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_1556478
_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         'C54 H72 N6 O6 Sn2, 2(C6 H6)'
_chemical_formula_sum            'C66 H84 N6 O6 Sn2'
_chemical_formula_weight         1294.77
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   14.4547(3)
_cell_length_b                   14.4547(3)
_cell_length_c                   8.7666(3)
_cell_measurement_reflns_used    1771
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.766
_cell_measurement_theta_min      2.815
_cell_volume                     1586.28(7)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
;
_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                 'CCD plate'
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0228833
_diffrn_orient_matrix_UB_12      -0.0500938
_diffrn_orient_matrix_UB_13      0.0376465
_diffrn_orient_matrix_UB_21      -0.0474412
_diffrn_orient_matrix_UB_22      -0.018199
_diffrn_orient_matrix_UB_23      -0.0432585
_diffrn_orient_matrix_UB_31      0.0208909
_diffrn_orient_matrix_UB_32      -0.0192605
_diffrn_orient_matrix_UB_33      -0.057079
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3618
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         2.82
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.97757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prim
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.042
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.06
_refine_ls_wR_factor_ref         0.0621
_reflns_number_gt                1868
_reflns_number_total             2160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            x2008.cif
_cod_data_source_block           x2008
_cod_original_sg_symbol_H-M      P-3
_cod_database_code               1556478