Investigations on the Reactivity of Li/Cl Phosphinidenoid Tungsten Complexes toward Various Iodine Compounds
Streubel, Rainer; Özbolat-Schön, Aysel; Bode, Maren; Daniels, Jörg; Schnakenburg, Gregor; Teixidor, Francesc; Vinas, Clara; Vaca, Albert; Pepiol, Ariadna; Farràs, Pau; Organometallics 28 (2009) 6031–; doi:10.1021/om900443v

data_4069843
_publ_section_title
;
 Investigations on the Reactivity of Li/Cl Phosphinidenoid Tungsten
 Complexes toward Various Iodine Compounds
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              6031
_journal_paper_doi               10.1021/om900443v
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C28 H28 I O5 P Si2 W'
_chemical_formula_weight         842.4
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2008-05-30T12:28:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.404(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4156(3)
_cell_length_b                   14.4943(5)
_cell_length_c                   17.6597(5)
_cell_measurement_reflns_used    78866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3177.00(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.628083E-1
_diffrn_orient_matrix_UB_12      -0.236524E-1
_diffrn_orient_matrix_UB_13      -0.285961E-1
_diffrn_orient_matrix_UB_21      -0.458232E-1
_diffrn_orient_matrix_UB_22      -0.25642E-2
_diffrn_orient_matrix_UB_23      -0.473176E-1
_diffrn_orient_matrix_UB_31      0.211248E-1
_diffrn_orient_matrix_UB_32      0.647614E-1
_diffrn_orient_matrix_UB_33      -0.123175E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31420
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.31
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.767
_exptl_absorpt_correction_T_max  0.3696
_exptl_absorpt_correction_T_min  0.2022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.39
_refine_diff_density_max         1.726
_refine_diff_density_min         -1.684
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         7154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+1.7487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0685
_reflns_number_gt                6523
_reflns_number_total             7154
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900443v_si_002.cif
_cod_data_source_block           joerg185
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4069843