#------------------------------------------------------------------------------
#$Date: 2019-11-23 13:25:53 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233442 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/88/4348865.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_4348865
loop_
_publ_author_name
'Echeverría, Raquel'
'López-de-Luzuriaga, José M'
'Monge, Miguel'
'Moreno, Sonia'
'Olmos, M. Elena'
_publ_section_title
;
 New Insights into the Au(I)···Pb(II) Closed-Shell
 Interaction: Tuning of the Emissive Properties with the Intermetallic
 Distance.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10523
_journal_page_last               10534
_journal_paper_doi               10.1021/acs.inorgchem.6b01749
_journal_volume                  55
_journal_year                    2016
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C21 H10 Au1 B1 F10 N6 Pb1'
_chemical_formula_sum            'C21 H10 Au B F10 N6 Pb'
_chemical_formula_weight         951.32
_chemical_name_common            dpg47re226
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2014-12-03T11:08:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.140(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7334(2)
_cell_length_b                   22.8741(9)
_cell_length_c                   13.6999(5)
_cell_measurement_reflns_used    2659
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.32
_cell_measurement_wavelength     0.71073
_cell_volume                     2419.80(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.112407
_diffrn_orient_matrix_UB_12      -0.136863E-1
_diffrn_orient_matrix_UB_13      0.246615E-1
_diffrn_orient_matrix_UB_21      0.45409E-2
_diffrn_orient_matrix_UB_22      -0.355404E-1
_diffrn_orient_matrix_UB_23      -0.422883E-1
_diffrn_orient_matrix_UB_31      0.06415
_diffrn_orient_matrix_UB_32      -0.21466E-1
_diffrn_orient_matrix_UB_33      0.542914E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_unetI/netI     0.059
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35327
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.32
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    13.106
_exptl_absorpt_correction_T_max  0.3671
_exptl_absorpt_correction_T_min  0.2659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.518
_refine_diff_density_min         -1.588
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.065
_refine_ls_R_factor_gt           0.037
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0442P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                4051
_reflns_number_total             5509
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic6b01749_si_003.cif
_cod_data_source_block           dpg47re226
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C21 H10 Au1 B1 F10 N6 Pb1'
_cod_database_code               4348865
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
Au1 Au -0.21167(4) 0.023029(12) 0.49563(2) 0.02780(9) Uani 1 1 d .
Pb1 Pb 0.06552(3) 0.130669(11) 0.527304(19) 0.02323(9) Uani 1 1 d .
C1 C -0.2111(9) 0.0056(3) 0.6415(5) 0.0282(16) Uani 1 1 d .
C2 C -0.2770(9) -0.0471(3) 0.6728(6) 0.0300(17) Uani 1 1 d .
C3 C -0.2732(10) -0.0651(3) 0.7675(6) 0.0339(18) Uani 1 1 d .
C4 C -0.2005(11) -0.0305(3) 0.8399(6) 0.039(2) Uani 1 1 d .
C5 C -0.1343(10) 0.0237(3) 0.8150(6) 0.0350(18) Uani 1 1 d .
C6 C -0.1447(9) 0.0392(3) 0.7197(6) 0.0318(17) Uani 1 1 d .
C7 C -0.2354(9) 0.0314(3) 0.3469(5) 0.0274(16) Uani 1 1 d .
C8 C -0.3232(9) -0.0119(3) 0.2919(6) 0.0287(16) Uani 1 1 d .
C9 C -0.3550(9) -0.0097(3) 0.1915(6) 0.0340(19) Uani 1 1 d .
C10 C -0.2966(10) 0.0376(3) 0.1414(6) 0.0350(18) Uani 1 1 d .
C11 C -0.2039(9) 0.0804(3) 0.1903(6) 0.0316(17) Uani 1 1 d .
C12 C -0.1793(9) 0.0763(3) 0.2901(5) 0.0283(16) Uani 1 1 d .
C13 C 0.2431(9) 0.1841(3) 0.7459(5) 0.0323(17) Uani 1 1 d .
H13 H 0.2918 0.1485 0.7657 0.039 Uiso 1 1 calc R
C14 C 0.2463(10) 0.2339(3) 0.8022(5) 0.0359(19) Uani 1 1 d .
H14 H 0.2948 0.2383 0.8654 0.043 Uiso 1 1 calc R
C15 C 0.1629(9) 0.2754(3) 0.7456(5) 0.0306(17) Uani 1 1 d .
