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_7131666
_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         'C42 H41 Si'
_chemical_formula_sum            'C42 H41 Si'
_chemical_formula_weight         573.84
_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   mixed
_atom_sites_solution_primary     dual
_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                70.660(3)
_cell_angle_beta                 80.850(2)
_cell_angle_gamma                74.740(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5487(5)
_cell_length_b                   11.5708(7)
_cell_length_c                   15.9662(11)
_cell_measurement_reflns_used    9757
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      33.15
_cell_measurement_theta_min      2.22
_cell_volume                     1600.80(17)
_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 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.0510
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            70612
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.223
_diffrn_reflns_theta_min         1.915
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1132 before and 0.0537 after correction.
The Ratio of minimum to maximum transmission is 0.9645.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       block
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         12194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0706P)^2^+0.9195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9222
_reflns_number_total             12194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00397c2.cif
_cod_data_source_block           janssenm220613_0m
_cod_depositor_comments
'Adding full bibliography for 7131666--7131671.cif.'
_cod_database_code               7131666
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.990
_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. Others
 Fixed Sof: C1A(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5) C2(0.5) H2A(0.5)
 H2B(0.5) H2C(0.5) C1(0.5) H1AA(0.5) H1(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C22(H22A,H22B)
3.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C54(H54), C53(H53), C51(H51), C13(H13), C64(H64), C44(H44),
 C34(H34), C43(H43), C52(H52), C32(H32), C61(H61), C41(H41), C33(H33), C42(H42),
  C63(H63), C62(H62)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C25(H25A,H25B,H25C), C24(H24A,H24B,
 H24C), C2A(H2AA,H2AB,H2AC), C2(H2A,H2B,H2C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24550
_shelx_hkl_checksum              85350
_olex2_submission_special_instructions 'No special instructions were received'