.02
 S6-C27 \\sim S6A-C27A
 with sigma of 0.02
 C25-C24 \\sim C25A-C24
 with sigma of 0.02
 C25-C26 \\sim C25A-C26A
 with sigma of 0.02
 C26-C27 \\sim C26A-C27A
 with sigma of 0.02
 S6-C26 \\sim S6A-C26A
 with sigma of 0.04
 C25-C27 \\sim C25A-C27A
 with sigma of 0.04
 C24-C26 \\sim C24-C26A
 with sigma of 0.04
 C24-C27 \\sim C24-C27A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
S6 \\sim C25 \\sim C26 \\sim C27 \\sim S6A \\sim C25A \\sim C26A \\sim C27A
\\sim I1 \\sim I2 \\sim S5 \\sim S2 \\sim S4 \\sim S3 \\sim S1 \\sim N1 \\sim
N2 \\sim N3 \\sim N4 \\sim C21 \\sim C14 \\sim C20 \\sim C5 \\sim C6 \\sim C22
\\sim C7 \\sim C19 \\sim C11 \\sim C23 \\sim C9 \\sim C18 \\sim C8 \\sim C4:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S6) = Uanis(S6A)
Uanis(C25) = Uanis(C25A)
Uanis(C27A) = Uanis(C27)
Uanis(C26) = Uanis(C26A)
4. Same fragment restrains
{S6A, C25A, C26A, C27A} sigma for 1-2: 0.02, 1-3: 0.04
{S6, C25, C26, C27} sigma for 1-2: 0.02, 1-3: 0.04
as
{S6, C25, C26, C27}
5. Others
 Sof(S6A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=1-FVAR(1)
 Sof(S6)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C27(H27), C25A(H25A), C26A(H26A), C27A(H27A), C14(H14),
 C11(H11), C18(H18), C3(H3), C10(H10), C29(H29), C12(H12), C16(H16), C17(H17),
 C1(H1), C2(H2)
6.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C)
;
_shelx_res_checksum              89801
_olex2_submission_special_instructions 'No special instructions were received'