Low-Valent Lead Hydride and Its Extreme Low-Field (1)H NMR Chemical Shift.
Schneider, Julia; Sindlinger, Christian P.; Eichele, Klaus; Schubert, Hartmut; Wesemann, Lars; Journal of the American Chemical Society 139 (2017) 6542–6545; doi:10.1021/jacs.7b01856

data_4126116
_publ_section_title
;
 Low-Valent Lead Hydride and Its Extreme Low-Field (1)H NMR Chemical
 Shift.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6542
_journal_page_last               6545
_journal_paper_doi               10.1021/jacs.7b01856
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C39 H57 Pb'
_chemical_formula_weight         733.03
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
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_cell_angle_beta                 104.3560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   15.9523(4)
_cell_length_c                   16.9850(4)
_cell_measurement_reflns_used    7545
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.51
_cell_measurement_theta_min      3.39
_cell_volume                     3489.87(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_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  0.0429
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            67957
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.502
_diffrn_reflns_theta_min         1.778
_exptl_absorpt_coefficient_mu    4.858
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6117
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       prism
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.084
_refine_diff_density_max         3.601
_refine_diff_density_min         -1.330
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         11431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+3.1401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0616
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9178
_reflns_number_total             11431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b01856_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               4126116
_shelxl_version_number           2014-3
_shelx_res_checksum              45344
_shelx_hkl_checksum              6007