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_7701075
_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         'C12 H13 I2 N3 Pd S, C H2 Cl2'
_chemical_formula_sum            'C13 H15 Cl2 I2 N3 Pd S'
_chemical_formula_weight         676.44
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-03
_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                90
_cell_angle_beta                 108.871(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.423(2)
_cell_length_b                   7.9595(10)
_cell_length_c                   15.932(2)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.62
_cell_volume                     1970.7(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 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Nonius Kappa CCD diffractometer using a Bruker AXS Apex II detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47017
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.443
_diffrn_reflns_theta_min         2.594
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.451
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0695 before and 0.0503 after correction.
The Ratio of minimum to maximum transmission is 0.7869.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.280
_exptl_crystal_description       prism
_exptl_crystal_F_000             1264
_exptl_crystal_recrystallization_method
'Vapor diffusion of ethyl ether into a sample solution of dichloromethane.'
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         4954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0168
_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^)+(0.0175P)^2^+2.0791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0406
_refine_ls_wR_factor_ref         0.0412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4588
_reflns_number_total             4954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03363g2.cif
_cod_data_source_block           Pd(ThIMe)(pyridine)I2
_cod_depositor_comments
'Adding full bibliography for 7701073--7701076.cif.'
_cod_original_cell_volume        1970.6(4)
_cod_database_code               7701075
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.680
_shelx_estimated_absorpt_t_min   0.508
_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.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C12(H12), C11(H11), C2(H2), C1(H1), C10(H10)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              54181
_olex2_submission_special_instructions 'No special instructions were received'