Low valent lead hydride chemistry: hydroplumbylation of phenylacetylene and 1,1-dimethylallene
Wesemann, Lars; Weiß, Sebastian; Schubert, Hartmut; Chemical Communications  (2019) –; doi:10.1039/C9CC05431F

data_7123935
_publ_section_title
;
 Low valent lead hydride chemistry: hydroplumbylation of phenylacetylene
 and 1,1-dimethylallene
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05431F
_journal_year                    2019
_chemical_formula_sum            'C41 H58 Pb'
_chemical_formula_weight         758.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-07-12 deposited with the CCDC.    2019-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                104.0660(10)
_cell_angle_beta                 102.0580(10)
_cell_angle_gamma                108.9560(10)
_cell_formula_units_Z            4
_cell_length_a                   14.0970(3)
_cell_length_b                   16.7228(4)
_cell_length_c                   17.7335(4)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.60
_cell_volume                     3641.58(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_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  0.0339
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            99884
_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         27.932
_diffrn_reflns_theta_min         1.247
_exptl_absorpt_coefficient_mu    4.658
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.193
_refine_diff_density_min         -1.418
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     852
_refine_ls_number_reflns         17385
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+15.6114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14036
_reflns_number_total             17385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05431f2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        3641.57(15)
_cod_database_code               7123935
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              35986