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_4338138
_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         'C16 H32 K O8, C3 H9 Sn'
_chemical_formula_sum            'C19 H41 K O8 Sn'
_chemical_formula_weight         555.31
_chemical_name_systematic
;
 ?
;
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_symmetry_space_group_name_Hall  '-P 2yb'
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_cell_angle_beta                 99.082(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.6217(12)
_cell_length_b                   21.232(4)
_cell_length_c                   8.1478(13)
_cell_measurement_reflns_used    3184
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.24
_cell_measurement_theta_min      2.52
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_computing_cell_refinement
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 CrysAlisPro, Agilent Technologies,
 Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
 (compiled Jan 23 2012,18:06:46)
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 CrysAlisPro, Agilent Technologies,
 Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
 (compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
 (compiled Jan 23 2012,18:06:46)
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_computing_molecular_graphics
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 ORTEP3 for Windows (L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.)
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 WinGX v1.80.05 (L. J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838.)
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 SHELXL-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)
;
_computing_structure_solution
;
 SHELXS-86 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, EOS'
_diffrn_measurement_method       \w-scan
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1239
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5732
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_diffrn_reflns_theta_max         26.99
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_exptl_absorpt_coefficient_mu    1.177
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_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
 (compiled Jan 23 2012,18:06:46)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             576
_exptl_crystal_recrystallization_method
;
 From solution in THF/12-Crown-4/n-pentane at -20 deg C.
;
_exptl_crystal_size_max          0.41
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_exptl_crystal_size_min          0.13
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_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5732
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0759P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1430
_reflns_number_gt                3720
_reflns_number_total             5732
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic500065s_si_002.cif
_cod_data_source_block           ck29ck
_cod_depositor_comments
'Adding full bibliography for 4338135--4338138.cif.'
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               4338138