Mn(II)-Induced Formation and Structural Elucidation of a [3 + 3] Benzene Dimer Derivative from m-Phenylenebis(N-tert-butylaminoxyl)
Fumiyasu Iwahori; Katsuya Inoue; Hiizu Iwamura; Journal of the American Chemical Society 121 (1999) 7264–7265; doi:10.1021/ja9844534

data_4116479
_publ_section_title
;
 Mn(II)-Induced Formation and Structural Elucidation of a [3 + 3] Benzene
 Dimer Derivative from m-Phenylenebis(N-tert-butylaminoxyl)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7264
_journal_page_last               7265
_journal_paper_doi               10.1021/ja9844534
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C25 H27 Br Cl2 F12 Mn N2 O7'
_chemical_formula_weight         901.23
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_audit_creation_date             'Mon Oct 26 12:19:25 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 102.23(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.036(3)
_cell_length_b                   9.582(3)
_cell_length_c                   26.118(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      6.9
_cell_measurement_theta_min      5.1
_cell_volume                     3677.5(18)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.06047
_diffrn_orient_matrix_UB_12      -0.03120
_diffrn_orient_matrix_UB_13      0.02074
_diffrn_orient_matrix_UB_21      0.00623
_diffrn_orient_matrix_UB_22      -0.06574
_diffrn_orient_matrix_UB_23      -0.02875
_diffrn_orient_matrix_UB_31      0.03059
_diffrn_orient_matrix_UB_32      0.07481
_diffrn_orient_matrix_UB_33      -0.01668
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  2.45
_diffrn_reflns_av_sigmaI/netI    0.055
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            7443
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        -25.11
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.696
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       needle
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_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
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_refine_diff_density_min         -0.50
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   3.305
_refine_ls_goodness_of_fit_obs   4.468
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     451
_refine_ls_number_reflns         3680
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1445
_refine_ls_R_factor_obs          0.0714
_refine_ls_shift/esd_max         2.5320
_refine_ls_shift/esd_mean        0.1770
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00003|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0803
_refine_ls_wR_factor_obs         0.0780
_reflns_number_observed          3680
_reflns_number_total             7107
_reflns_observed_criterion       >2.0sigma(I)
_cod_data_source_file            ja9844534.cif
_cod_data_source_block           BrBZD(P2/n)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00003|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00003|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3677(1)
_cod_original_sg_symbol_H-M      'P 2/n '
_cod_original_formula_sum        'C25 H27 Br Cl2 F12 N2 Mn O7 '
_cod_database_code               4116479