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_4085409
_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         'C61 H71 O P S2 W'
_chemical_formula_sum            'C61 H71 O P S2 W'
_chemical_formula_weight         1099.11
_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
_audit_creation_date             2014-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.520(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0112(5)
_cell_length_b                   22.0746(13)
_cell_length_c                   20.3751(14)
_cell_measurement_reflns_used    3661
_cell_measurement_temperature    101(1)
_cell_measurement_theta_max      23.4420
_cell_measurement_theta_min      3.1570
_cell_volume                     5400.4(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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(1)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -48.00   52.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.8240   77.0000   60.0000 100

  2 omega  -12.00   87.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2927   77.0000 -180.0000 99

  3 omega  -54.00  -29.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.2927  -38.0000 -150.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0477069000
_diffrn_orient_matrix_UB_12      -0.0130841000
_diffrn_orient_matrix_UB_13      0.0140789000
_diffrn_orient_matrix_UB_21      -0.0266188000
_diffrn_orient_matrix_UB_22      -0.0012396000
_diffrn_orient_matrix_UB_23      -0.0314720000
_diffrn_orient_matrix_UB_31      0.0225193000
_diffrn_orient_matrix_UB_32      -0.0293120000
_diffrn_orient_matrix_UB_33      -0.0049025000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.1361
_diffrn_reflns_Laue_measured_fraction_full 0.935
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20667
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         2.943
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.285
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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    1.352
_exptl_crystal_description       plate
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.932
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         9143
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0860
_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^)+(0.0434P)^2^+26.4621P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6437
_reflns_number_total             9143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5013105_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4085409--4085410.cif.'
_cod_database_code               4085409
_shelxl_version_number           2012-9
_chemical_oxdiff_formula         'C61 H71 O P S2 W'
_reflns_odcompleteness_completeness 98.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints
C59 \\sim C58 \\sim C60: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
C25 \\sim C23 \\sim C22: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
C42 \\sim C40 \\sim C39: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 C53(H53), C1(H1), C18(H18), C44(H44), C50(H50), C39(H39), C25(H25), C11(H11),
 C14(H14), C19(H19), C20(H20), C43(H43), C28(H28), C36(H36), C59(H59), C45(H45),
  C61(H61), C63(H63), C60(H60), C62(H62)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C35(H35A,H35B,H35C), C16(H16A,H16B,H16C), C3(H3A,H3B,H3C),
 C24(H24A,H24B,H24C), C4(H4A,H4B,H4C), C30(H30A,H30B,H30C), C27(H27A,H27B,H27C),
  C13(H13A,H13B,H13C), C41(H41A,H41B,H41C), C38(H38A,H38B,H38C), C52(H52A,H52B,
 H52C), C10(H10A,H10B,H10C), C49(H49A,H49B,H49C), C57(H57A,H57B,H57C), C56(H56A,
 H56B,H56C), C55(H55A,H55B,H55C)
;