Monoanionic Tin Oligomers Featuring Sn-Sn or Sn-Pb Bonds: Synthesis and Characterization of a Tris(Triheteroarylstannyl)Stannate and -Plumbate
Zeckert, K.; Inorganics 4 (2016) 19–; doi:10.3390/inorganics4020019

data_1556477
_publ_section_title
;
 Monoanionic Tin Oligomers Featuring Sn-Sn or Sn-Pb Bonds: Synthesis and
 Characterization of a Tris(Triheteroarylstannyl)Stannate and -Plumbate
;
_journal_name_full               Inorganics
_journal_page_first              19
_journal_paper_doi               10.3390/inorganics4020019
_journal_volume                  4
_journal_year                    2016
_chemical_formula_moiety         'C81 H108 Li N9 O9 Pb Sn3'
_chemical_formula_sum            'C81 H108 Li N9 O9 Pb Sn3'
_chemical_formula_weight         1921.96
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                88.874(2)
_cell_angle_beta                 85.776(2)
_cell_angle_gamma                65.256(3)
_cell_formula_units_Z            4
_cell_length_a                   17.2766(4)
_cell_length_b                   19.4489(6)
_cell_length_c                   28.6285(7)
_cell_measurement_reflns_used    17123
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.897
_cell_measurement_theta_min      3.042
_cell_volume                     8711.9(5)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 	SHELXS-97
 	Program for Crystal Structure Analysis (Release 97-2)
 	G. M. Sheldrick, Institut f\"ur Anorganische Chemie der Universit\"at,
 	Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998.
;
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0367312
_diffrn_orient_matrix_UB_12      0.006441
_diffrn_orient_matrix_UB_13      -0.0121261
_diffrn_orient_matrix_UB_21      -0.0066741
_diffrn_orient_matrix_UB_22      0.0382252
_diffrn_orient_matrix_UB_23      -0.0035104
_diffrn_orient_matrix_UB_31      0.0257011
_diffrn_orient_matrix_UB_32      -0.0104964
_diffrn_orient_matrix_UB_33      -0.0213992
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            74704
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    2.833
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.7805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.798
_refine_diff_density_min         -1.643
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1922
_refine_ls_number_reflns         41501
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+14.5643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.092
_refine_ls_wR_factor_ref         0.105
_reflns_number_gt                28567
_reflns_number_total             41501
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            x1964.cif
_cod_data_source_block           x1964
_cod_original_cell_volume        8711.9(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1556477