#------------------------------------------------------------------------------
#$Date: 2022-08-14 01:46:42 +0300 (Sun, 14 Aug 2022) $
#$Revision: 277242 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/09/7710964.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_7710964
loop_
_publ_author_name
'Radius, Udo'
'Philipp, Michael S. M.'
'Bertermann, Rüdiger'
_publ_section_title
;
 N-Heterocyclic Carbene and Cyclic (Alkyl)(amino)carbene Adducts of
 Plumbanes and Plumbylenes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02462D
_journal_year                    2022
_chemical_formula_moiety         'C23 H30 N2 Pb'
_chemical_formula_sum            'C23 H30 N2 Pb'
_chemical_formula_weight         541.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-07-28 deposited with the CCDC.	2022-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                107.157(2)
_cell_angle_beta                 91.178(2)
_cell_angle_gamma                109.297(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4065(2)
_cell_length_b                   9.8592(2)
_cell_length_c                   12.6428(4)
_cell_measurement_reflns_used    15720
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.1530
_cell_measurement_theta_min      3.7200
_cell_volume                     1048.29(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22043
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         77.773
_diffrn_reflns_theta_min         3.691
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    15.689
_exptl_absorpt_correction_T_max  0.640
_exptl_absorpt_correction_T_min  0.187
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.044
_refine_diff_density_max         1.441
_refine_diff_density_min         -1.475
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0408P)²+0.5244P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4226
_reflns_number_total             4381
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt02462d2.cif
_cod_data_source_block           compound_10
_cod_original_cell_volume        1048.28(5)
_cod_database_code               7710964
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.202
_shelx_estimated_absorpt_t_max   0.573
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb01 Pb 0.44635(2) 0.67999(2) 0.10357(2) 0.01727(6) Uani 1 1 d . . . . .
N002 N 0.1589(3) 0.4311(3) 0.1841(3) 0.0184(6) Uani 1 1 d . . . . .
N003 N 0.2950(3) 0.5943(3) 0.3367(3) 0.0177(6) Uani 1 1 d . . . . .
C004 C 0.1874(4) 0.4807(4) 0.3676(3) 0.0203(7) Uani 1 1 d . . . . .
C005 C 0.1778(4) 0.4731(5) 0.4834(3) 0.0247(8) Uani 1 1 d . . . . .
H00A H 0.119916 0.368906 0.480512 0.037 Uiso 1 1 calc R U . . .
H00B H 0.126827 0.541023 0.523837 0.037 Uiso 1 1 calc R U . . .
H00C H 0.280467 0.504392 0.522040 0.037 Uiso 1 1 calc R U . . .
C006 C 0.8626(5) 0.6445(5) 0.2716(4) 0.0290(8) Uani 1 1 d . . . . .
H006 H 0.899554 0.563991 0.264894 0.035 Uiso 1 1 calc R U . . .
C007 C 0.7516(4) 0.8771(4) 0.2903(3) 0.0218(7) Uani 1 1 d . . . . .
H007 H 0.715821 0.958335 0.296855 0.026 Uiso 1 1 calc R U . . .
C008 C 0.5408(4) 0.6843(4) 0.4561(3) 0.0247(7) Uani 1 1 d . . . . .
H00D H 0.567001 0.612977 0.394545 0.037 Uiso 1 1 calc R U . . .
H00E H 0.504225 0.636273 0.512828 0.037 Uiso 1 1 calc R U . . .
H00F H 0.631018 0.775216 0.489388 0.037 Uiso 1 1 calc R U . . .
C009 C 0.1008(4) 0.3782(4) 0.2713(3) 0.0195(7) Uani 1 1 d . . . . .
C00A C 0.4169(4) 0.7286(4) 0.4118(3) 0.0204(7) Uani 1 1 d . . . . .
H00G H 0.464883 0.793533 0.365382 0.025 Uiso 1 1 calc R U . . .
