#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:24:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179749 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/45/7004572.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_7004572
loop_
_publ_author_name
'Charmant, Jonathan P. H.'
'Haddow, Mairi F.'
'Hahn, F. Ekkehardt'
'Heitmann, Dennis'
'Fröhlich, Roland'
'Mansell, Stephen M.'
'Russell, Christopher A.'
'Wass, Duncan F.'
_publ_section_title
;
 Syntheses and molecular structures of some saturated N-heterocyclic
 plumbylenes
;
_journal_issue                   43
_journal_name_full               'Dalton Transactions'
_journal_page_first              6055
_journal_page_last               6059
_journal_paper_doi               10.1039/b808717b
_journal_year                    2008
_chemical_formula_sum            'C40 H52 N4 Pb2'
_chemical_formula_weight         1003.24
_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                66.2800(10)
_cell_angle_beta                 74.3180(10)
_cell_angle_gamma                68.1540(10)
_cell_formula_units_Z            1
_cell_length_a                   8.7974(5)
_cell_length_b                   10.0046(6)
_cell_length_c                   11.9931(7)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     887.91(9)
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2000)'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10817
_diffrn_reflns_theta_full        31.59
_diffrn_reflns_theta_max         31.59
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    9.502
_exptl_absorpt_correction_T_max  0.7024
_exptl_absorpt_correction_T_min  0.3298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Corrections were done with the SADABS program, utilizing the none merged
raw data obtained from the integration process. Integration and final cell
refinement were done with SAINT.

SADABS reports ratio of Tmin/Tmax = 0.506270

;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.528
_refine_diff_density_min         -1.336
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         5519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0201
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0266P)²+0.7869P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0502
_reflns_number_gt                5123
_reflns_number_total             5519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b808717b.txt
_cod_data_source_block           plumbylene-2
_cod_database_code               7004572
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
C1 C 0.0781(3) -0.2913(3) 0.1398(2) 0.0181(5) Uani 1 1 d . . .
H1A H 0.0029 -0.3191 0.2177 0.022 Uiso 1 1 calc R . .
H1B H 0.1879 -0.3689 0.1496 0.022 Uiso 1 1 calc R . .
C2 C 0.1860(3) -0.1428(3) 0.2000(2) 0.0147(4) Uani 1 1 d . . .
C3 C 0.1056(3) -0.1159(3) 0.3114(2) 0.0162(5) Uani 1 1 d . . .
C4 C 0.1933(3) -0.1035(3) 0.3851(3) 0.0197(5) Uani 1 1 d . . .
H4 H 0.1362 -0.0821 0.4584 0.024 Uiso 1 1 calc R . .
C5 C 0.3619(3) -0.1214(3) 0.3552(3) 0.0205(5) Uani 1 1 d . . .
C6 C 0.4423(3) -0.1637(3) 0.2535(3) 0.0212(5) Uani 1 1 d . . .
H6 H 0.5591 -0.1849 0.2352 0.025 Uiso 1 1 calc R . .
C7 C 0.3594(3) -0.1766(3) 0.1764(2) 0.0188(5) Uani 1 1 d . . .
C8 C -0.0750(3) -0.1028(3) 0.3592(3) 0.0214(5) Uani 1 1 d . . .
H8A H -0.0906 -0.1424 0.4494 0.032 Uiso 1 1 calc R . .
H8B H -0.1103 -0.1622 0.3286 0.032 Uiso 1 1 calc R . .
H8C H -0.1413 0.0049 0.3307 0.032 Uiso 1 1 calc R . .
C9 C 0.4511(4) -0.0966(4) 0.4325(3) 0.0282(6) Uani 1 1 d . . .
H9A H 0.5708 -0.1347 0.4091 0.042 Uiso 1 1 calc R . .
H9B H 0.4211 -0.1519 0.5195 0.042 Uiso 1 1 calc R . .
H9C H 0.4196 0.0129 0.4193 0.042 Uiso 1 1 calc R . .
C10 C 0.4670(4) -0.2343(4) 0.0730(3) 0.0268(6) Uani 1 1 d . . .
H10A H 0.4914 -0.1482 0.0022 0.040 Uiso 1 1 calc R . .
H10B H 0.4085 -0.2828 0.0491 0.040 Uiso 1 1 calc R . .
H10C H 0.5707 -0.3092 0.1011 0.040 Uiso 1 1 calc R . .
C11 C -0.0111(3) 0.2909(3) -0.0355(2) 0.0178(5) Uani 1 1 d . . .
H11A H 0.1030 0.2204 -0.0305 0.021 Uiso 1 1 calc R . .
H11B H -0.0076 0.3948 -0.0514 0.021 Uiso 1 1 calc R . .
C12 C -0.1341(3) 0.2999(3) 0.1737(2) 0.0163(5) Uani 1 1 d . . .
C13 C -0.2945(3) 0.3520(3) 0.2345(3) 0.0189(5) Uani 1 1 d . . .
C14 C -0.3179(4) 0.4141(3) 0.3250(3) 0.0233(5) Uani 1 1 d . . .
H14 H -0.4271 0.4491 0.3640 0.028 Uiso 1 1 calc R . .
C15 C -0.1873(4) 0.4267(3) 0.3605(3) 0.0210(5) Uani 1 1 d . . .
C16 C -0.0306(4) 0.3722(3) 0.3028(3) 0.0191(5) Uani 1 1 d . . .
