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_7107430
_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            'C35 H53 Cl N2 Pb'
_chemical_formula_weight         744.43
_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                 100.726(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5359(4)
_cell_length_b                   10.6225(2)
_cell_length_c                   19.5757(5)
_cell_measurement_temperature    123(2)
_cell_volume                     3378.45(14)
_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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22710
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    5.097
_exptl_absorpt_correction_T_max  0.556
_exptl_absorpt_correction_T_min  0.427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         7372
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0228
_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^)+(0.0147P)^2^+3.1987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0443
_refine_ls_wR_factor_ref         0.0487
_reflns_number_gt                6211
_reflns_number_total             7372
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc18086c.txt
_cod_data_source_block           (tBuNac)PbCl
_cod_original_cell_volume        3378.45(13)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7107430