N-Heterocyclic Carbene and Cyclic (Alkyl)(amino)carbene Adducts of Plumbanes and Plumbylenes
Radius, Udo; Philipp, Michael S. M.; Bertermann, Rüdiger; Dalton Transactions  (2022) –; doi:10.1039/D2DT02462D

data_7710966
_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         'C19 H22 N2 Pb'
_chemical_formula_sum            'C19 H22 N2 Pb'
_chemical_formula_weight         485.57
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   11.7933(3)
_cell_length_b                   15.7809(3)
_cell_length_c                   37.6134(8)
_cell_measurement_reflns_used    22815
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.5580
_cell_measurement_theta_min      2.1530
_cell_volume                     7000.2(3)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0911
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            74240
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.142
_diffrn_reflns_theta_min         2.038
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    9.639
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.402
_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    1.843
_exptl_crystal_description       plate
_exptl_crystal_F_000             3712
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.957
_refine_diff_density_min         -2.066
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         13342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0560
_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/[\s^2^(Fo^2^)+(0.0001P)^2^+39.0066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9860
_reflns_number_total             13342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02462d2.cif
_cod_data_source_block           compound_9
_cod_database_code               7710966
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.276
_shelx_estimated_absorpt_t_max   0.699
_shelx_res_checksum              76214