Manganese-Tin Triple Bonds: A New Synthetic Route to the Manganese Stannylidyne Complex Cation trans-[H(dmpe)2Mn\τbSn(C6H3-2,6-Mes2)]+ (dmpe = Me2PCH2CH2PMe2, Mes = 2,4,6-Trimethylphenyl)
Alexander C. Filippou; Priyabrata Ghana; Uttam Chakraborty; Gregor Schnakenburg; Journal of the American Chemical Society 135 (2013) 11525–11528; doi:10.1021/ja406290t

data_4120246
_publ_section_title
;
 Manganese-Tin Triple Bonds: A New Synthetic Route to the Manganese
 Stannylidyne Complex Cation trans-[H(dmpe)2Mn\\tbSn(C6H3-2,6-Mes2)]+
 (dmpe = Me2PCH2CH2PMe2, Mes = 2,4,6-Trimethylphenyl)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11525
_journal_page_last               11528
_journal_paper_doi               10.1021/ja406290t
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C36 H58 Mn P4 Sn, C32 H12 B F24, C6 H5, F'
_chemical_formula_sum            'C74 H75 B F25 Mn P4 Sn'
_chemical_formula_weight         1747.66
_chemical_name_systematic
; 
 ? 
;
_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                 97.7733(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.4964(3)
_cell_length_b                   15.7107(4)
_cell_length_c                   25.8856(6)
_cell_measurement_reflns_used    17724
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_cell_volume                     7856.0(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50740
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    0.660
_exptl_absorpt_correction_T_max  0.8793
_exptl_absorpt_correction_T_min  0.7690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       block
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.379
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     993
_refine_ls_number_reflns         18639
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1281
_reflns_number_gt                12372
_reflns_number_total             18639
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja406290t_si_002.cif
_cod_data_source_block           3a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4120246