#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:08:46 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179828 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/24/7012489.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_7012489
loop_
_publ_author_name
'Leung, Wing-Por'
'Hou, Henry L.'
'Cheng, Hui'
'Yang, Qing-Chuan'
'Li, Hung-Wing'
'Mak, Thomas C. W.'
_publ_section_title
;
 Synthesis and structural characterisation of low-valent Group 14 metal
 complexes containing tridentate 2,6-pyridyl-bridged bis(1-azaallyl)
 ligands
;
_journal_issue                   8
_journal_name_full               'Dalton Transactions'
_journal_page_first              1505
_journal_paper_doi               10.1039/b211305h
_journal_year                    2003
_chemical_formula_sum            'C23 H41 N3 Pb Si2'
_chemical_formula_weight         622.96
_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                103.36(3)
_cell_angle_beta                 100.73(3)
_cell_angle_gamma                100.66(3)
_cell_formula_units_Z            2
_cell_length_a                   9.751(2)
_cell_length_b                   12.115(2)
_cell_length_c                   12.609(3)
_cell_measurement_temperature    294(2)
_cell_volume                     1382.8(6)
_computing_cell_refinement       'BIOTEX RIGAKU'
_computing_data_collection       'RAXIS-IIC RIGAKU'
_computing_data_reduction        'BIOTEX RIGAKU'
_computing_molecular_graphics    'SIEMENS SHELXTL'
_computing_publication_material  'SIEMENS SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.844
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_device_type  'RAXIS-IIC RIGAKU'
_diffrn_measurement_method       IP
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0774
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4114
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    6.200
_exptl_absorpt_correction_T_max  1.073
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   ABSCOR
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.722
_refine_diff_density_min         -3.803
_refine_diff_density_rms         0.210
_refine_ls_extinction_coef       0.0129(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0734
_refine_ls_shift/su_max          0.604
_refine_ls_shift/su_mean         0.099
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1742P)²+1.6688P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2011
_refine_ls_wR_factor_ref         0.2156
_reflns_number_gt                3774
_reflns_number_total             4114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211305h.txt
_cod_data_source_block           p-1_b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1382.8(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012489
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 0.489181(19) 0.354746(15) 0.228489(14) 0.06455(6) Uani 1 1 d . . .
Si1 Si 0.73844(18) 0.38911(15) 0.08417(12) 0.0739(5) Uani 1 1 d . . .
Si2 Si 0.66782(19) 0.13241(14) 0.29413(14) 0.0760(5) Uani 1 1 d . . .
N1 N 0.5980(4) 0.4101(4) 0.4209(3) 0.0599(12) Uani 1 1 d . . .
N2 N 0.7058(5) 0.4590(4) 0.2095(3) 0.0646(13) Uani 1 1 d . . .
N3 N 0.5105(5) 0.1768(4) 0.2563(4) 0.0708(14) Uani 1 1 d . . .
C1 C 0.7163(6) 0.4982(4) 0.4666(4) 0.0663(16) Uani 1 1 d . . .
C2 C 0.7787(7) 0.5214(5) 0.5843(4) 0.0768(19) Uani 1 1 d . . .
H2A H 0.8595 0.5822 0.6199 0.092 Uiso 1 1 calc R . .
C3 C 0.7152(7) 0.4504(5) 0.6449(4) 0.0767(18) Uani 1 1 d . . .
H3A H 0.7537 0.4650 0.7214 0.092 Uiso 1 1 calc R . .
C4 C 0.5973(7) 0.3598(5) 0.5919(5) 0.0806(19) Uani 1 1 d . . .
H4A H 0.5567 0.3141 0.6332 0.097 Uiso 1 1 calc R . .
C5 C 0.5386(6) 0.3357(5) 0.4801(4) 0.0715(17) Uani 1 1 d . . .
C6 C 0.7693(5) 0.5723(5) 0.4082(4) 0.0644(15) Uani 1 1 d . . .
H6A H 0.8177 0.6465 0.4540 0.077 Uiso 1 1 calc R . .
C7 C 0.7657(7) 0.5599(5) 0.2955(4) 0.0722(17) Uani 1 1 d . . .
C8 C 0.8365(6) 0.6693(5) 0.2646(5) 0.0758(18) Uani 1 1 d . . .
C9 C 0.8869(10) 0.7816(6) 0.3638(6) 0.108(3) Uani 1 1 d . . .
H9A H 0.8076 0.7948 0.3961 0.161 Uiso 1 1 calc R . .
H9B H 0.9220 0.8470 0.3373 0.161 Uiso 1 1 calc R . .
H9C H 0.9624 0.7727 0.4197 0.161 Uiso 1 1 calc R . .
