#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:00:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180022 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/16/7031671.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_7031671
loop_
_publ_author_name
'Imran, Muhammad'
'Mix, Andreas'
'Neumann, Beate'
'Stammler, Hans-Georg'
'Monkowius, Uwe'
'Gründlinger, Petra'
'Mitzel, Norbert W.'
_publ_section_title
;
 Hemi- and holo-directed lead(II) complexes in a soft ligand environment.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              924
_journal_page_last               937
_journal_paper_doi               10.1039/c4dt01406e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C13 H14 B N9 O Pb S8'
_chemical_formula_sum            'C13 H14 B N9 O Pb S8'
_chemical_formula_weight         786.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.827(6)
_cell_angle_beta                 108.210(6)
_cell_angle_gamma                95.805(5)
_cell_formula_units_Z            2
_cell_length_a                   10.1258(9)
_cell_length_b                   11.5049(11)
_cell_length_c                   12.7990(19)
_cell_measurement_reflns_used    9141
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      43.998
_cell_measurement_theta_min      3.150
_cell_volume                     1274.3(3)
_computing_cell_refinement       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker KAPPA APEX II   '
_diffrn_measurement_device_type  'four three circle diffractometer'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'graphite monochromator  '
_diffrn_radiation_source         'fine focus sealed tube  '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0109
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            87623
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    7.303
_exptl_absorpt_correction_T_max  0.4279
_exptl_absorpt_correction_T_min  0.1664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.333
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         7414
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0153
_refine_ls_R_factor_gt           0.0150
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0123P)²+1.9951P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0354
_refine_ls_wR_factor_ref         0.0356
_reflns_number_gt                7306
_reflns_number_total             7414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01406e1.cif
_cod_data_source_block           compound1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7031671--7031680.cif.
;
_cod_database_code               7031671
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.102614(7) 0.448860(6) 0.320915(6) 0.01509(2) Uani 1 1 d . . .
S1 S 0.28211(5) 0.38624(4) 0.15974(4) 0.01926(8) Uani 1 1 d . . .
S2 S 0.14691(5) 0.12257(5) -0.04730(4) 0.02280(9) Uani 1 1 d . . .
S3 S 0.62187(5) 0.36106(5) 0.56276(4) 0.01918(8) Uani 1 1 d . . .
S4 S 0.78093(4) 0.21580(4) 0.41361(4) 0.01775(8) Uani 1 1 d . . .
S5 S 0.03892(5) 0.16679(4) 0.31599(5) 0.02120(9) Uani 1 1 d . . .
S6 S 0.14045(7) -0.02585(7) 0.40647(8) 0.04140(16) Uani 1 1 d . . .
S7 S 0.02291(6) 0.36638(5) 0.74585(5) 0.02642(10) Uani 1 1 d . . .
S8 S 0.30320(6) 0.38024(7) 0.69992(6) 0.03425(13) Uani 1 1 d . . .
N1 N 0.26907(16) 0.15176(15) 0.16842(14) 0.0165(3) Uani 1 1 d . . .
N2 N 0.22158(18) 0.01940(16) 0.10070(16) 0.0223(3) Uani 1 1 d . . .
N3 N 0.51418(16) 0.19456(14) 0.32454(14) 0.0154(3) Uani 1 1 d . . .
N4 N 0.54260(17) 0.11053(16) 0.22924(15) 0.0213(3) Uani 1 1 d . . .
N5 N 0.29650(16) 0.10709(16) 0.35158(15) 0.0185(3) Uani 1 1 d . . .
N6 N 0.3784(2) 0.0286(2) 0.3843(2) 0.0356(5) Uani 1 1 d . . .
N7 N 0.09150(16) 0.45503(15) 0.60014(14) 0.0163(3) Uani 1 1 d . . .
N8 N 0.19500(17) 0.48199(16) 0.55825(14) 0.0180(3) Uani 1 1 d . . .
B1 B 0.3563(2) 0.20158(19) 0.30669(18) 0.0157(3) Uani 1 1 d . . .
H1B H 0.350(2) 0.298(2) 0.355(2) 0.013(5) Uiso 1 1 d . . .
C1 C 0.23997(18) 0.22386(17) 0.10621(16) 0.0165(3) Uani 1 1 d . . .
C2 C 0.1563(2) -0.0080(2) -0.01241(19) 0.0250(4) Uani 1 1 d . . .
H2 H 0.1160 -0.0945 -0.0727 0.030 Uiso 1 1 calc R . .
C3 C 0.62669(18) 0.25767(16) 0.43019(16) 0.0149(3) Uani 1 1 d . . .
