A Mn(III)-superoxo complex of a zwitterionic calix[4]arene with an unprecedented linear end-on Mn(III)-O2 arrangement and good catalytic performance for alkene epoxidation
Lei-Lei Liu; Hong-Xi Li; Li-Min Wan; Zhi-Gang Ren; Hui-Fang Wang; Jian-Ping Lang; Chem.Commun. 47 (2011) 11146–; doi:10.1039/c1cc14262c

data_7106915
_publ_section_title
;
 A Mn(III)-superoxo complex of a zwitterionic calix[4]arene with an
 unprecedented linear end-on Mn(III)-O2 arrangement and good catalytic
 performance for alkene epoxidation
;
_journal_name_full               Chem.Commun.
_journal_page_first              11146
_journal_paper_doi               10.1039/c1cc14262c
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C40 H52 Mn N4 O7, 2(F6 P), 2(C O)'
_chemical_formula_sum            'C42 H52 F12 Mn N4 O9 P2'
_chemical_formula_weight         1101.76
_chemical_name_systematic
;
?
;
_space_group_IT_number           107
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4 -2'
_symmetry_space_group_name_H-M   'I 4 m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.590(2)
_cell_length_b                   14.590(2)
_cell_length_c                   13.553(3)
_cell_measurement_reflns_used    2971
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.4778
_cell_measurement_theta_min      3.4610
_cell_volume                     2885.0(8)
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3187
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         3.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_T_max  0.9296
_exptl_absorpt_correction_T_min  0.8659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Jacobson, R. (1998) Private communication to Rigaku Corp.'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1134
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.117
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.44(15)
_refine_ls_extinction_coef       0.061(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1199
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.1331
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1600P)^2^+25.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3268
_refine_ls_wR_factor_ref         0.3309
_reflns_number_gt                1112
_reflns_number_total             1199
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc14262c.txt
_cod_data_source_block           4
_cod_original_cell_volume        2884.9(8)
_cod_database_code               7106915