Simple Access to Tungsten-Stabilized Disecondary Diphosphines
Tian, Rongqiang; Mei, Yanbo; Duan, Zheng; Mathey, François; Organometallics 32 (2013) 5615–; doi:10.1021/om400637j

data_4081582
_publ_section_title
;
 Simple Access to Tungsten-Stabilized Disecondary Diphosphines
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5615
_journal_paper_doi               10.1021/om400637j
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C18 H8 O10 P2 S2 W2'
_chemical_formula_sum            'C18 H8 O10 P2 S2 W2'
_chemical_formula_weight         878.00
_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             2013-06-28
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.730(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9195(3)
_cell_length_b                   12.8070(3)
_cell_length_c                   21.7839(7)
_cell_measurement_reflns_used    4961
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.3083
_cell_measurement_theta_min      2.8819
_cell_volume                     2959.34(15)
_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
;
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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    9.00   79.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   42.0000  -57.0000 70

  2 omega   35.00   65.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  178.0000   90.0000 30

  3 omega  -43.00  -12.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  -57.0000  120.0000 31

  4 omega   25.00   89.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104   57.0000 -150.0000 64

  5 omega   50.00   94.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7104  178.0000  150.0000 44
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0291713000
_diffrn_orient_matrix_UB_12      0.0210300000
_diffrn_orient_matrix_UB_13      0.0230945000
_diffrn_orient_matrix_UB_21      -0.0485995000
_diffrn_orient_matrix_UB_22      0.0212284000
_diffrn_orient_matrix_UB_23      -0.0243252000
_diffrn_orient_matrix_UB_31      -0.0354205000
_diffrn_orient_matrix_UB_32      -0.0465905000
_diffrn_orient_matrix_UB_33      -0.0006277000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12931
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.07
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.059
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74520
_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
;
;
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         6031
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+1.7079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0793
_reflns_number_gt                4516
_reflns_number_total             6031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400637j_si_001.cif
_cod_data_source_block           20130432
_cod_original_cell_volume        2959.36(15)
_cod_database_code               4081582
_chemical_oxdiff_formula         C20H20O10W2S2P2
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C11-C12
 1.4 with sigma of 0.02
 C15-C16
 1.4 with sigma of 0.02
 C16-C17
 1.4 with sigma of 0.02
 C17-C18
 1.4 with sigma of 0.02
 C15A-C16A
 1.4 with sigma of 0.02
 C16A-C17A
 1.4 with sigma of 0.02
 C18A-C17A
 1.4 with sigma of 0.02
 S2A-C18A
 1.7 with sigma of 0.02
 S2A-C15A
 1.7 with sigma of 0.02
 C15-S2
 1.7 with sigma of 0.02
 S2-C18
 1.7 with sigma of 0.02
 C15-C16
 1.4 with sigma of 0.02
 C16-C17
 1.4 with sigma of 0.02
 C18-C17
 1.4 with sigma of 0.02
 C18A-C16A
 1.9 with sigma of 0.02
 C18A-C16A
 2.1 with sigma of 0.02
 C18A-C16A
 2.3 with sigma of 0.02
 C16-C18
 2.3 with sigma of 0.02
 S1A-C11
 1.7 with sigma of 0.02
 C11-S1
 1.7 with sigma of 0.02
 C14A-S1A
 1.7 with sigma of 0.02
 C14A-C13A
 1.4 with sigma of 0.02
 C14-C13
 1.4 with sigma of 0.02
 C13-C12
 1.4 with sigma of 0.02
 C13A-C12A
 1.4 with sigma of 0.02
 C12-C14
 2.3 with sigma of 0.02
 H1-P1 = H2-P2
 1 with sigma of 0.02
 C15A-P2
 1.85 with sigma of 0.02
 C15-P2
 1.85 with sigma of 0.02
 C11-P1
 1.85 with sigma of 0.02
 P2-C15A
 1.83 with sigma of 0.02
 C15A-P2
 1.83 with sigma of 0.02
 P1-C11
 1.85 with sigma of 0.02
 C11-P1
 1.85 with sigma of 0.02
 C15-P2
 1.85 with sigma of 0.02
 C15A-P2
 1.85 with sigma of 0.02
 C11A-C12A
 1.4 with sigma of 0.02
 C11-C12
 1.4 with sigma of 0.02
 C11A-P1
 1.85 with sigma of 0.02
 C15A-P2
 1.86 with sigma of 0.02
 C15-P2
 1.86 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C15A) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(S2) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(S2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S1) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(S1A) \\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C14A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S2) = Uanis(S2A)
Uanis(C16) = Uanis(C16A)
Uanis(C15) = Uanis(C15A)
Uanis(C17) = Uanis(C17A)
Uanis(C18) = Uanis(C18A)
Uanis(S1) = Uanis(S1A)
Uanis(C12) = Uanis(C12A)
Uanis(C13) = Uanis(C13A)
Uanis(C14) = Uanis(C14A)
Uanis(C11) = Uanis(C11A)
4. Others
 Sof(S2A)=Sof(C16A)=Sof(H16A)=Sof(C15A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=
 Sof(H18A)=1-FVAR(1)
 Sof(S2)=Sof(C16)=Sof(H16)=Sof(C15)=Sof(C18)=Sof(H18)=Sof(C17)=Sof(H17)=FVAR(1)
 Sof(S1A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=1-FVAR(2)
 Sof(S1)=Sof(C12)=Sof(H12)=Sof(C14)=Sof(H14)=Sof(C13)=Sof(H13)=FVAR(2)
 Sof(C11A)=1-FVAR(3)
 Sof(C11)=FVAR(3)
5.a Riding coordinates:
 C14A(H1,H2)
5.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C12(H12), C18(H18), C17(H17), C16A(H16A), C17A(H17A), C18A(H18A),
 C12A(H12A), C14(H14), C13(H13), C13A(H13A), C14A(H14A)
;