C00B C 0.1086(4) 0.3530(4) 0.0631(3) 0.0206(7) Uani 1 1 d . . . . .
H00H H 0.167057 0.424527 0.024229 0.025 Uiso 1 1 calc R U . . .
C00C C 0.3575(4) 0.8250(4) 0.5051(3) 0.0256(8) Uani 1 1 d . . . . .
H00I H 0.284106 0.857546 0.472623 0.038 Uiso 1 1 calc R U . . .
H00J H 0.442461 0.914407 0.550321 0.038 Uiso 1 1 calc R U . . .
H00K H 0.307831 0.765165 0.552317 0.038 Uiso 1 1 calc R U . . .
C00D C -0.0345(4) 0.2388(4) 0.2586(4) 0.0272(8) Uani 1 1 d . . . . .
H00L H -0.126474 0.253938 0.235203 0.041 Uiso 1 1 calc R U . . .
H00M H -0.043056 0.218976 0.330195 0.041 Uiso 1 1 calc R U . . .
H00N H -0.022390 0.152066 0.202156 0.041 Uiso 1 1 calc R U . . .
C00E C 0.9432(4) 0.7879(5) 0.3441(3) 0.0278(8) Uani 1 1 d . . . . .
H00O H 1.035842 0.806467 0.386905 0.033 Uiso 1 1 calc R U . . .
C00F C 0.3129(4) 0.9481(4) 0.2362(3) 0.0234(7) Uani 1 1 d . . . . .
H00P H 0.238897 0.870294 0.255930 0.028 Uiso 1 1 calc R U . . .
C00G C 0.6672(4) 0.7333(4) 0.2177(3) 0.0183(6) Uani 1 1 d . . . . .
C00H C 0.8875(4) 0.9047(4) 0.3538(3) 0.0262(8) Uani 1 1 d . . . . .
H00Q H 0.942007 1.003477 0.403585 0.031 Uiso 1 1 calc R U . . .
C00I C 0.1510(5) 0.2112(4) 0.0216(4) 0.0286(8) Uani 1 1 d . . . . .
H00R H 0.124896 0.167747 -0.059721 0.043 Uiso 1 1 calc R U . . .
H00S H 0.095021 0.136583 0.056561 0.043 Uiso 1 1 calc R U . . .
H00T H 0.260432 0.238392 0.041224 0.043 Uiso 1 1 calc R U . . .
C00J C -0.0589(4) 0.3231(5) 0.0317(4) 0.0318(9) Uani 1 1 d . . . . .
H00U H -0.080965 0.295622 -0.049532 0.048 Uiso 1 1 calc R U . . .
H00V H -0.081691 0.414714 0.067931 0.048 Uiso 1 1 calc R U . . .
H00W H -0.121547 0.239696 0.056401 0.048 Uiso 1 1 calc R U . . .
C00K C 0.5377(4) 1.0367(4) 0.1543(3) 0.0240(7) Uani 1 1 d . . . . .
H00X H 0.618997 1.019224 0.115931 0.029 Uiso 1 1 calc R U . . .
C00L C 0.7268(4) 0.6176(4) 0.2081(3) 0.0250(7) Uani 1 1 d . . . . .
H00Y H 0.673840 0.519084 0.157321 0.030 Uiso 1 1 calc R U . . .
C00M C 0.2797(4) 0.5634(4) 0.2241(3) 0.0178(6) Uani 1 1 d . . . . .
C00N C 0.3022(5) 1.0926(5) 0.2634(3) 0.0289(8) Uani 1 1 d . . . . .
H00Z H 0.219233 1.110169 0.299297 0.035 Uiso 1 1 calc R U . . .
C00O C 0.4310(4) 0.9166(4) 0.1803(3) 0.0191(7) Uani 1 1 d . . . . .
C00P C 0.4088(5) 1.2086(5) 0.2394(4) 0.0310(9) Uani 1 1 d . . . . .
