An unconventional route to [(Me3Si)2HCPCl2W(CO)5] and its conversion to the structurally characterized P-chalcogenides (Me3Si)2HCP(X)Cl2 [X = S, Se]
Khan, Arif Ali; Wismach, Cathleen; Jones, Peter G.; Streubel, Rainer; Dalton Transactions  (2003) 2483–; doi:10.1039/b301775c

data_7012852
_publ_section_title
;
 An unconventional route to [(Me3Si)2HCPCl2W(CO)5] and its conversion
 to the structurally characterized P-chalcogenides (Me3Si)2HCP(X)Cl2 [X
 = S, Se]
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              2483
_journal_paper_doi               10.1039/b301775c
_journal_year                    2003
_chemical_formula_sum            'C7 H19 Cl2 P S Si2'
_chemical_formula_weight         293.33
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.926(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.619(4)
_cell_length_b                   14.482(7)
_cell_length_c                   12.031(6)
_cell_measurement_reflns_used    5473
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     1444.1(12)
_computing_cell_refinement       'Bruker Saint'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  ShelXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker Samrt 1000 CCD'
_diffrn_measurement_method       '\w- and \f-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1682
_diffrn_reflns_av_sigmaI/netI    0.0848
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23211
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         31.11
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'cut tablet'
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.262
_refine_diff_density_min         -1.082
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    'Methyls rigid, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         4504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1130P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1607
_reflns_number_gt                3749
_reflns_number_total             4504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b301775c.txt
_cod_data_source_block           jhinga
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7012852