#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/00/7010036.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_7010036
loop_
_publ_author_name
'Gehrhus, Barbara'
'Hitchcock, Peter B.'
'Lappert, Michael F.'
_publ_section_title
;
 Crystalline (NN)C--M(NN) complexes: synthesis, structure, bonding and
 lability [M = Si, Ge, Sn or Pb;
 (NN) = 1,2-(ButCH2N)2C6H4]
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3094
_journal_paper_doi               10.1039/b005216g
_journal_year                    2000
_chemical_formula_sum            'C33 H52 N4 Pb'
_chemical_formula_weight         711.98
_chemical_name_common            '[C6H4(NCH2tBu)2CPb(NCH2tBu)2C6H4]'
_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                 102.61(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.421(4)
_cell_length_b                   16.015(4)
_cell_length_c                   20.254(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     3299(2)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'ORTEP3 for Windows'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_method       ω--2θ
_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  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0821
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6112
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    5.140
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       0.00019(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   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0206P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                4274
_reflns_number_total             5784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005216g.txt
_cod_data_source_block           GERHUS-HITCHCOCK-LAPPERT-11
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010036
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb 0.59140(3) 0.546054(17) 0.251867(13) 0.01806(9) Uani 1 1 d . . .
N1 N 0.9322(5) 0.6027(3) 0.3040(3) 0.0184(13) Uani 1 1 d . . .
N2 N 0.8927(5) 0.5339(3) 0.2102(3) 0.0195(13) Uani 1 1 d . . .
N3 N 0.6085(5) 0.5584(4) 0.3625(3) 0.0198(13) Uani 1 1 d . . .
N4 N 0.5149(6) 0.6701(3) 0.2617(3) 0.0203(13) Uani 1 1 d . . .
C1 C 0.8333(7) 0.5810(4) 0.2511(3) 0.0189(15) Uani 1 1 d . . .
C2 C 1.0263(7) 0.5251(4) 0.2382(4) 0.0217(17) Uani 1 1 d . . .
C3 C 1.0524(7) 0.5688(4) 0.2989(4) 0.0230(17) Uani 1 1 d . . .
C4 C 1.1761(7) 0.5706(5) 0.3413(4) 0.0304(19) Uani 1 1 d . . .
H4 H 1.1935 0.6018 0.3822 0.036 Uiso 1 1 calc R . .
C5 C 1.2729(7) 0.5245(5) 0.3211(4) 0.033(2) Uani 1 1 d . . .
H5 H 1.3582 0.5224 0.3498 0.040 Uiso 1 1 calc R . .
C6 C 1.2494(7) 0.4808(4) 0.2599(4) 0.0270(18) Uani 1 1 d . . .
H6 H 1.3191 0.4508 0.2473 0.032 Uiso 1 1 calc R . .
C7 C 1.1262(7) 0.4806(4) 0.2175(4) 0.0256(18) Uani 1 1 d . . .
H7 H 1.1099 0.4514 0.1756 0.031 Uiso 1 1 calc R . .
C8 C 0.9111(7) 0.6526(4) 0.3619(3) 0.0241(17) Uani 1 1 d . . .
H8A H 0.9731 0.6328 0.4031 0.029 Uiso 1 1 calc R . .
H8B H 0.8210 0.6415 0.3681 0.029 Uiso 1 1 calc R . .
C9 C 0.9280(7) 0.7472(4) 0.3565(4) 0.0246(17) Uani 1 1 d . . .
C10 C 0.9004(9) 0.7862(5) 0.4218(4) 0.042(2) Uani 1 1 d . . .
H10A H 0.9108 0.8469 0.4204 0.063 Uiso 1 1 calc R . .
H10B H 0.9625 0.7636 0.4612 0.063 Uiso 1 1 calc R . .
H10C H 0.8104 0.7728 0.4253 0.063 Uiso 1 1 calc R . .
C11 C 0.8286(8) 0.7818(5) 0.2961(4) 0.040(2) Uani 1 1 d . . .
