Structural characterization of surface immobilized platinum hydrides by sensitivity-enhanced <sup>195</sup>Pt solid state NMR spectroscopy and DFT calculations.
Atterberry, Benjamin A.; Wimmer, Erik J.; Klostermann, Sina; Frey, Wolfgang; Kästner, Johannes; Estes, Deven P.; Rossini, Aaron J.; Chemical science 16 (2025) 1271–1287; doi:10.1039/d4sc06450j

data_1573220
_publ_section_title
;
 Structural characterization of surface immobilized platinum hydrides by
 sensitivity-enhanced <sup>195</sup>Pt solid state NMR spectroscopy and
 DFT calculations.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              1271
_journal_page_last               1287
_journal_paper_doi               10.1039/d4sc06450j
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C26 H58 N P2 Pt, B F4'
_chemical_formula_sum            'C26 H58 B F4 N P2 Pt'
_chemical_formula_weight         728.57
_chemical_name_systematic        'Pt-H_PtBu3_2-CH3CN [BF3]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2jjpnf
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2024-03-12 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.461(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.585(2)
_cell_length_b                   12.110(3)
_cell_length_c                   29.773(6)
_cell_measurement_reflns_used    5278
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.392
_cell_measurement_theta_min      1.682
_cell_volume                     3095.2(12)
_computing_cell_refinement       'Bruker APEXII Software Suite, 2008'
_computing_data_collection       'Bruker APEXII Software Suite, 2008'
_computing_data_reduction        'Bruker APEXII Software Suite, 2008'
_computing_molecular_graphics    'SHELXTL-plus, XP (sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1200
_diffrn_reflns_av_unetI/netI     0.1473
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            28228
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.392
_diffrn_reflns_theta_min         1.682
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.677
_exptl_absorpt_correction_T_max  0.7365
_exptl_absorpt_correction_T_min  0.6496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.073
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.043
_refine_diff_density_max         5.440
_refine_diff_density_min         -3.319
_refine_diff_density_rms         0.284
_refine_ls_extinction_coef       0.0018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         7714
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.0863
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+97.6813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1980
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5278
_reflns_number_total             7714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06450j2.cif
_cod_data_source_block           Pt-H-PtBu3_2-CH3CN-BF4
_cod_depositor_comments
'Adding full bibliography for 1573220--1573222.cif.'
_cod_original_cell_volume        3095.2(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1573220
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.726
_shelx_estimated_absorpt_t_max   0.824
_shelx_res_checksum              94796