Contrasting reductions of group 14 metal(II) chloride complexes: synthesis of a ?-diketiminato tin(I) dimer
Sam L. Choong; Christian Schenk; Andreas Stasch; Deepak Dange; Cameron Jones; Chem.Commun. 48 (2012) 2504–; doi:10.1039/c2cc18086c

data_7107431
_publ_section_title
;
 Contrasting reductions of group 14 metal(II) chloride complexes:
 synthesis of a ?-diketiminato tin(I) dimer
;
_journal_name_full               Chem.Commun.
_journal_page_first              2504
_journal_paper_doi               10.1039/c2cc18086c
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C110 H154 Cl4 Mg2 N8 Pb2'
_chemical_formula_weight         2193.21
_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                 95.860(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0924(5)
_cell_length_b                   28.9325(9)
_cell_length_c                   27.2581(13)
_cell_measurement_temperature    123(2)
_cell_volume                     11055.8(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_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  0.1289
_diffrn_reflns_av_sigmaI/netI    0.1857
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            65659
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    3.197
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4504
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.203
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1187
_refine_ls_number_reflns         19435
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0149P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1102
_reflns_number_gt                12455
_reflns_number_total             19435
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc18086c.txt
_cod_data_source_block           {(MesNac)MgClPb(Cl)(tBuMesNac)}2
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7107431