H11A H 0.8407 0.8422 0.2932 0.060 Uiso 1 1 calc R . .
H11B H 0.7394 0.7701 0.3018 0.060 Uiso 1 1 calc R . .
H11C H 0.8419 0.7552 0.2545 0.060 Uiso 1 1 calc R . .
C12 C 1.0683(8) 0.7707(5) 0.3511(5) 0.046(2) Uani 1 1 d . . .
H12A H 1.0753 0.8316 0.3479 0.069 Uiso 1 1 calc R . .
H12B H 1.0882 0.7448 0.3107 0.069 Uiso 1 1 calc R . .
H12C H 1.1310 0.7508 0.3914 0.069 Uiso 1 1 calc R . .
C13 C 0.8260(7) 0.4966(4) 0.1461(3) 0.0222(16) Uani 1 1 d . . .
H13A H 0.7372 0.4789 0.1503 0.027 Uiso 1 1 calc R . .
H13B H 0.8748 0.4456 0.1386 0.027 Uiso 1 1 calc R . .
C14 C 0.8115(7) 0.5518(5) 0.0835(3) 0.0261(16) Uani 1 1 d . . .
C15 C 0.7467(9) 0.4978(6) 0.0227(4) 0.048(2) Uani 1 1 d . . .
H15A H 0.8028 0.4496 0.0194 0.073 Uiso 1 1 calc R . .
H15B H 0.7352 0.5310 -0.0188 0.073 Uiso 1 1 calc R . .
H15C H 0.6607 0.4784 0.0286 0.073 Uiso 1 1 calc R . .
C16 C 0.7243(10) 0.6259(5) 0.0886(4) 0.053(3) Uani 1 1 d . . .
H16A H 0.6378 0.6062 0.0934 0.079 Uiso 1 1 calc R . .
H16B H 0.7142 0.6599 0.0475 0.079 Uiso 1 1 calc R . .
H16C H 0.7643 0.6597 0.1280 0.079 Uiso 1 1 calc R . .
C17 C 0.9462(9) 0.5800(6) 0.0752(4) 0.055(3) Uani 1 1 d . . .
H17A H 1.0007 0.5310 0.0718 0.083 Uiso 1 1 calc R . .
H17B H 0.9882 0.6136 0.1144 0.083 Uiso 1 1 calc R . .
H17C H 0.9365 0.6137 0.0340 0.083 Uiso 1 1 calc R . .
C18 C 0.5674(6) 0.6359(4) 0.3803(3) 0.0199(15) Uani 1 1 d . . .
C19 C 0.5162(7) 0.6937(4) 0.3281(3) 0.0184(15) Uani 1 1 d . . .
C20 C 0.4701(7) 0.7708(5) 0.3453(4) 0.0253(17) Uani 1 1 d . . .
H20 H 0.4341 0.8091 0.3103 0.030 Uiso 1 1 calc R . .
C21 C 0.4753(8) 0.7933(5) 0.4126(4) 0.032(2) Uani 1 1 d . . .
H21 H 0.4438 0.8462 0.4232 0.039 Uiso 1 1 calc R . .
C22 C 0.5270(7) 0.7374(5) 0.4633(4) 0.0307(19) Uani 1 1 d . . .
H22 H 0.5316 0.7520 0.5092 0.037 Uiso 1 1 calc R . .
C23 C 0.5717(7) 0.6610(5) 0.4476(3) 0.0262(17) Uani 1 1 d . . .
H23 H 0.6068 0.6235 0.4833 0.031 Uiso 1 1 calc R . .
C24 C 0.6636(7) 0.5041(5) 0.4185(4) 0.0272(18) Uani 1 1 d . . .
H24A H 0.5995 0.5004 0.4480 0.033 Uiso 1 1 calc R . .
H24B H 0.7435 0.5314 0.4452 0.033 Uiso 1 1 calc R . .
C25 C 0.7003(7) 0.4158(5) 0.4029(4) 0.0270(18) Uani 1 1 d . . .
