Phosphonate−Stannylene Coupling in the Reactions of the Anion [Mn2{μ-OP(OEt)2}{μ-P(OEt)2}(CO)6]2-with SnR2Cl2(R = Bu, Ph)
Liu, Xiang-Yang; Ruiz, Miguel A.; Lanfranchi, Maurizio; Tiripicchio, Antonio; Organometallics 24 (2005) 3527–; doi:10.1021/om050250u

data_4075890
_publ_section_title
;
 Phosphonate&#x2212;Stannylene Coupling in the Reactions of the Anion
 [Mn2{\m-OP(OEt)2}{\m-P(OEt)2}(CO)6]2-with SnR2Cl2(R = Bu, Ph)
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3527
_journal_paper_doi               10.1021/om050250u
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C35 H51 Mn2 O11 P3 Sn, 0.5(C1 H2 Cl2)'
_chemical_formula_sum            'C35.5 H52 Cl Mn2 O11 P3 Sn'
_chemical_formula_weight         1011.70
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 91.24(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.367(4)
_cell_length_b                   20.625(5)
_cell_length_c                   35.067(7)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      8
_cell_volume                     8942(4)
_computing_cell_refinement       'local programs'
_computing_data_collection       'local programs'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Philips PW 1100'
_diffrn_measurement_method       theta/2theta
_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  0.0720
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7917
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.329
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7903
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Walker and Stuart'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4120
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         7786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.199
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1067P)^2^+19.2972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1810
_refine_ls_wR_factor_ref         0.2217
_reflns_number_gt                4587
_reflns_number_total             7786
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050250usi20050404_065744.cif
_cod_data_source_block           rie30s1
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C35.50 H52 Cl Mn2 O11 P3 Sn'
_cod_database_code               4075890