New Routes to High Nuclearity Clusters: Fluoride-Based Octametallic and Tridecametallic Clusters of Manganese
Leigh F. Jones; Euan K. Brechin; David Collison; James Raftery; Simon J. Teat; Inorganic Chemistry 42 (2003) 6971–6973; doi:10.1021/ic034979b

data_4312443
_publ_section_title
;
 New Routes to High Nuclearity Clusters: Fluoride-Based Octametallic and
 Tridecametallic Clusters of Manganese
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6971
_journal_page_last               6973
_journal_paper_doi               10.1021/ic034979b
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C110.5 H155.5 F6 Mn13 N36 O27.25'
_chemical_formula_weight         3252.43
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                89.695(2)
_cell_angle_beta                 73.548(2)
_cell_angle_gamma                60.850(2)
_cell_formula_units_Z            2
_cell_length_a                   17.5604(13)
_cell_length_b                   17.7334(13)
_cell_length_c                   30.679(2)
_cell_measurement_reflns_used    10085
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.48
_cell_measurement_theta_min      2.23
_cell_volume                     7901.1(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART Proteum 200 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6935
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0925
_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       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            29859
_diffrn_reflns_theta_full        21.51
_diffrn_reflns_theta_max         21.51
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange/Red
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3335
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.197
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1742
_refine_ls_number_reflns         19051
_refine_ls_number_restraints     1392
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0849
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1247P)^2^+60.6343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2400
_refine_ls_wR_factor_ref         0.2607
_reflns_number_gt                13869
_reflns_number_total             19051
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic034979bsi20030818_045831.cif
_cod_data_source_block           lfj200
_cod_original_formula_sum        'C110.50 H155.50 F6 Mn13 N36 O27.25'
_cod_database_code               4312443