#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:10:45 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179883 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/79/7017966.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_7017966
loop_
_publ_author_name
'Yang, Dongming'
'Guo, Jianmei'
'Wu, Haishun'
'Ding, Yuqiang'
'Zheng, Wenjun'
_publ_section_title
;
 Synthesis and structural characterization of two-coordinate low-valent
 14-group metal complexes bearing bulky bis(amido)silane ligands.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2187
_journal_page_last               2194
_journal_paper_doi               10.1039/c1dt11774b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C52 H80 N4 Pb2 Si2'
_chemical_formula_weight         1231.76
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.420(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.444(4)
_cell_length_b                   18.724(6)
_cell_length_c                   12.638(4)
_cell_measurement_reflns_used    926
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.750
_cell_measurement_theta_min      3.270
_cell_volume                     2637.1(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11715
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    6.457
_exptl_absorpt_correction_T_max  0.4442
_exptl_absorpt_correction_T_min  0.3583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0259
_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)+(0.0303P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0593
_reflns_number_gt                4027
_reflns_number_total             5195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11774b.txt
_cod_data_source_block           5a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2637.3(16)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7017966
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
Pb1 Pb 1.007798(14) 0.074020(8) 1.083742(13) 0.03179(6) Uani 1 1 d .
Si1 Si 0.76044(10) 0.04756(6) 0.88071(10) 0.0302(2) Uani 1 1 d .
N1 N 0.8158(3) 0.05116(17) 1.0311(3) 0.0301(7) Uani 1 1 d .
N2 N 0.8989(3) 0.05251(16) 0.8738(3) 0.0270(7) Uani 1 1 d .
C1 C 0.7560(3) 0.0651(2) 1.1036(3) 0.0291(9) Uani 1 1 d .
C2 C 0.7129(4) 0.0086(2) 1.1479(3) 0.0329(9) Uani 1 1 d .
C3 C 0.6583(4) 0.0239(3) 1.2201(4) 0.0418(11) Uani 1 1 d .
H3A H 0.6277 -0.0135 1.2471 0.050 Uiso 1 1 calc R
C4 C 0.6481(4) 0.0923(3) 1.2529(4) 0.0507(13) Uani 1 1 d .
H4A H 0.6125 0.1010 1.3026 0.061 Uiso 1 1 calc R
C5 C 0.6908(4) 0.1474(3) 1.2119(4) 0.0469(12) Uani 1 1 d .
H5A H 0.6845 0.1937 1.2351 0.056 Uiso 1 1 calc R
C6 C 0.7436(4) 0.1362(2) 1.1360(4) 0.0359(10) Uani 1 1 d .
C7 C 0.7851(4) 0.2008(2) 1.0909(4) 0.0451(11) Uani 1 1 d .
H7A H 0.8113 0.1838 1.0328 0.054 Uiso 1 1 calc R
C8 C 0.6825(5) 0.2541(3) 1.0285(5) 0.0642(15) Uani 1 1 d .
H8A H 0.6166 0.2303 0.9657 0.096 Uiso 1 1 calc R
H8B H 0.7099 0.2926 0.9966 0.096 Uiso 1 1 calc R
H8C H 0.6566 0.2727 1.0842 0.096 Uiso 1 1 calc R
C9 C 0.8922(5) 0.2377(3) 1.1906(6) 0.0735(17) Uani 1 1 d .
H9A H 0.9560 0.2039 1.2281 0.110 Uiso 1 1 calc R
H9B H 0.8682 0.2563 1.2477 0.110 Uiso 1 1 calc R
H9C H 0.9196 0.2762 1.1585 0.110 Uiso 1 1 calc R
C10 C 0.7243(4) -0.0697(2) 1.1201(4) 0.0383(10) Uani 1 1 d .
H10A H 0.7650 -0.0713 1.0692 0.046 Uiso 1 1 calc R
C11 C 0.6022(5) -0.1066(3) 1.0546(5) 0.0653(15) Uani 1 1 d .
H11A H 0.5543 -0.0811 0.9831 0.098 Uiso 1 1 calc R
H11B H 0.5618 -0.1072 1.1040 0.098 Uiso 1 1 calc R
H11C H 0.6140 -0.1548 1.0357 0.098 Uiso 1 1 calc R
C12 C 0.8005(5) -0.1107(3) 1.2328(4) 0.0573(14) Uani 1 1 d .
H12A H 0.8771 -0.0878 1.2736 0.086 Uiso 1 1 calc R
H12B H 0.8119 -0.1588 1.2131 0.086 Uiso 1 1 calc R
H12C H 0.7607 -0.1116 1.2827 0.086 Uiso 1 1 calc R
C13 C 0.6573(4) 0.1217(3) 0.7952(4) 0.0522(13) Uani 1 1 d .