C4 C 0.6779(2) 0.11353(19) 0.26423(18) 0.0211(4) Uani 1 1 d . . .
H4 H 0.7179 0.0624 0.2107 0.025 Uiso 1 1 calc R . .
C5 C 0.16574(19) 0.09189(18) 0.35681(18) 0.0192(3) Uani 1 1 d . . .
C6 C 0.3093(3) -0.0457(3) 0.4143(4) 0.0512(9) Uani 1 1 d . . .
H6 H 0.3486 -0.1071 0.4391 0.061 Uiso 1 1 calc R . .
C7 C 0.1304(2) 0.40209(18) 0.67650(17) 0.0184(3) Uani 1 1 d . . .
C8 C 0.3105(2) 0.4485(2) 0.6023(2) 0.0257(4) Uani 1 1 d . . .
H8 H 0.3922 0.4605 0.5824 0.031 Uiso 1 1 calc R . .
O1 O -0.15023(19) 0.29818(17) 0.14895(16) 0.0339(3) Uiso 1 1 d . . .
N9A N -0.2577(3) 0.3082(2) -0.0316(2) 0.0223(6) Uiso 0.686(5) 1 d PD A 1
C9A C -0.2612(3) 0.2912(3) 0.0652(3) 0.0205(6) Uiso 0.686(5) 1 d PD A 1
C10A C -0.3966(4) 0.2942(4) -0.1175(4) 0.0298(8) Uiso 0.686(5) 1 d PD A 1
H10A H -0.4263 0.2114 -0.1909 0.036 Uiso 0.686(5) 1 calc PR A 1
H10B H -0.3961 0.3661 -0.1423 0.036 Uiso 0.686(5) 1 calc PR A 1
C11A C -0.4960(5) 0.2969(4) -0.0493(4) 0.0417(9) Uiso 0.686(5) 1 d PD A 1
H11A H -0.5876 0.2309 -0.1028 0.050 Uiso 0.686(5) 1 calc PR A 1
H11B H -0.5169 0.3829 -0.0196 0.050 Uiso 0.686(5) 1 calc PR A 1
C12A C -0.4160(5) 0.2678(5) 0.0575(4) 0.0342(9) Uiso 0.686(5) 1 d PD A 1
H12A H -0.4535 0.1773 0.0412 0.041 Uiso 0.686(5) 1 calc PR A 1
H12B H -0.4238 0.3266 0.1336 0.041 Uiso 0.686(5) 1 calc PR A 1
C13A C -0.1323(4) 0.3179(5) -0.0587(4) 0.0320(9) Uiso 0.686(5) 1 d PD A 1
H13A H -0.0477 0.3367 0.0140 0.048 Uiso 0.686(5) 1 calc PR A 1
H13B H -0.1240 0.3876 -0.0845 0.048 Uiso 0.686(5) 1 calc PR A 1
H13C H -0.1387 0.2361 -0.1242 0.048 Uiso 0.686(5) 1 calc PR A 1
N9B N -0.3343(7) 0.2726(6) -0.0115(6) 0.0330(16) Uiso 0.314(5) 1 d PD A 2
C9B C -0.1944(7) 0.3066(6) 0.0467(6) 0.0231(14) Uiso 0.314(5) 1 d PD A 2
C10B C -0.3897(7) 0.2591(8) -0.1388(6) 0.0223(15) Uiso 0.314(5) 1 d PD A 2
H10C H -0.4444 0.3240 -0.1470 0.027 Uiso 0.314(5) 1 calc PR A 2
H10D H -0.4505 0.1714 -0.1967 0.027 Uiso 0.314(5) 1 calc PR A 2
C11B C -0.2431(11) 0.2854(11) -0.1568(9) 0.056(3) Uiso 0.314(5) 1 d PD A 2
H11C H -0.2248 0.2028 -0.2037 0.068 Uiso 0.314(5) 1 calc PR A 2
H11D H -0.2479 0.3394 -0.2020 0.068 Uiso 0.314(5) 1 calc PR A 2
C12B C -0.1274(8) 0.3528(9) -0.0355(8) 0.0266(18) Uiso 0.314(5) 1 d PD A 2
H12C H -0.1081 0.4477 -0.0070 0.032 Uiso 0.314(5) 1 calc PR A 2
H12D H -0.0378 0.3252 -0.0350 0.032 Uiso 0.314(5) 1 calc PR A 2
C13B C -0.4323(8) 0.2301(9) 0.0302(8) 0.0261(16) Uiso 0.314(5) 1 d PD A 2
H13D H -0.5299 0.2091 -0.0295 0.039 Uiso 0.314(5) 1 calc PR A 2
H13E H -0.4230 0.2984 0.1079 0.039 Uiso 0.314(5) 1 calc PR A 2
H13F H -0.4131 0.1530 0.0415 0.039 Uiso 0.314(5) 1 calc PR A 2
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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 '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
N7 Pb1 O1 74.82(5) 2_566 .
