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_7710961
_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         'C11 H20 I2 N2 Pb, 2(C4 H8 O)'
_chemical_formula_sum            'C19 H36 I2 N2 O2 Pb'
_chemical_formula_weight         785.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_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            4
_cell_length_a                   17.8013(2)
_cell_length_b                   15.2125(2)
_cell_length_c                   9.05780(10)
_cell_measurement_reflns_used    9367
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.8650
_cell_measurement_theta_min      3.8550
_cell_volume                     2452.87(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 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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14002
_diffrn_reflns_point_group_measured_fraction_full 0.865
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         74.498
_diffrn_reflns_theta_min         3.822
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    33.248
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.471
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (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    2.127
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.641
_refine_diff_density_min         -2.464
_refine_diff_density_rms         0.251
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.522(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         4274
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+1.0368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.600
_reflns_Friedel_fraction_full    0.710
_reflns_Friedel_fraction_max     0.684
_reflns_number_gt                4099
_reflns_number_total             4274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02462d2.cif
_cod_data_source_block           compound_2
_cod_database_code               7710961
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.082
_shelx_res_checksum              19983