New routes to high nuclearity cages: a fluoride-based hexaicosametallic manganese cage
Jones, Leigh F.; Brechin, Euan K.; Collison, David; Harrison, Andrew; Teat, Simon J.; Wernsdorfer, Wolfgang; Chemical Communications  (2002) 2974–; doi:10.1039/b209445b

data_7114194
_publ_section_title
;
 New routes to high nuclearity cages: a fluoride-based hexaicosametallic
 manganese cage
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2974
_journal_paper_doi               10.1039/b209445b
_journal_year                    2002
_chemical_formula_sum            'C151.5 H196 F10 Mn26 N66 O46.5'
_chemical_formula_weight         5304.18
_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                98.907(2)
_cell_angle_beta                 95.758(2)
_cell_angle_gamma                101.778(2)
_cell_formula_units_Z            2
_cell_length_a                   17.9570(10)
_cell_length_b                   24.0865(14)
_cell_length_c                   27.3871(16)
_cell_measurement_reflns_used    11487
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.07
_cell_measurement_theta_min      2.21
_cell_volume                     11349.2(11)
_computing_cell_refinement       'Bruker SAINT v6.02a'
_computing_data_collection       'Bruker SMART v5.054'
_computing_data_reduction        'Bruker SAINT v6.02a'
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART 1K 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     0.6867
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_sigmaI/netI    0.1050
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37727
_diffrn_reflns_theta_full        20.08
_diffrn_reflns_theta_max         20.08
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.475
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange/brown
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             5358
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.525
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2581
_refine_ls_number_reflns         23486
_refine_ls_number_restraints     1432
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1316
_refine_ls_R_factor_gt           0.0786
_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^)+(0.1650P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2619
_reflns_number_gt                13934
_reflns_number_total             23486
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b209445b.txt
_cod_data_source_block           lfjc34a
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C151.50 H196 F10 Mn26 N66 O46.50'
_cod_database_code               7114194