On the structural diversity of [K(18-crown-6)EPh3] complexes (E = C, Si, Ge, Sn, Pb): synthesis, crystal structures and NOESY NMR study.
Kleeberg, Christian; Dalton transactions (Cambridge, England : 2003) 42 (2013) 8276–8287; doi:10.1039/c3dt50523e

data_7021447
_publ_section_title
;
 On the structural diversity of [K(18-crown-6)EPh3] complexes (E = C, Si,
 Ge, Sn, Pb): synthesis, crystal structures and NOESY NMR study.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8276
_journal_page_last               8287
_journal_paper_doi               10.1039/c3dt50523e
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C31 H39 K O6'
_chemical_formula_sum            'C31 H39 K O6'
_chemical_formula_weight         546.72
_chemical_name_common            '18-Crown-6-potassium triphenyl-carbon'
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 90.447(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.8014(5)
_cell_length_b                   28.7693(14)
_cell_length_c                   19.7370(10)
_cell_measurement_reflns_used    20183
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.84
_cell_measurement_theta_min      2.17
_cell_volume                     5565.3(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_molecular_graphics
;
Diamond 3.2i, K. Brandenburg, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material
;
WinGX v1.80.05 (L. J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838.)
;
_computing_structure_refinement
;
SHELXL-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)
;
_computing_structure_solution
;
SIR-92 (A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi,
J. Appl. Crystallogr. 1993, 26, 343-350.)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    0.1051
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25554
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.840
_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            'dark red'
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2336
_exptl_crystal_recrystallization_method
;
Diffusion of PhMe into a solution in THF at rt.
;
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1396
_refine_ls_number_reflns         25554
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0328P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                17536
_reflns_number_total             25554
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3dt50523e.txt
_cod_data_source_block           ck22ck
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7021447