Syntheses and Molecular Structures of [RSn{W(CO)3Cp}2][W(CO)3Cp], [RSn{W(CO)3Cp}Cl2], and [RSn{W(CO)3Cp}Cr(CO)5] (R = [4-t-Bu-2,6-{P(O)(OR′)2}2C6H2], R′ = Et,i-Pr). Autoionization Induced by Intramolecular P═O→Sn Coordination
Krabbe, Stefan; Wagner, Michael; Löw, Christian; Dietz, Christina; Schürmann, Markus; Hoffmann, Alexander; Herres-Pawlis, Sonja; Lutter, Michael; Jurkschat, Klaus; Organometallics 33 (2014) 4433–; doi:10.1021/om500649d

data_4084277
_publ_section_title
;
 Syntheses and Molecular Structures of [RSn{W(CO)3Cp}2][W(CO)3Cp],
 [RSn{W(CO)3Cp}Cl2], and [RSn{W(CO)3Cp}Cr(CO)5] (R =
 [4-t-Bu-2,6-{P(O)(OR&#x2032;)2}2C6H2], R&#x2032; = Et,i-Pr).
 Autoionization Induced by Intramolecular P&#x2550;O\\rightarrow Sn
 Coordination
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4433
_journal_paper_doi               10.1021/om500649d
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C38 H49 O12 P2 Sn W2, C8 H5 O3 W, C4 H8 O'
_chemical_formula_sum            'C50 H62 O16 P2 Sn W3'
_chemical_formula_weight         1651.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.709(9)
_cell_angle_beta                 109.122(11)
_cell_angle_gamma                106.124(11)
_cell_formula_units_Z            2
_cell_length_a                   11.4054(14)
_cell_length_b                   16.747(3)
_cell_length_c                   17.288(3)
_cell_measurement_reflns_used    30263
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      3.34
_cell_volume                     2835.7(9)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'enCIFer Version 1.4'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_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  0.071
_diffrn_reflns_av_sigmaI/netI    0.3437
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10340
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    6.620
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.934
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.424
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         10340
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.428
_refine_ls_R_factor_all          0.1358
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0412P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0702
_reflns_number_gt                3708
_reflns_number_total             10340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500649d_si_001.cif
_cod_data_source_block           compound2*THF
_cod_original_cell_volume        2835.7(8)
_cod_database_code               4084277