New Dicyano Cyclometalated Compounds Containing Pd(II)-Tl(I) Bonds as Building Blocks in 2D Extended Structures: Synthesis, Structure, and Luminescence Studies
Violeta Sicilia; Juan Forniés; Sara Fuertes; Antonio Martín; Inorganic Chemistry 51 (2012) 10581–10589; doi:10.1021/ic300808z

data_4330571
_publ_section_title
;
 New Dicyano Cyclometalated Compounds Containing Pd(II)-Tl(I) Bonds as
 Building Blocks in 2D Extended Structures: Synthesis, Structure, and
 Luminescence Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10581
_journal_page_last               10589
_journal_paper_doi               10.1021/ic300808z
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C13 H8 N3 Pd Tl'
_chemical_formula_weight         516.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.9007(3)
_cell_length_b                   9.0620(3)
_cell_length_c                   23.4580(8)
_cell_measurement_reflns_used    20812
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.3222
_cell_measurement_theta_min      4.8747
_cell_volume                     1254.35(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8583
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         4.14
_exptl_absorpt_coefficient_mu    14.246
_exptl_absorpt_correction_T_max  0.1727
_exptl_absorpt_correction_T_min  0.0824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction,
Version 1.171.27p8 beta (release 03-06-2005 CrysAlis171 .NET)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.738
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.595
_refine_diff_density_min         -1.613
_refine_diff_density_rms         0.220
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.096(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2683
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+25.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                2668
_reflns_number_total             2683
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300808z_si_002_2.cif
_cod_data_source_block           4
_cod_database_code               4330571