N7 Pb1 N8 75.60(5) 2_566 .
O1 Pb1 N8 124.29(5) . .
N7 Pb1 S7 57.95(4) 2_566 2_566
O1 Pb1 S7 79.32(4) . 2_566
N8 Pb1 S7 120.40(4) . 2_566
N7 Pb1 S3 111.62(4) 2_566 2_666
O1 Pb1 S3 159.12(4) . 2_666
N8 Pb1 S3 76.39(4) . 2_666
S7 Pb1 S3 87.473(16) 2_566 2_666
N7 Pb1 S1 157.12(3) 2_566 .
O1 Pb1 S1 97.30(4) . .
N8 Pb1 S1 124.87(3) . .
S7 Pb1 S1 99.781(16) 2_566 .
S3 Pb1 S1 68.903(15) 2_666 .
C1 S1 Pb1 98.74(6) . .
C2 S2 C1 88.81(10) . .
C3 S3 Pb1 103.72(6) . 2_666
C4 S4 C3 88.21(9) . .
C6 S6 C5 88.77(11) . .
C7 S7 Pb1 80.09(6) . 2_566
C8 S8 C7 87.95(9) . .
C1 N1 N2 116.19(15) . .
C1 N1 B1 126.68(15) . .
N2 N1 B1 117.06(15) . .
C2 N2 N1 110.37(17) . .
C3 N3 N4 115.83(14) . .
C3 N3 B1 124.64(14) . .
N4 N3 B1 119.32(14) . .
C4 N4 N3 109.85(16) . .
C5 N5 N6 116.05(16) . .
C5 N5 B1 124.59(15) . .
N6 N5 B1 119.30(15) . .
C6 N6 N5 110.28(18) . .
C7 N7 N8 113.99(15) . .
C7 N7 Pb1 95.34(11) . 2_566
N8 N7 Pb1 142.32(12) . 2_566
C8 N8 N7 112.37(16) . .
C8 N8 Pb1 119.16(13) . .
N7 N8 Pb1 116.97(11) . .
N1 B1 N5 108.34(14) . .
N1 B1 N3 107.87(14) . .
N5 B1 N3 107.06(14) . .
N1 B1 H1B 110.6(13) . .
N5 B1 H1B 111.4(13) . .
N3 B1 H1B 111.4(13) . .
N1 C1 S1 128.48(14) . .
N1 C1 S2 109.13(13) . .
S1 C1 S2 122.39(11) . .
N2 C2 S2 115.50(15) . .
N2 C2 H2 122.3 . .
S2 C2 H2 122.3 . .
N3 C3 S3 125.95(13) . .
N3 C3 S4 110.14(12) . .
S3 C3 S4 123.90(11) . .
N4 C4 S4 115.95(14) . .
N4 C4 H4 122.0 . .
S4 C4 H4 122.0 . .
N5 C5 S5 127.27(15) . .
N5 C5 S6 109.55(14) . .
S5 C5 S6 123.11(11) . .
N6 C6 S6 115.34(18) . .
N6 C6 H6 122.3 . .
S6 C6 H6 122.3 . .
N7 C7 S7 122.55(14) . .
N7 C7 S8 111.55(14) . .
S7 C7 S8 125.87(11) . .
N8 C8 S8 114.14(15) . .
N8 C8 H8 122.9 . .
S8 C8 H8 122.9 . .
C9A O1 C9B 37.0(3) . .
C9A O1 Pb1 145.43(17) . .
C9B O1 Pb1 119.3(3) . .
C9A N9A C13A 123.4(3) . .
C9A N9A C10A 114.1(3) . .
C13A N9A C10A 121.8(3) . .
O1 C9A N9A 122.9(3) . .
O1 C9A C12A 127.7(3) . .
N9A C9A C12A 109.4(3) . .
N9A C10A C11A 104.3(3) . .
N9A C10A H10A 110.9 . .
C11A C10A H10A 110.9 . .
N9A C10A H10B 110.9 . .
C11A C10A H10B 110.9 . .
H10A C10A H10B 108.9 . .
