Novel synthetic route to soluble polyanions: synthesis and crystal structure of [K(18-crown-6)]4[Pb9]·en·tol †
Fässler, Thomas F.; Hoffmann, Rudolf; Journal of the Chemical Society, Dalton Transactions  (1999) 3339–; doi:10.1039/a906586e

data_7027770
_publ_contact_author
;
     Thomas F. Faessler
     Eidgenoessische Technische Hochschule Zuerich
     Laboratorium fuer Anorganische Chemie
     Universitaetstr.6
     ETH-Zentrum
     8092 Zuerich
     Switzerland
;
_publ_section_title
;
 Novel synthetic route to soluble polyanions: synthesis and crystal
 structure of [K(18-crown-6)]4[Pb9]&#x00B7;en&#x00B7;tol&#x200A;&#x2020;
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3339
_journal_paper_doi               10.1039/a906586e
_journal_year                    1999
_chemical_formula_sum            'C28.5 H56 K2 N O12 Pb4.5'
_chemical_formula_weight         1615.3
_chemical_name_common
;
     Potassium-[18]crown-6-Salt of Nonaplumbide(4-)
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 108.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.618(2)
_cell_length_b                   14.771(2)
_cell_length_c                   21.583(3)
_cell_measurement_reflns_used    512
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3.5
_cell_volume                     4428.9(13)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemnes SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Siemens Smart'
_diffrn_measurement_device_type  'Siemens Smart'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK/a
_diffrn_radiation_wavelength     0.71079
_diffrn_reflns_av_R_equivalents  0.0994
_diffrn_reflns_av_sigmaI/netI    0.0769
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39939
_diffrn_reflns_theta_full        26.45
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    17.289
_exptl_absorpt_correction_T_max  0.034995
_exptl_absorpt_correction_T_min  0.005537
_exptl_absorpt_correction_type   'empirical, Siemens SADABS'
_exptl_crystal_colour            'dark-red '
_exptl_crystal_density_diffrn    2.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             2948
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.508
_refine_diff_density_min         -1.744
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         9452
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                5934
_reflns_number_total             9452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906586esup1.cif
_cod_data_source_block           k4pb9
_cod_original_cell_volume        4428.8(11)
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               7027770