H15 H 0.1442 0.314 0.7637 0.037 Uiso 1 1 calc R
C16 C 0.2234(9) 0.2265(3) 0.3576(5) 0.0315(17) Uani 1 1 d .
H16 H 0.2603 0.1973 0.3164 0.038 Uiso 1 1 calc R
C17 C 0.2471(10) 0.2856(3) 0.3424(6) 0.0387(19) Uani 1 1 d .
H17 H 0.301 0.3032 0.291 0.046 Uiso 1 1 calc R
C18 C 0.1740(9) 0.3125(3) 0.4192(5) 0.0303(17) Uani 1 1 d .
H18 H 0.1692 0.3527 0.4296 0.036 Uiso 1 1 calc R
C19 C -0.3499(9) 0.1781(3) 0.5403(5) 0.0332(18) Uani 1 1 d .
H19 H -0.3965 0.141 0.53 0.04 Uiso 1 1 calc R
C20 C -0.4456(9) 0.2274(4) 0.5552(6) 0.0372(19) Uani 1 1 d .
H20 H -0.5653 0.2304 0.5571 0.045 Uiso 1 1 calc R
C21 C -0.3260(9) 0.2711(3) 0.5666(5) 0.0314(17) Uani 1 1 d .
H21 H -0.3515 0.3102 0.5778 0.038 Uiso 1 1 calc R
B1 B 0.0119(10) 0.2794(4) 0.5713(6) 0.0256(18) Uani 1 1 d .
H1 H -0.0037 0.3213 0.5834 0.031 Uiso 1 1 calc R
F1 F -0.3486(5) -0.08543(18) 0.6060(3) 0.0404(11) Uani 1 1 d .
F2 F -0.3382(7) -0.11776(19) 0.7924(4) 0.0556(14) Uani 1 1 d .
F3 F -0.1903(7) -0.0489(2) 0.9339(3) 0.0602(14) Uani 1 1 d .
F4 F -0.0638(6) 0.0588(2) 0.8854(3) 0.0544(13) Uani 1 1 d .
F5 F -0.0756(6) 0.09299(18) 0.7008(3) 0.0446(12) Uani 1 1 d .
F6 F -0.3849(5) -0.05923(18) 0.3390(3) 0.0407(11) Uani 1 1 d .
F7 F -0.4443(6) -0.0526(2) 0.1448(3) 0.0481(12) Uani 1 1 d .
F8 F -0.3281(6) 0.0414(2) 0.0435(3) 0.0494(12) Uani 1 1 d .
F9 F -0.1384(6) 0.12508(18) 0.1393(3) 0.0436(11) Uani 1 1 d .
F10 F -0.0857(6) 0.12156(18) 0.3335(3) 0.0381(11) Uani 1 1 d .
N1 N 0.1609(7) 0.1934(2) 0.6590(4) 0.0267(13) Uani 1 1 d .
N2 N 0.1125(7) 0.2511(2) 0.6593(4) 0.0225(12) Uani 1 1 d .
N3 N 0.1400(7) 0.2167(2) 0.4397(4) 0.0248(13) Uani 1 1 d .
N4 N 0.1093(7) 0.2706(2) 0.4782(4) 0.0232(13) Uani 1 1 d .
N5 N -0.1818(7) 0.1903(2) 0.5426(4) 0.0243(13) Uani 1 1 d .
