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_4126011
_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            'C43 H62 N2 Pb'
_chemical_formula_weight         814.13
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   mixed
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_cell_angle_beta                 77.4530(10)
_cell_angle_gamma                75.3800(10)
_cell_formula_units_Z            2
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_cell_length_c                   14.2456(4)
_cell_measurement_reflns_used    9239
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      2.48
_cell_volume                     2033.52(9)
_computing_cell_refinement       'APEX2 v2011.8-0 (Bruker AXS)'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0265
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_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
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_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
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_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
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_diffrn_reflns_theta_max         27.899
_diffrn_reflns_theta_min         2.102
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.177
_exptl_absorpt_correction_T_max  0.6044
_exptl_absorpt_correction_T_min  0.4560
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.140
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_refine_diff_density_max         0.690
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_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         9621
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0213
_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^)+(0.0206P)^2^+0.9975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0468
_refine_ls_wR_factor_ref         0.0476
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8992
_reflns_number_total             9621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b01856_si_002.cif
_cod_data_source_block           JS204_0m
_cod_depositor_comments          'Adding full bibliography for 4126011.cif.'
_cod_database_code               4126011
_shelx_estimated_absorpt_t_min   0.456
_shelx_estimated_absorpt_t_max   0.604
_shelxl_version_number           2014-3
_shelx_res_checksum              66223
_shelx_hkl_checksum              23941