C10 C 0.9699(8) 0.6529(6) 0.2155(6) 0.102(3) Uani 1 1 d . . .
H10A H 0.9427 0.5838 0.1533 0.153 Uiso 1 1 calc R . .
H10B H 1.0448 0.6451 0.2726 0.153 Uiso 1 1 calc R . .
H10C H 1.0041 0.7196 0.1904 0.153 Uiso 1 1 calc R . .
C11 C 0.7234(8) 0.6955(6) 0.1787(6) 0.094(2) Uani 1 1 d . . .
H11A H 0.6422 0.7058 0.2095 0.142 Uiso 1 1 calc R . .
H11B H 0.6931 0.6315 0.1117 0.142 Uiso 1 1 calc R . .
H11C H 0.7637 0.7655 0.1610 0.142 Uiso 1 1 calc R . .
C12 C 0.5927(9) 0.2504(6) 0.0164(4) 0.103(3) Uani 1 1 d . . .
H12A H 0.5008 0.2694 0.0032 0.155 Uiso 1 1 calc R . .
H12B H 0.5940 0.2003 0.0653 0.155 Uiso 1 1 calc R . .
H12C H 0.6093 0.2111 -0.0537 0.155 Uiso 1 1 calc R . .
C13 C 0.9156(8) 0.3402(7) 0.1062(7) 0.112(3) Uani 1 1 d . . .
H13A H 0.9214 0.3027 0.1657 0.168 Uiso 1 1 calc R . .
H13B H 0.9950 0.4070 0.1259 0.168 Uiso 1 1 calc R . .
H13C H 0.9189 0.2863 0.0382 0.168 Uiso 1 1 calc R . .
C14 C 0.4187(7) 0.2417(5) 0.4180(5) 0.0767(18) Uani 1 1 d . . .
H14A H 0.3418 0.2298 0.4514 0.092 Uiso 1 1 calc R . .
C15 C 0.4042(6) 0.1685(5) 0.3169(4) 0.0703(17) Uani 1 1 d . . .
C16 C 0.2649(8) 0.0724(7) 0.2562(5) 0.097(3) Uani 1 1 d . . .
C17 C 0.1493(7) 0.0671(7) 0.3260(7) 0.116(3) Uani 1 1 d . . .
H17A H 0.1233 0.1408 0.3423 0.173 Uiso 1 1 calc R . .
H17B H 0.1874 0.0507 0.3950 0.173 Uiso 1 1 calc R . .
H17C H 0.0658 0.0065 0.2839 0.173 Uiso 1 1 calc R . .
C18 C 0.3018(10) -0.0510(7) 0.2326(11) 0.170(5) Uani 1 1 d . . .
H18A H 0.3725 -0.0520 0.1889 0.255 Uiso 1 1 calc R . .
H18B H 0.2163 -0.1102 0.1920 0.255 Uiso 1 1 calc R . .
H18C H 0.3389 -0.0659 0.3026 0.255 Uiso 1 1 calc R . .
C19 C 0.2109(9) 0.0927(11) 0.1441(8) 0.183(4) Uani 1 1 d . . .
H19A H 0.1880 0.1676 0.1554 0.274 Uiso 1 1 calc R . .
H19B H 0.1264 0.0328 0.1029 0.274 Uiso 1 1 calc R . .
H19C H 0.2839 0.0906 0.1026 0.274 Uiso 1 1 calc R . .
C20 C 0.7270(10) 0.4631(7) -0.0335(6) 0.114(3) Uani 1 1 d . . .
H20A H 0.6384 0.4876 -0.0445 0.171 Uiso 1 1 calc R . .
H20B H 0.7302 0.4091 -0.1014 0.171 Uiso 1 1 calc R . .
H20C H 0.8064 0.5299 -0.0139 0.171 Uiso 1 1 calc R . .
C21 C 0.6447(9) 0.0406(6) 0.4014(7) 0.154(3) Uani 1 1 d . . .
H21A H 0.6237 0.0872 0.4663 0.231 Uiso 1 1 calc R . .
H21B H 0.7319 0.0170 0.4236 0.231 Uiso 1 1 calc R . .
H21C H 0.5671 -0.0274 0.3669 0.231 Uiso 1 1 calc R . .
C22 C 0.8317(7) 0.2556(6) 0.3580(6) 0.085(2) Uani 1 1 d . . .
H22A H 0.8446 0.3012 0.3062 0.128 Uiso 1 1 calc R . .
H22B H 0.9144 0.2245 0.3746 0.128 Uiso 1 1 calc R . .
H22C H 0.8199 0.3040 0.4260 0.128 Uiso 1 1 calc R . .
C23 C 0.7086(8) 0.0354(6) 0.1693(6) 0.103(2) Uani 1 1 d . . .
