Platinum(0)-mediated C-O bond activation of ethers via an SN2 mechanism.
Ortuño, Manuel A; Jasim, Nasarella A.; Whitwood, Adrian C.; Lledós, Agustí; Perutz, Robin N.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18842–18850; doi:10.1039/c6dt03241a

data_7040822
_publ_section_title
;
 Platinum(0)-mediated C-O bond activation of ethers via an SN2 mechanism.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18842
_journal_page_last               18850
_journal_paper_doi               10.1039/c6dt03241a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C39 H71 P2 Pt, C5 F4 N O'
_chemical_formula_sum            'C44 H71 F4 N O P2 Pt'
_chemical_formula_weight         963.04
_chemical_name_systematic
'Bis(tricyclohexylphoshine)platinum(eta3-allyl) 2,3,5,6-tetrafluoro-4-oxido-pyridine'
_chemical_properties_physical    ', Air-sensitive'
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-17 deposited with the CCDC.
2016-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.4669(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.67024(20)
_cell_length_b                   17.60500(17)
_cell_length_c                   16.44506(19)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      32.0490
_cell_measurement_theta_min      3.2990
_cell_volume                     4250.39(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -82.00  -37.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.0740  -57.0000   30.0000 45

  2 omega  -20.00   67.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4802  -99.0000  120.0000 87

  3 omega    9.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4802   57.0000  -90.0000 86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0006088000
_diffrn_orient_matrix_UB_12      0.0352411000
_diffrn_orient_matrix_UB_13      -0.0206906000
_diffrn_orient_matrix_UB_21      -0.0192505000
_diffrn_orient_matrix_UB_22      0.0180822000
_diffrn_orient_matrix_UB_23      0.0280866000
_diffrn_orient_matrix_UB_31      0.0442977000
_diffrn_orient_matrix_UB_32      0.0073818000
_diffrn_orient_matrix_UB_33      0.0300612000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21764
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.030
_diffrn_reflns_theta_min         3.007
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.428
_exptl_absorpt_correction_T_max  0.757
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/hexane'
_exptl_crystal_size_max          0.2442
_exptl_crystal_size_mid          0.1984
_exptl_crystal_size_min          0.0915
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         12386
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0140P)^2^+1.7582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10609
_reflns_number_total             12386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03241a2.cif
_cod_data_source_block           rnp1413
_cod_depositor_comments          'Adding full bibliography for 7040822.cif.'
_cod_database_code               7040822
_chemical_oxdiff_formula         'C44 H71 F4 N1 O1 P2 Pt1'
_chemical_oxdiff_usercomment     'Naser Ptallyloxipcy3 Toluene'
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C1-H1AB \\sim C1-H1BC \\sim C1-H1AA \\sim C1-H1BD \\sim C3-H3A \\sim C3-H3B
\\sim C3A-H3AA \\sim C3A-HA_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2A) = Uanis(C2)
Uanis(C3) = Uanis(C3A)
Uiso(H3AA) = Uiso(H3B)
Uiso(H1AA) = Uiso(H1AB) = Uiso(H1BC) = Uiso(H1BD)
4. Others
 Fixed Sof: H1AA(0.5) H1AB(0.5) H1BC(0.5) H1BD(0.5) C2(0.5) H(0.5) C2A(0.5)
 H2A(0.5) C3(0.5) H3A(0.5) H3B(0.5) C3A(0.5) H3AA(0.5) HA(0.5)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C10(H10), C16(H16), C22(H22), C28(H28), C34(H34)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,
 H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
  C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
 C33(H33A,H33B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
  C39(H39A,H39B)
;
_shelx_res_checksum              38368
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2014-04-22
_olex2_submission_special_instructions 'No special instructions were received'