Aryldimethylelement cations of the heavier group 14 elements. An essentially three-coordinate plumbylium ion.
Janssen, Marvin; Mebs, Stefan; Beckmann, Jens; Chemical communications (Cambridge, England) 59 (2023) 7267–7270; doi:10.1039/d3cc00397c

data_7131669
_publ_section_title
;
 Aryldimethylelement cations of the heavier group 14 elements. An
 essentially three-coordinate plumbylium ion.
;
_journal_issue                   47
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7267
_journal_page_last               7270
_journal_paper_doi               10.1039/d3cc00397c
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C43 H42 Pb'
_chemical_formula_sum            'C43 H42 Pb'
_chemical_formula_weight         765.95
_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_date             2022-07-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-12-17 deposited with the CCDC.	2023-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                101.750(3)
_cell_angle_beta                 96.006(3)
_cell_angle_gamma                109.536(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1370(7)
_cell_length_b                   12.5545(9)
_cell_length_c                   15.8115(11)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      36.39
_cell_measurement_theta_min      2.25
_cell_volume                     1823.8(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            72038
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.466
_diffrn_reflns_theta_min         2.485
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.652
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0968 before and 0.0590 after correction.
The Ratio of minimum to maximum transmission is 0.6737.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.928
_refine_diff_density_min         -1.305
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.00136(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         17740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+1.0433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16293
_reflns_number_total             17740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00397c2.cif
_cod_data_source_block           janssenm220712_0m
_cod_depositor_comments
'Adding full bibliography for 7131666--7131671.cif.'
_cod_database_code               7131669
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C34(H34), C32(H32), C54(H54), C51(H51), C52(H52), C31(H31),
 C64(H64), C42(H42), C53(H53), C13(H13), C41(H41), C43(H43), C61(H61), C44(H44),
  C63(H63), C62(H62)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C21(H21A,H21B,H21C), C3(H3A,H3B,H3C),
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C20(H20A,H20B,H20C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25938
_shelx_hkl_checksum              92351
_shelx_fab_checksum              92954
_olex2_submission_special_instructions 'No special instructions were received'