Hydration of Cyanohydrins by Highly Active Cationic Pt Catalysts: Mechanism and Scope
Li, Chengcheng; Chang, Xiao-Yong; Huo, Luqiong; Tan, Haibo; Xing, Xiangyou; Xu, Chen; ACS Catalysis 11 (2021) 8716–8726; doi:10.1021/acscatal.1c02254

data_4518850
_publ_section_title
;
 Hydration of Cyanohydrins by Highly Active Cationic Pt Catalysts:
 Mechanism and Scope
;
_journal_issue                   14
_journal_name_full               'ACS Catalysis'
_journal_page_first              8716
_journal_page_last               8726
_journal_paper_doi               10.1021/acscatal.1c02254
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety
'C43 H39 Fe I N O P3 Pt, 2(C F3 O3 S), 1.5(C7 H8)'
_chemical_formula_sum            'C55.5 H51 F6 Fe I N O7 P3 Pt S2'
_chemical_formula_weight         1492.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                89.708(3)
_cell_angle_beta                 73.604(3)
_cell_angle_gamma                66.285(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0101(7)
_cell_length_b                   13.0185(8)
_cell_length_c                   20.5982(12)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      68.497
_cell_measurement_theta_min      2.253
_cell_volume                     2807.1(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'Bruker PHOTON 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CMOS area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44392
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.497
_diffrn_reflns_theta_min         2.253
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.11
_diffrn_source_power             0.0555
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    13.109
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.3264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1467 before and 0.0937 after correction.
The Ratio of minimum to maximum transmission is 0.4334.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       block
_exptl_crystal_F_000             1470
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         5.319
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         10312
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0953P)^2^+2.1585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9531
_reflns_number_total             10312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c02254_si_006.cif
_cod_data_source_block           cxy3141_0m
_cod_depositor_comments
'Adding full bibliography for 4518848--4518852.cif.'
_cod_original_formula_sum        'C55.50 H51 F6 Fe I N O7 P3 Pt S2'
_cod_database_code               4518850
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.145
_shelx_estimated_absorpt_t_min   0.106
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C54-C53 = C58-C53 = C58-C57 = C57-C56 = C55-C54 = C56-C55
 1.39 with sigma of 0.02
 C51-C46 = C48-C47 = C47-C46 = C49-C48 = C50-C49 = C51-C50
 1.39 with sigma of 0.02
3. Restrained planarity
 C59, C56, C55, C57, C54, C58, C53
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C51 \\sim C49 \\sim C50 \\sim C48 \\sim C47 \\sim C46 \\sim C52: within 2.5A
with sigma of 0.1 and sigma for terminal atoms of 0.2 within 2.5A
C58 \\sim C56 \\sim C55 \\sim C57 \\sim C54 \\sim C53 \\sim C59: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C51) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C52) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.1
Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq:
with sigma of 0.05 and sigma for terminal atoms of 0.1
5. Others
 Fixed Sof: C49(0.5) H49(0.5) C50(0.5) H50(0.5) C48(0.5) H48(0.5) C47(0.5)
 H47(0.5) C51(0.5) H51(0.5) C46(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C28(H28), C6(H6), C29(H29), C7(H7), C40(H40), C39(H39),
 C13(H13), C33(H33), C25(H25), C37(H37), C36(H36), C4(H4), C26(H26), C14(H14),
 C41(H41), C22(H22), C19(H19), C20(H20), C21(H21), C31(H31), C16(H16), C34(H34),
  C17(H17), C30(H30), C23(H23), C43(H43), C24(H24), C42(H42), C27(H27),
 C35(H35), C15(H15), C49(H49), C50(H50), C48(H48), C47(H47), C51(H51), C56(H56),
  C55(H55), C57(H57), C54(H54), C58(H58)
6.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C52(H52A,H52B,H52C), C59(H59A,H59B,H59C)
;
_shelx_res_checksum              30045
_shelx_hkl_checksum              46056
_olex2_submission_special_instructions 'No special instructions were received'