#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:44:06 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178579 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/89/4068930.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_4068930
loop_
_publ_author_name
'Jana, Anukul'
'Sarish, Sankaranarayana Pillai'
'Roesky, Herbert W.'
'Schulzke, Carola'
'Döring, Alexander'
'John, Michael'
_publ_section_title
;
 Facile Access of Well-Defined Stable Divalent Lead Compounds with Small
 Organic Substituents
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2563
_journal_paper_doi               10.1021/om801167c
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C30 H44 N2 Pb'
_chemical_formula_weight         639.86
_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                90.45(3)
_cell_angle_beta                 107.02(3)
_cell_angle_gamma                108.52(3)
_cell_formula_units_Z            2
_cell_length_a                   10.439(2)
_cell_length_b                   11.973(2)
_cell_length_c                   12.424(3)
_cell_measurement_reflns_used    12613
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      53.9
_cell_measurement_theta_min      3.4
_cell_volume                     1399.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  IPDSII
_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  0.0669
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12613
_diffrn_reflns_theta_full        26.96
_diffrn_reflns_theta_max         26.96
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    6.048
_exptl_absorpt_correction_T_max  0.9441
_exptl_absorpt_correction_T_min  0.1913
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.935
_refine_diff_density_min         -1.668
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         6022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0542P)²+0.6267P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                5740
_reflns_number_total             6022
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801167c_si_001.cif
_cod_data_source_block           ja8
_cod_original_cell_volume        1399.2(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068930
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
Pb1 Pb 0.429873(12) 0.334692(10) 0.387401(9) 0.01782(6) Uani 1 1 d .
N1 N 0.3376(3) 0.2192(3) 0.5164(2) 0.0163(5) Uani 1 1 d .
N2 N 0.2335(3) 0.1944(3) 0.2579(2) 0.0151(5) Uani 1 1 d .
C1 C 0.5672(4) 0.2173(4) 0.3895(4) 0.0286(8) Uani 1 1 d .
H1A H 0.5088 0.1338 0.3831 0.046(3) Uiso 1 1 calc R
H1B H 0.6458 0.2374 0.4607 0.046(3) Uiso 1 1 calc R
H1C H 0.6054 0.2307 0.3257 0.046(3) Uiso 1 1 calc R
C2 C 0.3800(4) 0.2857(3) 0.6242(3) 0.0163(6) Uani 1 1 d .
C3 C 0.3008(4) 0.3566(3) 0.6411(3) 0.0175(7) Uani 1 1 d .
C4 C 0.3523(4) 0.4328(3) 0.7412(3) 0.0215(7) Uani 1 1 d .
H4 H 0.3000 0.4809 0.7536 0.026(5) Uiso 1 1 calc R
C5 C 0.4793(4) 0.4395(4) 0.8234(3) 0.0253(8) Uani 1 1 d .
H5 H 0.5139 0.4928 0.8905 0.026(5) Uiso 1 1 calc R
C6 C 0.5542(4) 0.3682(4) 0.8065(3) 0.0237(7) Uani 1 1 d .
H6 H 0.6406 0.3730 0.8627 0.026(5) Uiso 1 1 calc R
C7 C 0.5062(4) 0.2893(3) 0.7088(3) 0.0188(7) Uani 1 1 d .
C8 C 0.1631(4) 0.3510(3) 0.5523(3) 0.0189(7) Uani 1 1 d .
H8 H 0.1473 0.2940 0.4866 0.021(5) Uiso 1 1 calc R
C9 C 0.0362(4) 0.3049(4) 0.5980(4) 0.0295(8) Uani 1 1 d .
H9A H 0.0347 0.2293 0.6281 0.046(3) Uiso 1 1 calc R
H9B H -0.0524 0.2934 0.5365 0.046(3) Uiso 1 1 calc R
H9C H 0.0453 0.3627 0.6584 0.046(3) Uiso 1 1 calc R
C10 C 0.1718(4) 0.4715(4) 0.5097(4) 0.0255(8) Uani 1 1 d .
H10A H 0.1970 0.5308 0.5739 0.046(3) Uiso 1 1 calc R
H10B H 0.0796 0.4666 0.4564 0.046(3) Uiso 1 1 calc R
H10C H 0.2446 0.4944 0.4713 0.046(3) Uiso 1 1 calc R
C11 C 0.5896(4) 0.2087(3) 0.6959(3) 0.0225(7) Uani 1 1 d .
