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_7011206
_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            'C9 H15 Na O2'
_chemical_formula_weight         178.20
_space_group_IT_number           33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.799(13)
_cell_length_b                   8.149(3)
_cell_length_c                   9.379(4)
_cell_measurement_temperature    296(2)
_cell_volume                     2277.5(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1673
_diffrn_reflns_av_sigmaI/netI    0.1724
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10030
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  0.9898
_exptl_absorpt_correction_T_min  0.9697
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.144
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   3(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.803
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3239
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.803
_refine_ls_R_factor_all          0.2679
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          1.289
_refine_ls_shift/su_mean         0.218
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0867P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.2395
_reflns_number_gt                749
_reflns_number_total             3239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109124g.txt
_cod_data_source_block
COMPOUND_1#d:\junkie\xtals\bonocpxs\marcus\nacpdme\pj269
_cod_original_cell_volume        2277.7(17)
_cod_database_code               7011206