N6 N -0.1656(7) 0.2492(2) 0.5593(4) 0.0227(12) 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Pb Pb -3.3944 10.1111 '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
C1 Au1 C7 172.3(3)
C1 Au1 Pb1 92.9(2)
C7 Au1 Pb1 94.8(2)
N5 Pb1 N1 78.73(19)
N5 Pb1 N3 77.77(19)
N1 Pb1 N3 79.16(19)
N5 Pb1 Au1 85.36(13)
N1 Pb1 Au1 136.35(14)
N3 Pb1 Au1 136.49(13)
C2 C1 C6 111.6(7)
C2 C1 Au1 119.5(5)
C6 C1 Au1 128.8(5)
C3 C2 F1 115.6(7)
C3 C2 C1 124.8(7)
F1 C2 C1 119.6(7)
C2 C3 F2 121.3(7)
C2 C3 C4 120.3(7)
F2 C3 C4 118.4(7)
F3 C4 C3 120.8(7)
F3 C4 C5 120.5(8)
C3 C4 C5 118.7(7)
C6 C5 F4 122.3(7)
C6 C5 C4 117.9(7)
F4 C5 C4 119.8(7)
C5 C6 F5 114.5(7)
C5 C6 C1 126.7(7)
F5 C6 C1 118.7(6)
C12 C7 C8 112.5(6)
C12 C7 Au1 128.4(5)
C8 C7 Au1 119.0(5)
F6 C8 C9 116.9(6)
F6 C8 C7 118.7(6)
C9 C8 C7 124.4(7)
F7 C9 C10 121.0(7)
F7 C9 C8 120.3(7)
C10 C9 C8 118.7(7)
F8 C10 C11 120.1(7)
F8 C10 C9 120.0(7)
C11 C10 C9 119.9(7)
F9 C11 C10 119.2(7)
F9 C11 C12 122.1(7)
C10 C11 C12 118.7(7)
C11 C12 C7 125.8(7)
C11 C12 F10 114.7(6)
C7 C12 F10 119.5(6)
N1 C13 C14 111.1(7)
N1 C13 H13 124.4
C14 C13 H13 124.4
C15 C14 C13 105.3(6)
C15 C14 H14 127.3
C13 C14 H14 127.3
N2 C15 C14 108.4(6)
N2 C15 H15 125.8
C14 C15 H15 125.8
N3 C16 C17 111.3(6)
N3 C16 H16 124.4
C17 C16 H16 124.4
C18 C17 C16 105.1(7)
C18 C17 H17 127.4
C16 C17 H17 127.4
C17 C18 N4 108.6(6)
C17 C18 H18 125.7
N4 C18 H18 125.7
N5 C19 C20 111.1(7)
N5 C19 H19 124.4
C20 C19 H19 124.4
C21 C20 C19 104.5(6)
C21 C20 H20 127.7
C19 C20 H20 127.7
N6 C21 C20 109.9(7)
N6 C21 H21 125.1
C20 C21 H21 125.1
N4 B1 N6 109.1(5)
N4 B1 N2 110.2(6)
N6 B1 N2 107.7(6)
N4 B1 H1 109.9
N6 B1 H1 109.9
N2 B1 H1 109.9
C13 N1 N2 105.6(6)
C13 N1 Pb1 133.5(5)
N2 N1 Pb1 120.4(4)
C15 N2 N1 109.5(5)
C15 N2 B1 128.5(6)
N1 N2 B1 121.9(5)
C16 N3 N4 105.9(5)
C16 N3 Pb1 134.1(5)
N4 N3 Pb1 119.7(4)
N3 N4 C18 109.1(5)
N3 N4 B1 123.0(5)
C18 N4 B1 127.8(6)
C19 N5 N6 106.9(5)
C19 N5 Pb1 132.2(5)
N6 N5 Pb1 120.9(4)
C21 N6 N5 107.6(5)
C21 N6 B1 130.1(6)
N5 N6 B1 122.2(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Au1 C1 2.037(7)
Au1 C7 2.044(7)
Au1 Pb1 3.2778(4)
Pb1 N5 2.369(5)
Pb1 N1 2.390(6)
Pb1 N3 2.392(5)
C1 C2 1.386(10)
C1 C6 1.394(10)
C2 C3 1.359(10)
C2 F1 1.363(8)
C3 F2 1.356(8)
C3 C4 1.366(11)
C4 F3 1.353(8)
C4 C5 1.390(10)
C5 C6 1.352(10)
C5 F4 1.347(9)
C6 F5 1.371(8)
C7 C12 1.372(10)
C7 C8 1.399(10)
C8 F6 1.359(8)
C8 C9 1.385(10)
C9 F7 1.342(8)
C9 C10 1.372(11)
C10 F8 1.353(8)
C10 C11 1.366(10)
C11 F9 1.353(8)
C11 C12 1.373(10)
C12 F10 1.380(8)
C13 N1 1.336(9)
C13 C14 1.375(10)
C13 H13 0.93
C14 C15 1.367(10)
C14 H14 0.93
C15 N2 1.346(8)
C15 H15 0.93
C16 N3 1.345(8)
C16 C17 1.381(10)
C16 H16 0.93
C17 C18 1.368(10)
C17 H17 0.93
C18 N4 1.367(8)
C18 H18 0.93
C19 N5 1.328(8)
C19 C20 1.369(10)
C19 H19 0.93
C20 C21 1.365(10)
C20 H20 0.93
C21 N6 1.347(8)
C21 H21 0.93
B1 N4 1.530(9)
B1 N6 1.538(9)
B1 N2 1.541(9)
B1 H1 0.98
N1 N2 1.371(7)
N3 N4 1.367(7)
N5 N6 1.370(7)
