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_1573222
_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         'C24 H55 P2 Pt, B F4, 2(C H2 Cl2)'
_chemical_formula_sum            'C26 H59 B Cl4 F4 P2 Pt'
_chemical_formula_weight         857.37
_chemical_name_systematic        'Pt-H_PtBu3_2 [BF3]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2jjpqh
_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                 96.6660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1587(3)
_cell_length_b                   19.7667(5)
_cell_length_c                   16.9439(5)
_cell_measurement_reflns_used    8774
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.305
_cell_measurement_theta_min      2.061
_cell_volume                     3712.06(18)
_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_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0259
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31125
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.305
_diffrn_reflns_theta_min         2.061
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.190
_exptl_absorpt_correction_T_max  0.7191
_exptl_absorpt_correction_T_min  0.4984
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS, Bruker, 2008'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       prism
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.124
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.502(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         9210
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0280P)^2^+1.1868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0523
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                8774
_reflns_number_total             9210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06450j2.cif
_cod_data_source_block           Pt-H-PtBu3_2-BF4
_cod_depositor_comments
'Adding full bibliography for 1573220--1573222.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1573222
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.430
_shelx_estimated_absorpt_t_max   0.625
_shelx_res_checksum              36996