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_4069842
_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            'C12 H19 Cl I O5 P Si2 W'
_chemical_formula_weight         676.62
_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             2007-12-14T12:52:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.3970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7403(4)
_cell_length_b                   9.6381(2)
_cell_length_c                   15.3230(3)
_cell_measurement_reflns_used    19714
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2133.99(8)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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      -0.110079E-1
_diffrn_orient_matrix_UB_12      0.54058E-2
_diffrn_orient_matrix_UB_13      -0.66433E-1
_diffrn_orient_matrix_UB_21      -0.673072E-1
_diffrn_orient_matrix_UB_22      0.169592E-1
_diffrn_orient_matrix_UB_23      -0.19916E-2
_diffrn_orient_matrix_UB_31      0.11749E-1
_diffrn_orient_matrix_UB_32      0.10222
_diffrn_orient_matrix_UB_33      0.38437E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.053
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20403
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.71
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    7.188
_exptl_absorpt_correction_T_max  0.5378
_exptl_absorpt_correction_T_min  0.1471
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        (see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.749
_refine_diff_density_min         -4.643
_refine_diff_density_rms         0.3
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                4302
_reflns_number_total             4838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900443v_si_001.cif
_cod_data_source_block           joerg103
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4069842