C10A C11A C12A 105.8(3) . .
C10A C11A H11A 110.6 . .
C12A C11A H11A 110.6 . .
C10A C11A H11B 110.6 . .
C12A C11A H11B 110.6 . .
H11A C11A H11B 108.7 . .
C11A C12A C9A 103.0(3) . .
C11A C12A H12A 111.2 . .
C9A C12A H12A 111.2 . .
C11A C12A H12B 111.2 . .
C9A C12A H12B 111.2 . .
H12A C12A H12B 109.1 . .
C9B N9B C13B 124.6(7) . .
C9B N9B C10B 117.1(6) . .
C13B N9B C10B 117.5(6) . .
O1 C9B N9B 115.2(5) . .
O1 C9B C12B 138.6(5) . .
N9B C9B C12B 106.2(6) . .
N9B C10B C11B 100.3(6) . .
N9B C10B H10C 111.7 . .
C11B C10B H10C 111.7 . .
N9B C10B H10D 111.7 . .
C11B C10B H10D 111.7 . .
H10C C10B H10D 109.5 . .
C12B C11B C10B 107.9(7) . .
C12B C11B H11C 110.1 . .
C10B C11B H11C 110.1 . .
C12B C11B H11D 110.1 . .
C10B C11B H11D 110.1 . .
H11C C11B H11D 108.4 . .
C11B C12B C9B 101.8(6) . .
C11B C12B H12C 111.4 . .
C9B C12B H12C 111.4 . .
C11B C12B H12D 111.4 . .
C9B C12B H12D 111.4 . .
H12C C12B H12D 109.3 . .
N9B C13B H13D 109.5 . .
N9B C13B H13E 109.5 . .
H13D C13B H13E 109.5 . .
N9B C13B H13F 109.5 . .
H13D C13B H13F 109.5 . .
H13E C13B H13F 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 N7 2.6376(15) 2_566
Pb1 O1 2.6735(18) .
Pb1 N8 2.7456(16) .
Pb1 S7 2.8430(6) 2_566
Pb1 S3 2.9208(6) 2_666
Pb1 S1 3.0953(5) .
S1 C1 1.6869(19) .
S2 C2 1.723(2) .
S2 C1 1.7391(18) .
S3 C3 1.6909(18) .
S3 Pb1 2.9208(6) 2_666
S4 C4 1.721(2) .
S4 C3 1.7319(17) .
S5 C5 1.6744(19) .
S6 C6 1.725(3) .
S6 C5 1.725(2) .
S7 C7 1.711(2) .
S7 Pb1 2.8430(6) 2_566
S8 C8 1.720(2) .
S8 C7 1.7409(19) .
N1 C1 1.343(2) .
N1 N2 1.382(2) .
N1 B1 1.551(3) .
N2 C2 1.285(3) .
N3 C3 1.339(2) .
N3 N4 1.380(2) .
N3 B1 1.558(2) .
N4 C4 1.294(2) .
N5 C5 1.344(2) .
N5 N6 1.377(2) .
N5 B1 1.558(3) .
N6 C6 1.287(3) .
N7 C7 1.316(2) .
N7 N8 1.375(2) .
N7 Pb1 2.6377(15) 2_566
N8 C8 1.295(2) .
B1 H1B 1.06(2) .
C2 H2 0.9500 .
C4 H4 0.9500 .
C6 H6 0.9500 .
C8 H8 0.9500 .
O1 C9A 1.259(3) .
O1 C9B 1.289(6) .
N9A C9A 1.334(4) .
N9A C13A 1.422(5) .
N9A C10A 1.438(4) .
C9A C12A 1.529(5) .
C10A C11A 1.521(6) .
C10A H10A 0.9900 .
C10A H10B 0.9900 .
C11A C12A 1.529(6) .
C11A H11A 0.9900 .
C11A H11B 0.9900 .
C12A H12A 0.9900 .
C12A H12B 0.9900 .
C13A H13A 0.9800 .
C13A H13B 0.9800 .
C13A H13C 0.9800 .
N9B C9B 1.314(8) .
N9B C13B 1.391(9) .
N9B C10B 1.488(9) .
C9B C12B 1.623(9) .
C10B C11B 1.588(11) .
C10B H10C 0.9900 .
C10B H10D 0.9900 .
C11B C12B 1.472(12) .
C11B H11C 0.9900 .
C11B H11D 0.9900 .
C12B H12C 0.9900 .
C12B H12D 0.9900 .
C13B H13D 0.9800 .
C13B H13E 0.9800 .
C13B H13F 0.9800 .
