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_7112196
_publ_contact_author_address
;Department of Chemistry
University of York
York
YO10 5DD
;
_publ_contact_author_email       robin.perutz@york.ac.uk
_publ_contact_author_name        'Professor Robin N Perutz'
_publ_contact_author_phone       '(+44)904 322549'
_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 H59 F3 O P2 Pt'
_chemical_formula_sum            'C37 H59 F3 O P2 Pt'
_chemical_formula_weight         833.87
_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     iterative
_audit_creation_date             2014-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.3566(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.72738(15)
_cell_length_b                   26.6352(4)
_cell_length_c                   13.74424(18)
_cell_measurement_reflns_used    19988
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      32.1010
_cell_measurement_theta_min      3.2580
_cell_volume                     3478.51(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0439272000
_diffrn_orient_matrix_UB_12      -0.0162412000
_diffrn_orient_matrix_UB_13      -0.0207670000
_diffrn_orient_matrix_UB_21      -0.0076869000
_diffrn_orient_matrix_UB_22      -0.0188514000
_diffrn_orient_matrix_UB_23      0.0348737000
_diffrn_orient_matrix_UB_31      -0.0598786000
_diffrn_orient_matrix_UB_32      -0.0094925000
_diffrn_orient_matrix_UB_33      -0.0337960000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41481
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         30.046
_diffrn_reflns_theta_min         2.798
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.171
_exptl_absorpt_correction_T_max  0.559
_exptl_absorpt_correction_T_min  0.314
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.3546
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.1671
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         10210
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0217
_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^)+(0.0122P)^2^+2.9793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0442
_refine_ls_wR_factor_ref         0.0457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9326
_reflns_number_total             10210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc00853g2.cif
_cod_data_source_block           added_by_encifer
_cod_database_code               7112196
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C37 H59 F3 O1 P2 Pt1'
_chemical_oxdiff_usercomment     'Naser's 2,3,6-trifluoroanisol-Pt'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2A) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C3A) = Uanis(C7)
Uanis(F7) = Uanis(F3A)
Uanis(F4) = Uanis(F6A)
Uanis(C25A) = Uanis(C26A)
Uanis(C4A) = Uanis(C6)
Uanis(C7A) = Uanis(C3)
Uanis(C6A) = Uanis(C4)
Uanis(C2) = Uanis(C2A)
3. Others
 Sof(C2A)=Sof(C3A)=Sof(C4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=
 Sof(H24C)=Sof(H24D)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C26A)=Sof(H26C)=
 Sof(H26D)=Sof(H27C)=Sof(H27D)=Sof(F3A)=Sof(F6A)=Sof(F7A)=1-FVAR(1)
 Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H24A)=
 Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H27A)=
 Sof(H27B)=Sof(F3)=Sof(F4)=Sof(F7)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C13(H13), C18(H18), C23(H23), C28(H28), C33(H33)
4.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), C24(H24C,H24D), C25(H25A,
 H25B), C25A(H25C,H25D), C26(H26A,H26B), C26A(H26C,H26D), C27(H27C,H27D),
 C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
  C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C5A(H5A), C6(H6), C6A(H6A)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              25963
_shelx_hkl_checksum              70496