H010 H 0.402221 1.306887 0.260640 0.037 Uiso 1 1 calc R U . . .
C00Q C 0.5274(5) 1.1808(4) 0.1832(4) 0.0304(9) Uani 1 1 d . . . . .
H011 H 0.601234 1.259958 0.164660 0.036 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 '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
C00O Pb01 C00G 94.62(12) . . ?
C00O Pb01 C00M 95.15(12) . . ?
C00G Pb01 C00M 93.68(11) . . ?
C00M N002 C009 110.9(3) . . ?
C00M N002 C00B 122.3(3) . . ?
C009 N002 C00B 126.7(3) . . ?
C00M N003 C004 111.3(3) . . ?
C00M N003 C00A 122.1(3) . . ?
C004 N003 C00A 126.6(3) . . ?
C009 C004 N003 106.3(3) . . ?
C009 C004 C005 128.1(3) . . ?
N003 C004 C005 125.6(3) . . ?
C004 C005 H00A 109.5 . . ?
C004 C005 H00B 109.5 . . ?
H00A C005 H00B 109.5 . . ?
C004 C005 H00C 109.5 . . ?
H00A C005 H00C 109.5 . . ?
H00B C005 H00C 109.5 . . ?
C00E C006 C00L 120.2(3) . . ?
C00E C006 H006 119.9 . . ?
C00L C006 H006 119.9 . . ?
C00G C007 C00H 121.7(3) . . ?
C00G C007 H007 119.2 . . ?
C00H C007 H007 119.2 . . ?
C00A C008 H00D 109.5 . . ?
C00A C008 H00E 109.5 . . ?
H00D C008 H00E 109.5 . . ?
C00A C008 H00F 109.5 . . ?
H00D C008 H00F 109.5 . . ?
H00E C008 H00F 109.5 . . ?
C004 C009 N002 106.7(3) . . ?
C004 C009 C00D 127.8(3) . . ?
N002 C009 C00D 125.5(3) . . ?
N003 C00A C008 111.2(3) . . ?
N003 C00A C00C 113.0(3) . . ?
C008 C00A C00C 112.3(3) . . ?
N003 C00A H00G 106.6 . . ?
C008 C00A H00G 106.6 . . ?
C00C C00A H00G 106.6 . . ?
N002 C00B C00J 112.3(3) . . ?
N002 C00B C00I 111.5(3) . . ?
C00J C00B C00I 113.3(3) . . ?
N002 C00B H00H 106.4 . . ?
C00J C00B H00H 106.4 . . ?
C00I C00B H00H 106.4 . . ?
C00A C00C H00I 109.5 . . ?
C00A C00C H00J 109.5 . . ?
H00I C00C H00J 109.5 . . ?
C00A C00C H00K 109.5 . . ?
H00I C00C H00K 109.5 . . ?
H00J C00C H00K 109.5 . . ?
C009 C00D H00L 109.5 . . ?
C009 C00D H00M 109.5 . . ?
H00L C00D H00M 109.5 . . ?
C009 C00D H00N 109.5 . . ?
H00L C00D H00N 109.5 . . ?
H00M C00D H00N 109.5 . . ?
C006 C00E C00H 119.4(3) . . ?
C006 C00E H00O 120.3 . . ?
C00H C00E H00O 120.3 . . ?
C00O C00F C00N 121.0(4) . . ?
C00O C00F H00P 119.5 . . ?
C00N C00F H00P 119.5 . . ?
C007 C00G C00L 117.2(3) . . ?
C007 C00G Pb01 123.9(2) . . ?
C00L C00G Pb01 118.7(3) . . ?
C00E C00H C007 120.1(4) . . ?
C00E C00H H00Q 120.0 . . ?
C007 C00H H00Q 120.0 . . ?
C00B C00I H00R 109.5 . . ?
C00B C00I H00S 109.5 . . ?
H00R C00I H00S 109.5 . . ?
C00B C00I H00T 109.5 . . ?