C26 C 0.8107(7) 0.4126(5) 0.3623(4) 0.0329(19) Uani 1 1 d . . .
H26A H 0.8302 0.3543 0.3536 0.049 Uiso 1 1 calc R . .
H26B H 0.8900 0.4395 0.3885 0.049 Uiso 1 1 calc R . .
H26C H 0.7814 0.4419 0.3192 0.049 Uiso 1 1 calc R . .
C27 C 0.5792(8) 0.3663(5) 0.3662(4) 0.036(2) Uani 1 1 d . . .
H27A H 0.6058 0.3095 0.3571 0.055 Uiso 1 1 calc R . .
H27B H 0.5402 0.3940 0.3233 0.055 Uiso 1 1 calc R . .
H27C H 0.5144 0.3639 0.3947 0.055 Uiso 1 1 calc R . .
C28 C 0.7536(8) 0.3722(5) 0.4706(4) 0.038(2) Uani 1 1 d . . .
H28A H 0.7776 0.3145 0.4624 0.057 Uiso 1 1 calc R . .
H28B H 0.6859 0.3720 0.4974 0.057 Uiso 1 1 calc R . .
H28C H 0.8314 0.4020 0.4953 0.057 Uiso 1 1 calc R . .
C29 C 0.4888(7) 0.7303(4) 0.2080(3) 0.0211(16) Uani 1 1 d . . .
H29A H 0.5554 0.7229 0.1803 0.025 Uiso 1 1 calc R . .
H29B H 0.5018 0.7867 0.2284 0.025 Uiso 1 1 calc R . .
C30 C 0.3511(7) 0.7279(4) 0.1599(3) 0.0238(17) Uani 1 1 d . . .
C31 C 0.3427(8) 0.8006(5) 0.1102(4) 0.041(2) Uani 1 1 d . . .
H31A H 0.4128 0.7953 0.0851 0.061 Uiso 1 1 calc R . .
H31B H 0.3530 0.8534 0.1352 0.061 Uiso 1 1 calc R . .
H31C H 0.2570 0.7997 0.0785 0.061 Uiso 1 1 calc R . .
C32 C 0.3310(8) 0.6465(5) 0.1194(4) 0.0338(19) Uani 1 1 d . . .
H32A H 0.4003 0.6406 0.0939 0.051 Uiso 1 1 calc R . .
H32B H 0.2450 0.6475 0.0879 0.051 Uiso 1 1 calc R . .
H32C H 0.3347 0.5992 0.1504 0.051 Uiso 1 1 calc R . .
C33 C 0.2416(7) 0.7353(5) 0.1992(4) 0.0327(19) Uani 1 1 d . . .
H33A H 0.2529 0.7872 0.2255 0.049 Uiso 1 1 calc R . .
H33B H 0.2460 0.6875 0.2299 0.049 Uiso 1 1 calc R . .
H33C H 0.1560 0.7358 0.1674 0.049 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Pb N3 77.0(2) . . ?
N4 Pb C1 100.4(2) . . ?
N3 Pb C1 97.1(2) . . ?
C1 N1 C3 112.4(6) . . ?
C1 N1 C8 123.1(6) . . ?
C3 N1 C8 124.3(6) . . ?
C1 N2 C2 110.8(6) . . ?
C1 N2 C13 125.1(6) . . ?
C2 N2 C13 124.1(6) . . ?
C18 N3 C24 115.3(5) . . ?
C18 N3 Pb 112.4(4) . . ?
C24 N3 Pb 132.1(5) . . ?
C19 N4 C29 120.7(6) . . ?
C19 N4 Pb 114.3(4) . . ?
C29 N4 Pb 123.9(4) . . ?
N1 C1 N2 104.7(6) . . ?
N1 C1 Pb 128.5(4) . . ?
N2 C1 Pb 117.1(4) . . ?
N2 C2 C3 107.1(6) . . ?
N2 C2 C7 132.3(7) . . ?
