Reversible PtII‒CH3 deuteration without methane loss: metal‒ligand cooperation vs. ligand-assisted PtII-protonation
Pal, Shrinwantu; Nozaki, Kyoko; Vedernikov, Andrei N.; Love, Jennifer A.; Chemical Science 12 (2021) 2960–2969; doi:10.1039/D0SC06518H

data_1559953
_publ_section_title
;
 Reversible PtII--CH3 deuteration without methane loss: metal--ligand
 cooperation vs. ligand-assisted PtII-protonation
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              2960
_journal_page_last               2969
_journal_paper_doi               10.1039/D0SC06518H
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C14 H19 N2 O2 Pt, C F3 O3 S'
_chemical_formula_sum            'C15 H19 F3 N2 O5 Pt S'
_chemical_formula_weight         591.47
_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     dual
_audit_creation_date             2020-06-08
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_audit_update_record
;
2020-09-04 deposited with the CCDC.	2021-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.717(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3867(2)
_cell_length_b                   13.3132(3)
_cell_length_c                   12.4183(2)
_cell_measurement_reflns_used    17474
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.3150
_cell_measurement_theta_min      2.8190
_cell_volume                     1880.42(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -93.00  47.00   0.50    0.50    --   -3.30  38.00 -92.00  280
  2  \w    -41.00   5.00   0.50    0.50    --    4.40  38.00 -92.00   92
  3  \w     28.00  89.00   0.50    0.50    --    4.40  28.00-150.00  122
  4  \w    -84.00  94.00   0.50    0.50    --    4.40  18.00   0.00  356
  5  \w    -79.00 -53.00   0.50    0.50    --    4.40  37.00  60.00   52
  6  \w    -18.00  12.00   0.50    0.50    --    4.40  28.00-150.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0315599000
_diffrn_orient_matrix_UB_12      0.0327990000
_diffrn_orient_matrix_UB_13      0.0331028000
_diffrn_orient_matrix_UB_21      0.0468818000
_diffrn_orient_matrix_UB_22      -0.0013923000
_diffrn_orient_matrix_UB_23      0.0396096000
_diffrn_orient_matrix_UB_31      0.0262857000
_diffrn_orient_matrix_UB_32      0.0419922000
_diffrn_orient_matrix_UB_33      -0.0246032000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30286
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.260
_diffrn_reflns_theta_min         2.244
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    7.631
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.72a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_recrystallization_method 'MeOH, THF, Et2O'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.870
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0028P)^2^+4.6063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0536
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4246
_reflns_number_total             4591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06518h2.cif
_cod_data_source_block           spz0208
_cod_depositor_comments          'Adding full bibliography for 1559953.cif.'
_cod_database_code               1559953
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C15H20N2O2Pt1
_chemical_oxdiff_usercomment     '0.4 x 0.1 x 0.1 colorless block'
_diffrn_oxdiff_digest_frames
;
011f59e626830665d3fbe21ee2504bead300041949a
;
_diffrn_oxdiff_digest_hkl
;
015eccad37c9978280ee9f4d2b0b5c06726d89
;
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
2. Others
 Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=Sof(Pt2)=1-FVAR(1)
 Sof(Pt1)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1)
3.a Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C13(H13D,H13E,H13F), C12(H12A,H12B,H12C), C12(H12D,H12E,
 H12F), C14(H14A,H14B,H14C), C14(H14D,H14E,H14F)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C2(H2A), C11(H11), C5(H5), C4(H4), C9(H9), C3(H3), C8(H8)
;
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.967
_oxdiff_exptl_absorpt_empirical_full_min 0.765