H11 H 0.5431 0.1624 0.6193 0.021(5) Uiso 1 1 calc R
C12 C 0.7437(4) 0.2790(4) 0.7062(4) 0.0293(9) Uani 1 1 d .
H12A H 0.7460 0.3384 0.6524 0.046(3) Uiso 1 1 calc R
H12B H 0.7906 0.2250 0.6894 0.046(3) Uiso 1 1 calc R
H12C H 0.7935 0.3186 0.7835 0.046(3) Uiso 1 1 calc R
C13 C 0.5881(5) 0.1210(4) 0.7856(4) 0.0296(9) Uani 1 1 d .
H13A H 0.6388 0.1647 0.8611 0.046(3) Uiso 1 1 calc R
H13B H 0.6350 0.0657 0.7719 0.046(3) Uiso 1 1 calc R
H13C H 0.4896 0.0768 0.7810 0.046(3) Uiso 1 1 calc R
C14 C 0.2567(4) 0.1065(3) 0.4941(3) 0.0188(7) Uani 1 1 d .
C15 C 0.2169(5) 0.0374(4) 0.5877(4) 0.0274(8) Uani 1 1 d .
H15A H 0.2460 0.0918 0.6565 0.046(3) Uiso 1 1 calc R
H15B H 0.2651 -0.0216 0.6029 0.046(3) Uiso 1 1 calc R
H15C H 0.1138 -0.0028 0.5643 0.046(3) Uiso 1 1 calc R
C16 C 0.1979(4) 0.0432(3) 0.3847(3) 0.0193(7) Uani 1 1 d .
H16 H 0.1673 -0.0405 0.3839 0.040(15) Uiso 1 1 calc R
C17 C 0.1768(4) 0.0829(3) 0.2769(3) 0.0172(6) Uani 1 1 d .
C18 C 0.0793(4) -0.0084(3) 0.1783(4) 0.0232(8) Uani 1 1 d .
H18A H 0.0128 0.0247 0.1276 0.046(3) Uiso 1 1 calc R
H18B H 0.0260 -0.0787 0.2064 0.046(3) Uiso 1 1 calc R
H18C H 0.1359 -0.0307 0.1368 0.046(3) Uiso 1 1 calc R
C19 C 0.1906(4) 0.2335(3) 0.1487(3) 0.0166(6) Uani 1 1 d .
C20 C 0.0898(4) 0.2933(3) 0.1277(3) 0.0204(7) Uani 1 1 d .
C21 C 0.0558(5) 0.3381(4) 0.0239(4) 0.0259(8) Uani 1 1 d .
H21 H -0.0135 0.3764 0.0080 0.026(5) Uiso 1 1 calc R
C22 C 0.1205(4) 0.3281(4) -0.0569(3) 0.0266(8) Uani 1 1 d .
H22 H 0.0963 0.3600 -0.1268 0.026(5) Uiso 1 1 calc R
C23 C 0.2210(4) 0.2712(3) -0.0346(3) 0.0233(7) Uani 1 1 d .
H23 H 0.2657 0.2647 -0.0898 0.026(5) Uiso 1 1 calc R
C24 C 0.2573(4) 0.2236(3) 0.0673(3) 0.0188(7) Uani 1 1 d .
C25 C 0.0210(4) 0.3089(3) 0.2171(3) 0.0226(7) Uani 1 1 d .
H25 H 0.0978 0.3310 0.2919 0.021(5) Uiso 1 1 calc R
C26 C -0.0926(5) 0.1959(4) 0.2269(4) 0.0334(9) Uani 1 1 d .
H26A H -0.1679 0.1694 0.1539 0.046(3) Uiso 1 1 calc R
H26B H -0.1331 0.2115 0.2850 0.046(3) Uiso 1 1 calc R
H26C H -0.0500 0.1340 0.2481 0.046(3) Uiso 1 1 calc R
C27 C -0.0428(5) 0.4083(4) 0.1989(4) 0.0295(9) Uani 1 1 d .
H27A H -0.1244 0.3863 0.1296 0.046(3) Uiso 1 1 calc R
H27B H 0.0290 0.4814 0.1917 0.046(3) Uiso 1 1 calc R
H27C H -0.0741 0.4209 0.2637 0.046(3) Uiso 1 1 calc R
C28 C 0.3680(4) 0.1619(3) 0.0854(3) 0.0203(7) Uani 1 1 d .
