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_4084276
_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, 0.5(C7 H8)'
_chemical_formula_sum            'C49.5 H58 O15 P2 Sn W3'
_chemical_formula_weight         1625.14
_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                97.518(5)
_cell_angle_beta                 97.034(5)
_cell_angle_gamma                94.070(5)
_cell_formula_units_Z            2
_cell_length_a                   11.1707(6)
_cell_length_b                   15.8064(9)
_cell_length_c                   16.0709(9)
_cell_measurement_reflns_used    6079
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.1470
_cell_measurement_theta_min      2.5600
_cell_volume                     2781.1(3)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.33.55''
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.33.55''
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.33.55''
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XcaliburS, Sapphire3'
_diffrn_measurement_method       '\w und \y scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_sigmaI/netI    0.0907
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36360
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    6.747
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1554
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.206
_refine_diff_density_min         -1.879
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.813
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         10365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.813
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1233
_reflns_number_gt                7361
_reflns_number_total             10365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500649d_si_001.cif
_cod_data_source_block           compound2*0.5toluene
_cod_original_formula_sum        'C49.50 H58 O15 P2 Sn W3'
_cod_database_code               4084276