K-H3C and K-Sn Interactions in Potassium Trimethylstannyl Complexes: A Structural, Mechanochemical, and NMR Study.
Kleeberg, Christian; Grunenberg, Jörg; Xie, Xiulan; Inorganic chemistry 53 (2014) 4400–4410; doi:10.1021/ic500065s

data_4338135
_publ_section_title
;
 K-H3C and K-Sn Interactions in Potassium Trimethylstannyl Complexes: A
 Structural, Mechanochemical, and NMR Study.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4400
_journal_page_last               4410
_journal_paper_doi               10.1021/ic500065s
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C12 H24 K O6, C3 H9 Sn'
_chemical_formula_sum            'C15 H33 K O6 Sn'
_chemical_formula_weight         467.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.612(7)
_cell_angle_beta                 81.612(7)
_cell_angle_gamma                67.214(8)
_cell_formula_units_Z            2
_cell_length_a                   8.8884(9)
_cell_length_b                   8.8903(8)
_cell_length_c                   15.0357(12)
_cell_measurement_reflns_used    10860
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.77
_cell_measurement_theta_min      3.85
_cell_volume                     1076.26(18)
_computing_cell_refinement
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
 (compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
 (compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
 (compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics
;
 Diamond 3.2i, K. Brandenburg, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material
;
 WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838.)
;
_computing_structure_refinement
;
 SHELXL-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 122-122)'
;
_computing_structure_solution
;
 SHELXS-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, Atlas, Nova'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16780
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         75.00
_diffrn_reflns_theta_min         5.42
_exptl_absorpt_coefficient_mu    11.372
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
 (compiled May 16 2011,17:55:39)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             480
_exptl_crystal_recrystallization_method
;
 From a solution in PhMe at ambient temperature.
;
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4418
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0400P)^2^+0.8738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                4300
_reflns_number_total             4418
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic500065s_si_002.cif
_cod_data_source_block           ck17ck
_cod_depositor_comments
;Adding full bibliography for 4338135--4338138.cif.

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom and difmap' was changed
to 'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1076.26(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4338135