H13A H 0.5843 0.1019 0.7355 0.078 Uiso 1 1 calc R
H13B H 0.6953 0.1503 0.7585 0.078 Uiso 1 1 calc R
H13C H 0.6393 0.1509 0.8477 0.078 Uiso 1 1 calc R
C14 C 0.6718(4) -0.0358(3) 0.8165(4) 0.0450(11) Uani 1 1 d .
H14A H 0.5960 -0.0235 0.7520 0.067 Uiso 1 1 calc R
H14B H 0.6583 -0.0604 0.8762 0.067 Uiso 1 1 calc R
H14C H 0.7156 -0.0663 0.7883 0.067 Uiso 1 1 calc R
C15 C 0.9010(4) 0.0941(2) 0.7763(3) 0.0323(9) Uani 1 1 d .
C16 C 0.8666(4) 0.0609(2) 0.6632(4) 0.0404(11) Uani 1 1 d .
C17 C 0.8675(4) 0.1015(3) 0.5712(4) 0.0508(12) Uani 1 1 d .
H17A H 0.8472 0.0796 0.4987 0.061 Uiso 1 1 calc R
C18 C 0.8976(4) 0.1730(3) 0.5839(4) 0.0549(14) Uani 1 1 d .
H18A H 0.8972 0.1990 0.5210 0.066 Uiso 1 1 calc R
C19 C 0.9275(4) 0.2045(3) 0.6892(5) 0.0503(13) Uani 1 1 d .
H19A H 0.9478 0.2527 0.6976 0.060 Uiso 1 1 calc R
C20 C 0.9293(4) 0.1678(2) 0.7869(4) 0.0379(10) Uani 1 1 d .
C21 C 0.9644(4) 0.2116(2) 0.9003(4) 0.0427(11) Uani 1 1 d .
H21A H 0.9386 0.1842 0.9509 0.051 Uiso 1 1 calc R
C22 C 1.0989(5) 0.2211(3) 0.9686(5) 0.0722(17) Uani 1 1 d .
H22A H 1.1374 0.1753 0.9825 0.108 Uiso 1 1 calc R
H22B H 1.1174 0.2438 1.0429 0.108 Uiso 1 1 calc R
H22C H 1.1272 0.2503 0.9238 0.108 Uiso 1 1 calc R
C23 C 0.9001(6) 0.2849(3) 0.8779(6) 0.084(2) Uani 1 1 d .
H23A H 0.9251 0.3097 0.9516 0.125 Uiso 1 1 calc R
H23B H 0.8149 0.2776 0.8426 0.125 Uiso 1 1 calc R
H23C H 0.9205 0.3128 0.8257 0.125 Uiso 1 1 calc R
C24 C 0.8305(5) -0.0167(3) 0.6369(4) 0.0496(12) Uani 1 1 d .
H24A H 0.8267 -0.0370 0.7066 0.059 Uiso 1 1 calc R
C25 C 0.9257(7) -0.0581(3) 0.6172(6) 0.0785(19) Uani 1 1 d .
H25A H 1.0022 -0.0523 0.6846 0.118 Uiso 1 1 calc R
H25B H 0.9301 -0.0402 0.5480 0.118 Uiso 1 1 calc R
H25C H 0.9048 -0.1078 0.6066 0.118 Uiso 1 1 calc R
C26 C 0.7062(5) -0.0245(3) 0.5328(4) 0.0743(18) Uani 1 1 d .
H26A H 0.6488 0.0016 0.5489 0.111 Uiso 1 1 calc R
H26B H 0.6842 -0.0741 0.5215 0.111 Uiso 1 1 calc R
H26C H 0.7077 -0.0060 0.4626 0.111 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
N1 Pb1 N2 68.62(11) . .
N1 Pb1 N2 102.11(11) . 3_757
N2 Pb1 N2 93.21(10) . 3_757
N1 Pb1 Si1 33.48(8) . .
N2 Pb1 Si1 35.41(8) . .
N2 Pb1 Si1 102.59(7) 3_757 .
N1 Pb1 Pb1 84.36(8) . 3_757
N2 Pb1 Pb1 48.67(7) . 3_757
N2 Pb1 Pb1 44.54(7) 3_757 3_757
Si1 Pb1 Pb1 65.88(3) . 3_757
N1 Si1 N2 97.68(16) . .
N1 Si1 C13 116.5(2) . .
N2 Si1 C13 111.45(19) . .
N1 Si1 C14 112.48(19) . .
N2 Si1 C14 114.91(19) . .
C13 Si1 C14 104.3(2) . .
N1 Si1 Pb1 45.66(11) . .
N2 Si1 Pb1 52.46(11) . .
C13 Si1 Pb1 122.82(17) . .
C14 Si1 Pb1 132.81(16) . .
C1 N1 Si1 130.4(3) . .
C1 N1 Pb1 124.6(2) . .
Si1 N1 Pb1 100.86(15) . .
C15 N2 Si1 116.9(3) . .
C15 N2 Pb1 128.5(2) . .
Si1 N2 Pb1 92.13(13) . .
