Multi-layered molecular charge-transfer salts containing alkali metal ions
Martin, Lee; Day, Peter; Clegg, William; Harrington, Ross W.; Horton, Peter N.; Bingham, Ann; Hursthouse, Michael B.; McMillan, Paul; Firth, Steven; Journal of Materials Chemistry 17 (2007) 3324–; doi:10.1039/b702442h

data_7202823
_publ_section_title
;
 Multi-layered molecular charge-transfer salts containing alkali metal
 ions
;
_journal_issue                   31
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              3324
_journal_paper_doi               10.1039/b702442h
_journal_volume                  17
_journal_year                    2007
_chemical_formula_moiety
'2.5 C 10 H 8 S 8 0.6+, 1.5 C 12 H 24 O 6, 1.5 K +, C 6 Fe O 12 3-, 6 H 2 O'
_chemical_formula_sum            'C49 H68 Fe K1.5 O27 S20'
_chemical_formula_weight         1844.73
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.622(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.9933(11)
_cell_length_b                   11.0441(4)
_cell_length_c                   20.7262(7)
_cell_measurement_reflns_used    9182
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.62
_cell_measurement_theta_min      2.19
_cell_volume                     7307.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX2 CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6712
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            79494
_diffrn_reflns_theta_full        28.64
_diffrn_reflns_theta_max         28.64
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3810
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.164
_refine_diff_density_min         -2.296
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1046
_refine_ls_number_reflns         22106
_refine_ls_number_restraints     1448
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0466P)^2^+5.4225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1126
_reflns_number_gt                16946
_reflns_number_total             22106
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b702442h.txt
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C49 H68 Fe K1.50 O27 S20'
_cod_database_code               7202823