H28 H 0.3773 0.1292 0.1600 0.021(5) Uiso 1 1 calc R
C29 C 0.5129(4) 0.2477(4) 0.0904(4) 0.0302(9) Uani 1 1 d .
H29A H 0.5065 0.2826 0.0187 0.046(3) Uiso 1 1 calc R
H29B H 0.5813 0.2051 0.1028 0.046(3) Uiso 1 1 calc R
H29C H 0.5446 0.3106 0.1527 0.046(3) Uiso 1 1 calc R
C30 C 0.3214(5) 0.0582(4) -0.0057(4) 0.0284(8) Uani 1 1 d .
H30A H 0.3153 0.0881 -0.0796 0.046(3) Uiso 1 1 calc R
H30B H 0.2280 0.0034 -0.0077 0.046(3) Uiso 1 1 calc R
H30C H 0.3908 0.0166 0.0117 0.046(3) 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'
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 Pb1 N2 91.04(13)
C1 Pb1 N1 88.33(13)
N2 Pb1 N1 81.44(10)
C14 N1 C2 123.2(3)
C14 N1 Pb1 125.2(2)
C2 N1 Pb1 111.6(2)
C17 N2 C19 121.7(3)
C17 N2 Pb1 124.0(2)
C19 N2 Pb1 113.7(2)
C7 C2 C3 120.5(3)
C7 C2 N1 120.6(3)
C3 C2 N1 118.7(3)
C4 C3 C2 118.6(3)
C4 C3 C8 120.5(3)
C2 C3 C8 120.9(3)
C5 C4 C3 121.2(3)
C6 C5 C4 119.5(4)
C5 C6 C7 121.5(3)
C6 C7 C2 118.6(3)
C6 C7 C11 119.6(3)
C2 C7 C11 121.7(3)
C3 C8 C10 111.2(3)
C3 C8 C9 111.2(3)
C10 C8 C9 110.6(3)
C7 C11 C12 112.0(3)
C7 C11 C13 110.7(3)
C12 C11 C13 108.8(3)
N1 C14 C16 124.2(3)
N1 C14 C15 120.4(3)
C16 C14 C15 115.4(3)
C17 C16 C14 131.0(3)
N2 C17 C16 124.4(3)
N2 C17 C18 119.3(3)
C16 C17 C18 116.3(3)
C24 C19 C20 120.2(3)
C24 C19 N2 120.8(3)
C20 C19 N2 118.8(3)
C21 C20 C19 118.4(3)
C21 C20 C25 120.9(3)
C19 C20 C25 120.7(3)
C22 C21 C20 121.7(3)
C21 C22 C23 119.4(4)
C22 C23 C24 121.0(4)
C23 C24 C19 119.2(3)
C23 C24 C28 118.0(3)
C19 C24 C28 122.8(3)
C26 C25 C27 108.6(3)
C26 C25 C20 113.2(3)
C27 C25 C20 113.2(3)
C29 C28 C24 111.8(3)
C29 C28 C30 110.3(3)
C24 C28 C30 111.5(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pb1 C1 2.300(4)
Pb1 N2 2.335(3)
Pb1 N1 2.345(3)
N1 C14 1.321(5)
N1 C2 1.428(5)
N2 C17 1.332(5)
N2 C19 1.430(4)
C2 C7 1.412(5)
C2 C3 1.411(5)
C3 C4 1.395(5)
C3 C8 1.516(5)
C4 C5 1.394(6)
C5 C6 1.380(5)
C6 C7 1.394(5)
C7 C11 1.525(5)
C8 C10 1.525(5)
C8 C9 1.537(5)
C11 C12 1.527(5)
C11 C13 1.536(5)
C14 C16 1.414(5)
C14 C15 1.513(5)
C16 C17 1.404(5)
C17 C18 1.509(5)
C19 C24 1.409(5)
C19 C20 1.417(5)
C20 C21 1.393(6)
C20 C25 1.528(5)
C21 C22 1.387(6)
C22 C23 1.388(5)
C23 C24 1.393(5)
C24 C28 1.524(5)
C25 C26 1.523(6)
C25 C27 1.527(5)
C28 C29 1.518(6)
C28 C30 1.527(5)
