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_7107429
_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            'C64 H96 N4 Pb'
_chemical_formula_weight         1128.64
_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                74.160(3)
_cell_angle_beta                 76.098(3)
_cell_angle_gamma                86.034(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6557(4)
_cell_length_b                   12.1595(4)
_cell_length_c                   22.2271(8)
_cell_measurement_temperature    123(2)
_cell_volume                     2941.78(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19383
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    2.908
_exptl_absorpt_correction_T_max  0.756
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.351
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         10856
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0295P)^2^+2.0039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                9340
_reflns_number_total             10856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc18086c.txt
_cod_data_source_block           (tBuMesNac)2Pb
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107429