C15 N2 Pb1 119.1(2) . 3_757
Si1 N2 Pb1 107.42(14) . 3_757
Pb1 N2 Pb1 86.79(10) . 3_757
C2 C1 C6 118.6(4) . .
C2 C1 N1 120.9(3) . .
C6 C1 N1 120.4(3) . .
C3 C2 C1 119.4(4) . .
C3 C2 C10 118.1(4) . .
C1 C2 C10 122.5(4) . .
C4 C3 C2 122.0(4) . .
C4 C3 H3A 119.0 . .
C2 C3 H3A 119.0 . .
C5 C4 C3 119.3(4) . .
C5 C4 H4A 120.4 . .
C3 C4 H4A 120.4 . .
C4 C5 C6 121.9(4) . .
C4 C5 H5A 119.0 . .
C6 C5 H5A 119.0 . .
C5 C6 C1 118.8(4) . .
C5 C6 C7 118.7(4) . .
C1 C6 C7 122.6(4) . .
C6 C7 C9 111.5(4) . .
C6 C7 C8 111.4(4) . .
C9 C7 C8 110.5(4) . .
C6 C7 H7A 107.7 . .
C9 C7 H7A 107.7 . .
C8 C7 H7A 107.7 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C7 C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C7 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C12 C10 C2 110.6(4) . .
C12 C10 C11 109.4(4) . .
C2 C10 C11 112.7(4) . .
C12 C10 H10A 108.0 . .
C2 C10 H10A 108.0 . .
C11 C10 H10A 108.0 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
Si1 C13 H13A 109.5 . .
Si1 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
Si1 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
Si1 C14 H14A 109.5 . .
Si1 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
Si1 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C20 C15 C16 117.9(4) . .
C20 C15 N2 122.3(4) . .
C16 C15 N2 119.7(3) . .
C17 C16 C15 119.0(4) . .
C17 C16 C24 116.8(4) . .
C15 C16 C24 124.2(4) . .
C18 C17 C16 122.3(5) . .
C18 C17 H17A 118.8 . .
C16 C17 H17A 118.8 . .
C19 C18 C17 118.7(4) . .
C19 C18 H18A 120.6 . .
C17 C18 H18A 120.6 . .
C18 C19 C20 122.9(4) . .
C18 C19 H19A 118.5 . .
C20 C19 H19A 118.5 . .
C19 C20 C15 119.2(4) . .
C19 C20 C21 116.4(4) . .
C15 C20 C21 124.4(4) . .
C22 C21 C20 112.3(4) . .
C22 C21 C23 110.5(4) . .
C20 C21 C23 113.2(4) . .
C22 C21 H21A 106.8 . .
C20 C21 H21A 106.8 . .
C23 C21 H21A 106.8 . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C21 C23 H23A 109.5 . .
C21 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C21 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C16 C24 C25 110.4(4) . .
C16 C24 C26 111.6(4) . .
C25 C24 C26 111.9(5) . .
C16 C24 H24A 107.6 . .
C25 C24 H24A 107.6 . .
C26 C24 H24A 107.6 . .
C24 C25 H25A 109.5 . .
C24 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
C24 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C24 C26 H26A 109.5 . .
C24 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C24 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 N1 2.218(3) .
Pb1 N2 2.417(3) .
Pb1 N2 2.587(3) 3_757
Pb1 Si1 3.0457(14) .
Pb1 Pb1 3.4404(9) 3_757
Si1 N1 1.711(3) .
Si1 N2 1.766(3) .
Si1 C13 1.873(5) .
Si1 C14 1.875(5) .
N1 C1 1.438(5) .
N2 C15 1.468(5) .
N2 Pb1 2.587(3) 3_757
C1 C2 1.409(5) .
C1 C6 1.423(5) .
C2 C3 1.389(6) .
C2 C10 1.529(6) .
C3 C4 1.368(7) .
C3 H3A 0.9300 .
C4 C5 1.364(7) .
C4 H4A 0.9300 .
C5 C6 1.399(6) .
C5 H5A 0.9300 .
C6 C7 1.522(6) .
C7 C9 1.532(7) .
C7 C8 1.534(7) .
C7 H7A 0.9800 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 C12 1.523(6) .
C10 C11 1.534(7) .
C10 H10A 0.9800 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 C20 1.415(5) .
C15 C16 1.437(6) .
C16 C17 1.394(6) .
C16 C24 1.515(6) .
C17 C18 1.381(7) .
C17 H17A 0.9300 .
C18 C19 1.348(7) .
C18 H18A 0.9300 .
C19 C20 1.404(6) .
C19 H19A 0.9300 .
C20 C21 1.536(6) .
C21 C22 1.514(7) .
C21 C23 1.550(6) .
C21 H21A 0.9800 .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 C25 1.525(8) .
C24 C26 1.527(7) .
C24 H24A 0.9800 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C26 H26A 0.9600 .
C26 H26B 0.9600 .
C26 H26C 0.9600 .