H23A H 0.7209 0.0776 0.1147 0.154 Uiso 1 1 calc R . .
H23B H 0.6303 -0.0324 0.1365 0.154 Uiso 1 1 calc R . .
H23C H 0.7951 0.0117 0.1933 0.154 Uiso 1 1 calc R . .
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'
Si Si 0.0817 0.0704 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Pb1 N2 110.95(17) . . ?
N3 Pb1 N1 79.17(15) . . ?
N2 Pb1 N1 85.58(15) . . ?
N3 Pb1 C15 29.88(18) . . ?
N2 Pb1 C15 136.17(17) . . ?
N1 Pb1 C15 71.29(14) . . ?
N2 Si1 C12 108.7(3) . . ?
N2 Si1 C20 118.7(3) . . ?
C12 Si1 C20 101.1(3) . . ?
N2 Si1 C13 112.1(3) . . ?
C12 Si1 C13 105.6(4) . . ?
C20 Si1 C13 109.4(4) . . ?
N3 Si2 C22 114.1(3) . . ?
N3 Si2 C23 111.7(3) . . ?
C22 Si2 C23 106.1(3) . . ?
N3 Si2 C21 109.1(3) . . ?
C22 Si2 C21 108.5(3) . . ?
C23 Si2 C21 107.0(4) . . ?
C1 N1 C5 123.7(4) . . ?
C1 N1 Pb1 121.9(3) . . ?
C5 N1 Pb1 114.1(3) . . ?
C7 N2 Si1 138.3(4) . . ?
C7 N2 Pb1 113.0(4) . . ?
Si1 N2 Pb1 108.61(18) . . ?
C15 N3 Si2 121.3(4) . . ?
C15 N3 Pb1 95.1(4) . . ?
Si2 N3 Pb1 127.6(2) . . ?
N1 C1 C6 122.7(4) . . ?
N1 C1 C2 117.5(5) . . ?
C6 C1 C2 119.5(4) . . ?
C3 C2 C1 118.7(5) . . ?
C4 C3 C2 120.6(5) . . ?
C5 C4 C3 121.3(6) . . ?
C4 C5 N1 118.1(5) . . ?
C4 C5 C14 124.9(6) . . ?
N1 C5 C14 117.0(5) . . ?
C1 C6 C7 133.6(4) . . ?
N2 C7 C6 125.9(5) . . ?
N2 C7 C8 117.5(5) . . ?
C6 C7 C8 116.6(4) . . ?
C11 C8 C7 108.0(5) . . ?
C11 C8 C9 105.0(6) . . ?
C7 C8 C9 114.0(5) . . ?
C11 C8 C10 109.9(6) . . ?
C7 C8 C10 112.5(6) . . ?
C9 C8 C10 107.0(5) . . ?
C15 C14 C5 127.3(6) . . ?
C14 C15 N3 122.6(5) . . ?
C14 C15 C16 122.2(6) . . ?
N3 C15 C16 115.2(5) . . ?
C14 C15 Pb1 91.5(4) . . ?
N3 C15 Pb1 55.0(3) . . ?
C16 C15 Pb1 120.7(4) . . ?
C19 C16 C15 107.2(6) . . ?
C19 C16 C17 112.7(7) . . ?
C15 C16 C17 113.5(5) . . ?
C19 C16 C18 107.3(8) . . ?
C15 C16 C18 109.5(6) . . ?
C17 C16 C18 106.6(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N3 2.302(5) . ?
Pb1 N2 2.335(4) . ?
Pb1 N1 2.342(3) . ?
Pb1 C15 2.800(6) . ?
Si1 N2 1.728(5) . ?
Si1 C12 1.891(7) . ?
Si1 C20 1.899(8) . ?
Si1 C13 1.921(9) . ?
Si2 N3 1.739(5) . ?
Si2 C22 1.874(6) . ?
Si2 C23 1.889(8) . ?
Si2 C21 1.958(9) . ?
N1 C1 1.347(6) . ?
N1 C5 1.409(7) . ?
N2 C7 1.378(6) . ?
N3 C15 1.401(8) . ?
C1 C6 1.375(8) . ?
C1 C2 1.434(7) . ?
C2 C3 1.411(9) . ?
C3 C4 1.371(8) . ?
C4 C5 1.359(8) . ?
C5 C14 1.426(7) . ?
C6 C7 1.387(8) . ?
C7 C8 1.545(9) . ?
C8 C11 1.527(10) . ?
C8 C9 1.548(8) . ?
C8 C10 1.567(11) . ?
C14 C15 1.340(7) . ?
C15 C16 1.549(8) . ?
C16 C19 1.505(13) . ?
C16 C17 1.556(11) . ?
C16 C18 1.576(12) . ?