H16 H 0.0610 0.3774 0.3267 0.023 Uiso 1 1 calc R . .
C17 C -0.0003(3) 0.3097(3) 0.2110(2) 0.0171(5) Uani 1 1 d . . .
C18 C -0.4449(4) 0.3462(4) 0.2009(3) 0.0288(6) Uani 1 1 d . . .
H18A H -0.4461 0.2399 0.2306 0.043 Uiso 1 1 calc R . .
H18B H -0.4410 0.3883 0.1112 0.043 Uiso 1 1 calc R . .
H18C H -0.5452 0.4067 0.2389 0.043 Uiso 1 1 calc R . .
C19 C -0.2169(4) 0.4954(4) 0.4579(3) 0.0295(6) Uani 1 1 d . . .
H19A H -0.2268 0.4177 0.5394 0.044 Uiso 1 1 calc R . .
H19B H -0.3192 0.5811 0.4496 0.044 Uiso 1 1 calc R . .
H19C H -0.1238 0.5324 0.4484 0.044 Uiso 1 1 calc R . .
C20 C 0.1771(3) 0.2525(3) 0.1560(3) 0.0219(5) Uani 1 1 d . . .
H20A H 0.2005 0.3283 0.0761 0.033 Uiso 1 1 calc R . .
H20B H 0.1948 0.1557 0.1448 0.033 Uiso 1 1 calc R . .
H20C H 0.2513 0.2362 0.2113 0.033 Uiso 1 1 calc R . .
N1 N 0.0932(3) -0.1384(2) 0.1145(2) 0.0147(4) Uani 1 1 d . . .
N2 N -0.1163(3) 0.2423(3) 0.0799(2) 0.0172(4) Uani 1 1 d . . .
Pb1 Pb -0.187459(11) 0.045057(10) 0.096862(9) 0.01642(3) 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'
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
N1 C1 C11 110.6(2) . 2 ?
C7 C2 C3 117.4(2) . . ?
C7 C2 N1 121.5(2) . . ?
C3 C2 N1 121.1(2) . . ?
C4 C3 C2 120.2(2) . . ?
C4 C3 C8 116.1(2) . . ?
C2 C3 C8 123.6(2) . . ?
C3 C4 C5 122.0(3) . . ?
C6 C5 C4 117.2(3) . . ?
C6 C5 C9 122.1(3) . . ?
C4 C5 C9 120.7(3) . . ?
C5 C6 C7 122.6(3) . . ?
C6 C7 C2 119.8(2) . . ?
C6 C7 C10 116.1(2) . . ?
C2 C7 C10 124.0(2) . . ?
N2 C11 C1 109.7(2) . 2 ?
N2 C12 C13 118.6(2) . . ?
N2 C12 C17 123.9(2) . . ?
C13 C12 C17 117.5(2) . . ?
C14 C13 C12 120.4(3) . . ?
C14 C13 C18 118.3(3) . . ?
C12 C13 C18 121.3(2) . . ?
C13 C14 C15 122.4(3) . . ?
C16 C15 C14 116.8(2) . . ?
C16 C15 C19 122.1(3) . . ?
C14 C15 C19 121.1(3) . . ?
C15 C16 C17 123.1(3) . . ?
C16 C17 C12 119.7(2) . . ?
C16 C17 C20 118.0(2) . . ?
C12 C17 C20 122.3(2) . . ?
C2 N1 C1 111.7(2) . . ?
C2 N1 Pb1 117.82(16) . 2 ?
C1 N1 Pb1 106.54(15) . 2 ?
C2 N1 Pb1 118.03(15) . . ?
C1 N1 Pb1 106.94(16) . . ?
Pb1 N1 Pb1 93.90(7) 2 . ?
C12 N2 C11 119.7(2) . . ?
C12 N2 Pb1 127.21(17) . . ?
C11 N2 Pb1 111.80(15) . . ?
N2 Pb1 N1 77.28(8) . 2 ?
N2 Pb1 N1 95.43(8) . . ?
N1 Pb1 N1 86.10(7) 2 . ?
N2 Pb1 Pb1 85.38(6) . 2 ?
N1 Pb1 Pb1 44.40(5) 2 2 ?
N1 Pb1 Pb1 41.70(5) . 2 ?
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
C1 N1 1.485(3) . ?
C1 C11 1.518(4) 2 ?
C2 C7 1.407(4) . ?
C2 C3 1.412(4) . ?
C2 N1 1.452(3) . ?
C3 C4 1.386(4) . ?
C3 C8 1.511(4) . ?
C4 C5 1.389(4) . ?
C5 C6 1.376(4) . ?
C5 C9 1.503(4) . ?
C6 C7 1.391(4) . ?
C7 C10 1.517(4) . ?
C11 N2 1.453(3) . ?
C11 C1 1.518(4) 2 ?
C12 N2 1.408(3) . ?
C12 C13 1.413(4) . ?
C12 C17 1.414(4) . ?
C13 C14 1.390(4) . ?
C13 C18 1.510(4) . ?
C14 C15 1.390(4) . ?
C15 C16 1.381(4) . ?
C15 C19 1.502(4) . ?
C16 C17 1.394(4) . ?
C17 C20 1.511(4) . ?
N1 Pb1 2.350(2) 2 ?
N1 Pb1 2.471(2) . ?
N2 Pb1 2.203(2) . ?
Pb1 N1 2.350(2) 2 ?
Pb1 Pb1 3.5241(2) 2 ?
