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#$Date: 2016-03-23 20:20:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179408 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/05/4330570.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4330570
loop_
_publ_author_name
'Violeta Sicilia'
'Juan Forniés'
'Sara Fuertes'
'Antonio Martín'
_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            'C15 H8 N3 Pd Tl'
_chemical_formula_weight         541.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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            8
_cell_length_a                   15.1048(3)
_cell_length_b                   24.1782(5)
_cell_length_c                   7.19840(10)
_cell_measurement_reflns_used    7666
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8131
_cell_measurement_theta_min      4.2106
_cell_volume                     2628.91(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10822
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         4.00
_exptl_absorpt_coefficient_mu    13.601
_exptl_absorpt_correction_T_max  0.1204
_exptl_absorpt_correction_T_min  0.0605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.734
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.146
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0327P)²+0.0737P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0504
_reflns_number_gt                2278
_reflns_number_total             2607
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300808z_si_002_1.cif
_cod_data_source_block           3
_cod_database_code               4330570
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pd Pd 0.081975(18) 0.568328(13) 0.36271(4) 0.00844(9) Uani 1 1 d .
Tl Tl 0.066169(10) 0.616921(7) -0.02250(2) 0.01248(7) Uani 1 1 d .
N1 N 0.2873(2) 0.56847(15) 0.3676(4) 0.0154(8) Uani 1 1 d .
N2 N 0.0617(2) 0.45377(17) 0.1432(5) 0.0181(8) Uani 1 1 d .
N3 N -0.0543(2) 0.57659(14) 0.3885(4) 0.0099(7) Uani 1 1 d .
C1 C 0.2111(3) 0.56876(16) 0.3633(5) 0.0111(8) Uani 1 1 d .
C2 C 0.0723(2) 0.49497(18) 0.2196(6) 0.0110(9) Uani 1 1 d .
C3 C -0.1177(3) 0.54209(18) 0.3314(5) 0.0137(9) Uani 1 1 d .
H3 H -0.1015 0.5098 0.2643 0.016 Uiso 1 1 calc R
C4 C -0.2073(2) 0.55198(18) 0.3672(5) 0.0142(9) Uani 1 1 d .
H4 H -0.2508 0.5263 0.3265 0.017 Uiso 1 1 calc R
C5 C -0.2321(3) 0.59860(18) 0.4607(5) 0.0124(9) Uani 1 1 d .
H5 H -0.2930 0.6062 0.4821 0.015 Uiso 1 1 calc R
C6 C -0.1666(3) 0.63516(18) 0.5248(5) 0.0110(9) Uani 1 1 d .
C7 C -0.1850(3) 0.68457(17) 0.6311(5) 0.0140(9) Uani 1 1 d .
H7 H -0.2446 0.6941 0.6588 0.017 Uiso 1 1 calc R
C8 C -0.1180(3) 0.71756(17) 0.6919(5) 0.0137(9) Uani 1 1 d .
H8 H -0.1319 0.7495 0.7629 0.016 Uiso 1 1 calc R
C9 C -0.0274(3) 0.70535(17) 0.6517(5) 0.0114(8) Uani 1 1 d .
C10 C 0.0435(3) 0.73867(18) 0.7093(5) 0.0146(9) Uani 1 1 d .
H10 H 0.0324 0.7716 0.7773 0.018 Uiso 1 1 calc R
C11 C 0.1294(3) 0.72369(17) 0.6674(5) 0.0163(9) Uani 1 1 d .
H11 H 0.1769 0.7467 0.7062 0.020 Uiso 1 1 calc R
C12 C 0.1479(3) 0.67493(17) 0.5682(5) 0.0143(9) Uani 1 1 d .
H12 H 0.2077 0.6654 0.5429 0.017 Uiso 1 1 calc R
C13 C 0.0806(3) 0.64033(18) 0.5063(5) 0.0107(9) Uani 1 1 d .
C14 C -0.0078(3) 0.65681(16) 0.5503(5) 0.0100(8) Uani 1 1 d .
C15 C -0.0779(3) 0.62242(18) 0.4863(5) 0.0106(9) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 Pd C13 90.26(17) . .
C1 Pd C2 94.42(15) . .
C13 Pd C2 175.29(15) . .
C1 Pd N3 172.13(15) . .
C13 Pd N3 82.03(15) . .
C2 Pd N3 93.27(14) . .
C1 Pd Tl 94.54(11) . .
C13 Pd Tl 97.66(11) . .
C2 Pd Tl 82.54(11) . .
N3 Pd Tl 88.08(9) . .
N1 Tl N2 102.80(11) 8_655 5_565
N1 Tl Pd 92.09(7) 8_655 .
N2 Tl Pd 96.02(8) 5_565 .
C1 N1 Tl 148.0(3) . 8_656
C2 N2 Tl 142.7(3) . 5_565
C3 N3 C15 118.7(4) . .
C3 N3 Pd 128.6(3) . .
C15 N3 Pd 112.6(3) . .
N1 C1 Pd 178.5(4) . .
N2 C2 Pd 175.9(3) . .
N3 C3 C4 122.1(4) . .
C5 C4 C3 119.9(4) . .
C4 C5 C6 119.2(4) . .
C15 C6 C5 118.0(4) . .
C15 C6 C7 118.0(4) . .
C5 C6 C7 123.9(4) . .
C8 C7 C6 120.8(4) . .
C7 C8 C9 121.7(4) . .
C10 C9 C14 118.0(4) . .
C10 C9 C8 123.6(4) . .
C14 C9 C8 118.5(4) . .
C11 C10 C9 120.2(4) . .
C10 C11 C12 121.2(4) . .
C13 C12 C11 121.5(4) . .
C12 C13 C14 116.4(4) . .
C12 C13 Pd 132.4(3) . .
C14 C13 Pd 111.2(3) . .
C9 C14 C15 119.8(4) . .
C9 C14 C13 122.8(4) . .
C15 C14 C13 117.4(4) . .
N3 C15 C6 122.1(4) . .
N3 C15 C14 116.6(4) . .
C6 C15 C14 121.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd C1 1.951(4) .
Pd C13 2.025(4) .
Pd C2 2.056(4) .
Pd N3 2.076(3) .
Pd Tl 3.0210(3) .
Tl N1 2.626(3) 8_655
Tl N2 2.721(4) 5_565
N1 C1 1.152(5) .
N1 Tl 2.626(3) 8_656
N2 C2 1.149(6) .
N2 Tl 2.721(4) 5_565
N3 C3 1.336(5) .
N3 C15 1.360(5) .
C3 C4 1.398(5) .
C4 C5 1.365(6) .
C5 C6 1.405(6) .
C6 C15 1.403(6) .
C6 C7 1.446(6) .
C7 C8 1.360(6) .
C8 C9 1.431(6) .
C9 C10 1.403(6) .
C9 C14 1.413(5) .
C10 C11 1.380(6) .
C11 C12 1.406(6) .
C12 C13 1.389(6) .
C13 C14 1.429(5) .
C14 C15 1.423(6) .
