1JWSnas a Solution State Predictor for Tungsten−Tin Solid State Bond Length in Sterically Crowded Tungstenocene Stannyl Complexes
Mobley, T. Andrew; Gandour, Rochelle; Gillis, Eric P.; Nti-Addae, Kwame; Palchaudhuri, Rahul; Rajbhandari, Presha; Tomson, Neil; Vargas, Angel; Zheng, Qi; Organometallics 24 (2005) 3897–; doi:10.1021/om049006d

data_4075645
_publ_section_title
;
 1JWSnas a Solution State Predictor for Tungsten&#x2212;Tin Solid State
 Bond Length in Sterically Crowded Tungstenocene Stannyl Complexes
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3897
_journal_paper_doi               10.1021/om049006d
_journal_volume                  24
_journal_year                    2005
_chemical_compound_source        'see text'
_chemical_formula_analytical     'C22 H21 Cl Sn W'
_chemical_formula_moiety         'C22 H21 Cl Sn W'
_chemical_formula_sum            'C22 H21 Cl Sn W'
_chemical_formula_weight         623.38
_chemical_melting_point          190
_chemical_name_common
'hydridotungstenocene diphenylstannyl chloride'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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             2004-10-31T12:58:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.23(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.952(2)
_cell_length_b                   13.417(3)
_cell_length_c                   15.161(3)
_cell_measurement_reflns_used    8986
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1962.3(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL v5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL v5.1 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL v5.1 (Sheldrick, 1997)'
_diffrn_ambient_temperature      190(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       ' ?'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD phi and omega Scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16527
_diffrn_reflns_reduction_process ' ?'
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.16
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.268
_exptl_absorpt_correction_T_max  0.418
_exptl_absorpt_correction_T_min  0.321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        HKL Scalepack (Otwinowiski & Minor, 1997)
         Reported T_min and T_max are the scale factor range (after scaling by
     0.0369) reported in Scalepack output, since output does not include 
    real T_min and T_max values.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.11
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             1176
_exptl_crystal_recrystallization_method 'THF/hexanes at -80 degrees Celsius'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.1
_refine_ls_abs_structure_details unknown
_refine_ls_extinction_coef       0.00091(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.022
_refine_ls_goodness_of_fit_gt    1.022
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_restrained_S_gt       1.029
_refine_ls_R_factor_all          0.026
_refine_ls_R_factor_gt           0.020
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0115P)^2^+1.4805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.041
_refine_ls_wR_factor_gt          0.039
_refine_ls_wR_factor_ref         0
_reflns_number_gt                3943
_reflns_number_total             4492
_reflns_threshold_expression     F>4\s(F)
_cod_data_source_file            om049006dsi20041214_032017.cif
_cod_data_source_block           Cp2WHSnClPh2_cmpd_1b
_cod_original_cell_volume        1962.2(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4075645