Strongly σ Donating Thiophenoxide in Silica-Supported Tungsten Oxo Catalysts for Improved 1-Alkene Metathesis Efficiency
Mougel, Victor; Pucino, Margherita; Copéret, Christophe; Organometallics 34 (2015) 551–; doi:10.1021/om5013105

data_4085410
_publ_section_title
;
 Strongly \s Donating Thiophenoxide in Silica-Supported Tungsten Oxo
 Catalysts for Improved 1-Alkene Metathesis Efficiency
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              551
_journal_paper_doi               10.1021/om5013105
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C53 H60 O S2 W'
_chemical_formula_sum            'C53 H60 O S2 W'
_chemical_formula_weight         960.98
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 134.22(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.271(4)
_cell_length_b                   13.1156(3)
_cell_length_c                   17.822(2)
_cell_measurement_reflns_used    16388
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1268
_cell_measurement_theta_min      2.8856
_cell_volume                     4568.4(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_details
;
  1 omega  -39.00   51.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9802   57.0000  150.0000 90

  2 omega  -25.00   60.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490  -99.0000 -120.0000 85

  3 omega   -3.00   83.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490   57.0000  -60.0000 86

  4 omega   -3.00   56.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490   57.0000  150.0000 59

  5 omega    8.00   87.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490   57.0000 -150.0000 79

  6 omega  -25.00   60.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490  -99.0000   60.0000 85

  7 omega   -8.00   83.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490   77.0000   30.0000 91

  8 omega  -50.00   40.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490  -38.0000  -90.0000 90

  9 omega  -87.00  -25.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9802  -57.0000    0.0000 62

 10 omega  -25.00   60.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       18.4490  -99.0000    0.0000 85
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0297452000
_diffrn_orient_matrix_UB_12      0.0295408000
_diffrn_orient_matrix_UB_13      0.0247955000
_diffrn_orient_matrix_UB_21      0.0207495000
_diffrn_orient_matrix_UB_22      -0.0410364000
_diffrn_orient_matrix_UB_23      0.0345301000
_diffrn_orient_matrix_UB_31      0.0013062000
_diffrn_orient_matrix_UB_32      -0.0192252000
_diffrn_orient_matrix_UB_33      -0.0357743000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1068
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            69775
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.191
_diffrn_reflns_theta_min         2.891
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.2532
_exptl_crystal_size_mid          0.2255
_exptl_crystal_size_min          0.0729
_refine_diff_density_max         2.530
_refine_diff_density_min         -2.208
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         11431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0714
_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^)+(0.0309P)^2^+69.3949P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7965
_reflns_number_total             11431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5013105_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4085409--4085410.cif.'
_cod_original_cell_volume        4568.3(15)
_cod_database_code               4085410
_shelxl_version_number           2012-9
_chemical_oxdiff_formula         'W1 O1 S2 C53 H60'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C18(H18), C9(H9), C24(H24), C15(H15), C10(H10), C8(H8), C27(H27),
 C32(H32), C39(H39), C34(H34), C33(H33), C42(H42), C48(H48), C51(H51)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C3(H3A,H3B,H3C), C17(H17A,H17B,H17C), C23(H23A,H23B,
 H23C), C20(H20A,H20B,H20C), C4(H4A,H4B,H4C), C26(H26A,H26B,H26C), C5(H5A,H5B,
 H5C), C29(H29A,H29B,H29C), C38(H38A,H38B,H38C), C41(H41A,H41B,H41C), C47(H47A,
 H47B,H47C), C44(H44A,H44B,H44C), C50(H50A,H50B,H50C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              90957
_shelx_hkl_checksum              11926
_olex2_date_sample_data_collection 2014-09-18
_olex2_submission_special_instructions 'No special instructions were received'