C3 C2 C7 120.5(7) . . ?
C4 C3 C2 122.3(7) . . ?
C4 C3 N1 132.7(7) . . ?
C2 C3 N1 105.0(6) . . ?
C5 C4 C3 116.5(7) . . ?
C4 C5 C6 122.1(7) . . ?
C5 C6 C7 120.8(7) . . ?
C2 C7 C6 117.7(7) . . ?
N1 C8 C9 116.1(6) . . ?
C11 C9 C12 110.2(7) . . ?
C11 C9 C8 110.4(6) . . ?
C12 C9 C8 112.0(6) . . ?
C11 C9 C10 108.6(6) . . ?
C12 C9 C10 108.6(6) . . ?
C8 C9 C10 107.0(6) . . ?
N2 C13 C14 116.3(6) . . ?
C16 C14 C17 110.9(8) . . ?
C16 C14 C13 110.6(6) . . ?
C17 C14 C13 109.8(6) . . ?
C16 C14 C15 109.3(7) . . ?
C17 C14 C15 109.5(7) . . ?
C13 C14 C15 106.7(6) . . ?
N3 C18 C23 124.0(6) . . ?
N3 C18 C19 118.5(6) . . ?
C23 C18 C19 117.5(6) . . ?
N4 C19 C20 123.2(6) . . ?
N4 C19 C18 117.8(6) . . ?
C20 C19 C18 119.0(6) . . ?
C19 C20 C21 121.9(7) . . ?
C22 C21 C20 119.0(7) . . ?
C21 C22 C23 120.2(7) . . ?
C22 C23 C18 122.4(7) . . ?
N3 C24 C25 118.2(6) . . ?
C24 C25 C28 107.3(6) . . ?
C24 C25 C27 111.3(6) . . ?
C28 C25 C27 107.3(6) . . ?
C24 C25 C26 113.0(6) . . ?
C28 C25 C26 107.0(6) . . ?
C27 C25 C26 110.6(6) . . ?
N4 C29 C30 117.2(6) . . ?
C33 C30 C31 110.0(6) . . ?
C33 C30 C32 108.3(6) . . ?
C31 C30 C32 108.3(6) . . ?
C33 C30 C29 111.3(6) . . ?
C31 C30 C29 107.9(6) . . ?
C32 C30 C29 111.0(6) . . ?
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
Pb N4 2.167(5) . ?
Pb N3 2.218(5) . ?
Pb C1 2.586(7) . ?
N1 C1 1.360(8) . ?
N1 C3 1.389(9) . ?
N1 C8 1.474(8) . ?
N2 C1 1.364(8) . ?
N2 C2 1.391(9) . ?
N2 C13 1.460(8) . ?
N3 C18 1.386(9) . ?
N3 C24 1.445(9) . ?
N4 C19 1.393(8) . ?
N4 C29 1.435(8) . ?
C2 C3 1.390(10) . ?
C2 C7 1.399(9) . ?
C3 C4 1.385(10) . ?
C4 C5 1.382(10) . ?
C5 C6 1.398(10) . ?
C6 C7 1.380(10) . ?
C8 C9 1.532(10) . ?
C9 C11 1.524(10) . ?
C9 C12 1.537(10) . ?
C9 C10 1.546(10) . ?
C13 C14 1.524(10) . ?
C14 C16 1.512(11) . ?
C14 C17 1.519(10) . ?
C14 C15 1.536(10) . ?
C18 C23 1.412(9) . ?
C18 C19 1.419(9) . ?
C19 C20 1.397(10) . ?
C20 C21 1.399(10) . ?
C21 C22 1.379(10) . ?
C22 C23 1.372(10) . ?
C24 C25 1.517(10) . ?
C25 C28 1.531(10) . ?
C25 C27 1.538(10) . ?
C25 C26 1.554(10) . ?
C29 C30 1.549(10) . ?
C30 C33 1.532(10) . ?
C30 C31 1.528(10) . ?
C30 C32 1.531(10) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652728
