Ether and crown ether adduct complexes of sodium and potassium cyclopentadienide and methylcyclopentadienide—molecular structures of [Na(dme)Cp]∞ , [K(dme)0.5Cp]∞ , [Na(15-crown-5)Cp], [Na(18-crown-6)CpMe] and the “naked Cp−” complex [K(15-crown-5)2][Cp]
Marcus L. Cole; Cameron Jones; Peter C. Junk; J. Chem. Soc., Dalton Trans.  (2002) 896–905; doi:10.1039/b109124g

data_7011207
_publ_section_title
;
 Ether and crown ether adduct complexes of sodium and potassium
 cyclopentadienide and methylcyclopentadienide---molecular structures
 of [Na(dme)Cp]\\infty , [K(dme)0.5Cp]\\infty , [Na(15-crown-5)Cp],
 [Na(18-crown-6)CpMe] and the &#x201C;naked Cp&#x2212;&#x201D; complex
 [K(15-crown-5)2][Cp]
;
_journal_issue                   6
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              896
_journal_page_last               905
_journal_paper_doi               10.1039/b109124g
_journal_year                    2002
_chemical_formula_sum            'C28 H40 K4 O4'
_chemical_formula_weight         597.00
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.372(5)
_cell_angle_beta                 83.498(4)
_cell_angle_gamma                82.935(7)
_cell_formula_units_Z            2
_cell_length_a                   8.972(3)
_cell_length_b                   11.280(4)
_cell_length_c                   17.045(6)
_cell_measurement_temperature    296(2)
_cell_volume                     1691.9(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0987
_diffrn_reflns_av_sigmaI/netI    0.0955
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7399
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.9217
_exptl_absorpt_correction_T_min  0.8091
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.000(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         4528
_refine_ls_number_restraints     205
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1798
_refine_ls_R_factor_gt           0.0971
_refine_ls_shift/su_max          0.558
_refine_ls_shift/su_mean         0.090
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1758P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2543
_refine_ls_wR_factor_ref         0.3152
_reflns_number_gt                1817
_reflns_number_total             4528
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109124g.txt
_cod_data_source_block
COMPOUND_2#d:\junkie\xtals\bonocpxs\marcus\kcpdme\pj285a
_cod_original_cell_volume        1692.0(10)
_cod_database_code               7011207