A mixed-valence manganese(III)‒manganese(IV) di-μ-oxo complex, [(cyclam)MnO]~2~(ClO~4~)~2~(NO~3~)
Lu, Ying-Hong; Fun, Hoong-Kun; Chantrapromma, Suchada; Razak, Ibrahim Abdul; Shen, Zhen; Zuo, Jing-Lin; You, Xiao-Zeng; Acta Crystallographica Section C 57 (2001) 911–913; doi:10.1107/S0108270101008617

data_2012165
_publ_section_title
;
 A mixed-valence manganese(III)--manganese(IV) di-\m-oxo complex,
 [(cyclam)MnO]~2~(ClO~4~)~2~(NO~3~)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              911
_journal_page_last               913
_journal_paper_doi               10.1107/S0108270101008617
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[Mn2 O2 (C10 H24 N4 )2 ](ClO4 )2(NO3 )'
_chemical_formula_moiety         'C20 H48 Mn2 N8 O2 3+ , 2Cl O4 - , N O3 -'
_chemical_formula_sum            'C20 H48 Cl2 Mn2 N9 O13'
_chemical_formula_weight         803.45
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.5080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.9616(4)
_cell_length_b                   13.8047(4)
_cell_length_c                   12.1531(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      38.62
_cell_measurement_theta_min      2.45
_cell_volume                     3348.82(14)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material
;
SHELXTL and PLATON (Spek, 1990)
;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full .994
_diffrn_measured_fraction_theta_max .994
_diffrn_measurement_device_type
;
Siemens SMART CCD area detector diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0344
_diffrn_reflns_av_sigmaI/netI    .0362
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11565
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .986
_exptl_absorpt_correction_T_max  .8908
_exptl_absorpt_correction_T_min  .7057
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          .38
_exptl_crystal_size_mid          .36
_exptl_crystal_size_min          .12
_refine_diff_density_max         .801
_refine_diff_density_min         -.538
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          .0564
_refine_ls_R_factor_gt           .0493
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0856P)^2^+5.1838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1495
_reflns_number_gt                3292
_reflns_number_total             3823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk1485.cif
_cod_data_source_block           I
_cod_original_cell_volume        3348.80(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2012165
_cod_database_fobs_code          2012165