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

data_4081583
_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         'C25 H16 O10 P2 W2'
_chemical_formula_sum            'C25 H16 O10 P2 W2'
_chemical_formula_weight         906.02
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-06-07
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                80.461(9)
_cell_angle_beta                 89.905(9)
_cell_angle_gamma                67.404(12)
_cell_formula_units_Z            2
_cell_length_a                   9.0784(11)
_cell_length_b                   10.2990(13)
_cell_length_c                   16.9775(16)
_cell_measurement_reflns_used    3722
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      28.0860
_cell_measurement_theta_min      3.3670
_cell_volume                     1441.9(3)
_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
;
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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_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  -19.00   24.00   1.0000    2.3600
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000 -180.0000 43

  2 omega  -25.00   20.00   1.0000    2.3600
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000   30.0000 45

  3 omega   54.00   96.00   1.0000    2.3600
omega____ theta____ kappa____ phi______ frames
    -       19.7885 -178.0000   30.0000 42

  4 omega   -6.00   78.00   1.0000    2.3600
omega____ theta____ kappa____ phi______ frames
    -       19.7885   37.0000 -150.0000 84

  5 omega   37.00   91.00   1.0000    2.3600
omega____ theta____ kappa____ phi______ frames
    -       19.7885  178.0000   60.0000 54

  6 omega  -46.00   63.00   1.0000    2.3600
omega____ theta____ kappa____ phi______ frames
    -       19.7885  -19.0000    0.0000 109

  7 omega  -38.00   24.00   1.0000    2.3600
omega____ theta____ kappa____ phi______ frames
    -      -17.1323   57.0000 -180.0000 62
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0097001000
_diffrn_orient_matrix_UB_12      0.0363655000
_diffrn_orient_matrix_UB_13      0.0328650000
_diffrn_orient_matrix_UB_21      -0.0037779000
_diffrn_orient_matrix_UB_22      0.0625187000
_diffrn_orient_matrix_UB_23      -0.0263161000
_diffrn_orient_matrix_UB_31      -0.0841823000
_diffrn_orient_matrix_UB_32      0.0227485000
_diffrn_orient_matrix_UB_33      -0.0055202000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11835
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.134
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32029
_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
;
;
_exptl_crystal_density_diffrn    2.087
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.764
_refine_diff_density_min         -1.524
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0204P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0644
_reflns_number_gt                4654
_reflns_number_total             5880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400637j_si_001.cif
_cod_data_source_block           20130698
_cod_database_code               4081583
_chemical_oxdiff_formula         C20H20N4O4P2W2
_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, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C21(H21), C22(H22),
 C23(H23), C24(H24), C25(H25)
;