Synthesis and studies of a tetradecanuclear manganese(ii)/(iii) cage
Aromí, Guillem; Bell, Aidan; Teat, Simon J.; Whittaker, A. Gavin; Winpenny, Richard E. P.; Chemical Communications  (2002) 1896–1897; doi:10.1039/b205157p

data_7111236
_publ_section_title
;
 Synthesis and studies of a tetradecanuclear manganese(ii)/(iii) cage
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1896
_journal_page_last               1897
_journal_paper_doi               10.1039/b205157p
_journal_year                    2002
_chemical_formula_sum            'C217 H194.5 Mn14 N55.5 O41'
_chemical_formula_weight         5004.94
_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                74.856(2)
_cell_angle_beta                 77.870(2)
_cell_angle_gamma                69.345(2)
_cell_formula_units_Z            2
_cell_length_a                   20.9499(18)
_cell_length_b                   22.6189(19)
_cell_length_c                   27.567(2)
_cell_measurement_reflns_used    33433
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      22.45
_cell_measurement_theta_min      2.21
_cell_volume                     11697.8(17)
_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      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     0.6872
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            74037
_diffrn_reflns_theta_full        22.44
_diffrn_reflns_theta_max         22.44
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             5126
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.206
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3225
_refine_ls_number_reflns         33472
_refine_ls_number_restraints     1668
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0835P)^2^+48.5107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1907
_reflns_number_gt                23416
_reflns_number_total             33472
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b205157psup1.cif
_cod_data_source_block           ga10b
_cod_original_cell_volume        11697.7(17)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C217 H194.50 Mn14 N55.50 O41'
_cod_database_code               7111236