Oxidative addition of ether O-methyl bonds at a Pt(0) centre
Perutz, Robin N; Jasim, Naser A; Procacci, Barbara; Whitwood, Adrian C; Chem.Commun. 50 (2014) 3914–; doi:10.1039/C4CC00853G

data_7112195
_publ_section_title
;
 Oxidative addition of ether O-methyl bonds at a Pt(0) centre
;
_journal_name_full               Chem.Commun.
_journal_page_first              3914
_journal_paper_doi               10.1039/C4CC00853G
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C37 H57 F5 O P2 Pt'
_chemical_formula_sum            'C37 H57 F5 O P2 Pt'
_chemical_formula_weight         869.86
_chemical_name_systematic
;
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-07
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.677(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8789(6)
_cell_length_b                   26.7643(10)
_cell_length_c                   13.7600(5)
_cell_measurement_reflns_used    16415
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      29.0222
_cell_measurement_theta_min      2.8796
_cell_volume                     3535.0(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -49.00   50.00   1.0000    5.8000
omega____ theta____ kappa____ phi______ frames
    -      -17.6138    0.0000 -180.0000 99

  2 omega   -4.00   62.00   1.0000    5.8000
omega____ theta____ kappa____ phi______ frames
    -       18.8638 -113.0000  114.0000 66

  3 omega   16.00   67.00   1.0000    5.8000
omega____ theta____ kappa____ phi______ frames
    -       18.8638 -113.0000  -25.0000 51

  4 omega  -17.00    8.00   1.0000    5.8000
omega____ theta____ kappa____ phi______ frames
    -      -17.6138  -37.0000 -180.0000 25

  5 omega   37.00   78.00   1.0000    5.8000
omega____ theta____ kappa____ phi______ frames
    -       18.8638   77.0000    0.0000 41

  6 omega  -53.00  -28.00   1.0000    5.8000
omega____ theta____ kappa____ phi______ frames
    -       18.8638  -37.0000 -150.0000 25

  7 omega   19.00   45.00   1.0000    5.8000
omega____ theta____ kappa____ phi______ frames
    -       18.8638  -37.0000 -150.0000 26

  8 omega   13.00   41.00   1.0000    5.8000
omega____ theta____ kappa____ phi______ frames
    -       18.8638  -37.0000 -120.0000 28

  9 omega   20.00   46.00   1.0000    5.8000
omega____ theta____ kappa____ phi______ frames
    -       18.8638  -77.0000   30.0000 26
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0015976000
_diffrn_orient_matrix_UB_12      0.0244824000
_diffrn_orient_matrix_UB_13      0.0199374000
_diffrn_orient_matrix_UB_21      -0.0319055000
_diffrn_orient_matrix_UB_22      -0.0088897000
_diffrn_orient_matrix_UB_23      0.0376946000
_diffrn_orient_matrix_UB_31      0.0664959000
_diffrn_orient_matrix_UB_32      -0.0048974000
_diffrn_orient_matrix_UB_33      0.0313373000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27536
_diffrn_reflns_theta_full        25.63
_diffrn_reflns_theta_max         25.63
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.116
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
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    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.4069
_exptl_crystal_size_mid          0.2344
_exptl_crystal_size_min          0.1778
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         8391
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+2.2905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.0469
_reflns_number_gt                7679
_reflns_number_total             8391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc00853g2.cif
_cod_data_source_block           rnp1103
_cod_database_code               7112195
_chemical_oxdiff_formula         'C37 H57 F5 O P2 Pt'
_chemical_oxdiff_usercomment     'Naser's Pt anisol'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C36-C37 \\sim C36A-C37
 with sigma of 0.01
 C36-C35 \\sim C36A-C35
 with sigma of 0.01
 C31-C32 \\sim C31A-C32
 with sigma of 0.01
 C31-C30 \\sim C31A-C30
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C31) = Uanis(C31A)
Uanis(C36) = Uanis(C36A)
4. Others
 Sof(H30C)=Sof(H30D)=Sof(C31A)=Sof(H31C)=Sof(H31D)=Sof(H32C)=Sof(H32D)=1-FVAR(1)
 Sof(H30A)=Sof(H30B)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H32A)=Sof(H32B)=FVAR(1)
 Sof(H35C)=Sof(H35D)=Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(H37C)=Sof(H37D)=1-FVAR(2)
 Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H37A)=Sof(H37B)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C13(H13), C18(H18), C23(H23), C28(H28), C33(H33)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B), C30(H30C,H30D),
 C31(H31A,H31B), C31A(H31C,H31D), C32(H32A,H32B), C32(H32C,H32D), C34(H34A,
 H34B), C35(H35A,H35B), C35(H35C,H35D), C36(H36A,H36B), C36A(H36C,H36D),
 C37(H37A,H37B), C37(H37C,H37D)
;