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_7131667
_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 H39 Cl Sn, C7 H8'
_chemical_formula_sum            'C49 H47 Cl Sn'
_chemical_formula_weight         790.00
_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                82.746(2)
_cell_angle_beta                 81.826(2)
_cell_angle_gamma                70.414(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4150(6)
_cell_length_b                   13.8081(8)
_cell_length_c                   15.8413(10)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    103.74
_cell_measurement_theta_max      33.18
_cell_measurement_theta_min      2.53
_cell_volume                     1913.7(2)
_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)'
_diffrn_ambient_temperature      103.74
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0303
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            70341
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.215
_diffrn_reflns_theta_min         2.336
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1048 before and 0.0416 after correction.
The Ratio of minimum to maximum transmission is 0.9279.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         14692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0269P)^2^+0.9610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12033
_reflns_number_total             14692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00397c2.cif
_cod_data_source_block           janssenm220208_0m
_cod_depositor_comments
'Adding full bibliography for 7131666--7131671.cif.'
_cod_database_code               7131667
_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. Others
 Fixed Sof: Sn1(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C1A(0.5) H1AA(0.5)
 H1AB(0.5) H1AC(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) Sn1A(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:
 C62(H62), C44(H44), C33(H33), C61(H61), C34(H34), C51(H51), C32(H32),
 C41(H41), C63(H63), C31(H31), C53(H53), C54(H54), C74(H74), C73(H73), C13(H13),
  C42(H42), C52(H52), C71(H71), C72(H72), C64(H64), C75(H75), C43(H43)
3.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C76(H76A,H76B,H76C), C24(H24A,H24B,H24C), C20(H20A,H20B,
 H20C), C19(H19A,H19B,H19C), C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC), C2A(H2AA,
 H2AB,H2AC), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              92054
_shelx_hkl_checksum              57147
_olex2_submission_special_instructions 'No special instructions were received'