H00R C00I H00T 109.5 . . ?
H00S C00I H00T 109.5 . . ?
C00B C00J H00U 109.5 . . ?
C00B C00J H00V 109.5 . . ?
H00U C00J H00V 109.5 . . ?
C00B C00J H00W 109.5 . . ?
H00U C00J H00W 109.5 . . ?
H00V C00J H00W 109.5 . . ?
C00Q C00K C00O 121.8(4) . . ?
C00Q C00K H00X 119.1 . . ?
C00O C00K H00X 119.1 . . ?
C006 C00L C00G 121.3(4) . . ?
C006 C00L H00Y 119.3 . . ?
C00G C00L H00Y 119.3 . . ?
N003 C00M N002 104.9(3) . . ?
N003 C00M Pb01 131.0(2) . . ?
N002 C00M Pb01 123.3(2) . . ?
C00P C00N C00F 121.2(4) . . ?
C00P C00N H00Z 119.4 . . ?
C00F C00N H00Z 119.4 . . ?
C00F C00O C00K 116.8(3) . . ?
C00F C00O Pb01 125.9(3) . . ?
C00K C00O Pb01 116.6(2) . . ?
C00N C00P C00Q 119.2(4) . . ?
C00N C00P H010 120.4 . . ?
C00Q C00P H010 120.4 . . ?
C00P C00Q C00K 120.0(4) . . ?
C00P C00Q H011 120.0 . . ?
C00K C00Q H011 120.0 . . ?
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
Pb01 C00O 2.302(3) . ?
Pb01 C00G 2.320(3) . ?
Pb01 C00M 2.457(3) . ?
N002 C00M 1.362(4) . ?
N002 C009 1.401(5) . ?
N002 C00B 1.480(5) . ?
N003 C00M 1.359(5) . ?
N003 C004 1.399(4) . ?
N003 C00A 1.476(4) . ?
C004 C009 1.363(5) . ?
C004 C005 1.491(5) . ?
C005 H00A 0.9800 . ?
C005 H00B 0.9800 . ?
C005 H00C 0.9800 . ?
C006 C00E 1.383(6) . ?
C006 C00L 1.397(6) . ?
C006 H006 0.9500 . ?
C007 C00G 1.393(5) . ?
C007 C00H 1.397(5) . ?
C007 H007 0.9500 . ?
C008 C00A 1.522(5) . ?
C008 H00D 0.9800 . ?
C008 H00E 0.9800 . ?
C008 H00F 0.9800 . ?
C009 C00D 1.496(5) . ?
C00A C00C 1.524(5) . ?
C00A H00G 1.0000 . ?
C00B C00J 1.524(5) . ?
C00B C00I 1.528(5) . ?
C00B H00H 1.0000 . ?
C00C H00I 0.9800 . ?
C00C H00J 0.9800 . ?
C00C H00K 0.9800 . ?
C00D H00L 0.9800 . ?
C00D H00M 0.9800 . ?
C00D H00N 0.9800 . ?
C00E C00H 1.391(6) . ?
C00E H00O 0.9500 . ?
C00F C00O 1.400(5) . ?
C00F C00N 1.402(5) . ?
C00F H00P 0.9500 . ?
C00G C00L 1.406(5) . ?
C00H H00Q 0.9500 . ?
C00I H00R 0.9800 . ?
C00I H00S 0.9800 . ?
C00I H00T 0.9800 . ?
C00J H00U 0.9800 . ?
C00J H00V 0.9800 . ?
C00J H00W 0.9800 . ?
C00K C00Q 1.396(5) . ?
C00K C00O 1.405(5) . ?
C00K H00X 0.9500 . ?
C00L H00Y 0.9500 . ?
C00N C00P 1.366(6) . ?
C00N H00Z 0.9500 . ?
C00P C00Q 1.394(6) . ?
C00P H010 0.9500 . ?
C00Q H011 0.9500 . ?
